Overview of strategies for developing high thermostability industrial enzymes: Discovery, mechanism, modification and challenges

✅ 全文

高耐热性工业酶开发策略综述:发现、机制、改造与挑战

作者 Hao Wu; Qiuming Chen; Wenli Zhang; Wanmeng Mu 期刊 Critical Reviews in Food Science and Nutrition 发表日期 2021 ISSN 1040-8398 DOI 10.1080/10408398.2021.1970508 类型 原创研究 (Original Research)

📄 中文摘要 Chinese Abstract

中文
工业酶由于其底物特异性和环境友好性,被广泛应用于食品、制药、纺织、生物炼制和饲料等行业。然而,恶劣的工业条件——如高温、有机溶剂和极端pH值——往往会使酶失稳,降低其催化效率并限制其应用。因此,热稳定酶(thermozymes)备受青睐,因为它们能在高温条件下保持活性,具有反应速率更快和微生物污染减少等优势。开发此类酶的方法包括:从嗜极生物中发现新型热稳定变体,或利用蛋白质工程策略改造现有的常温酶。

📋 英文结构化总结 English Structured Summary

全文整理

EN

Background:

Industrial enzymes are widely used in food, pharmaceutical, textile, bio-refining, and feed industries due to their substrate specificity and environmental friendliness. However, harsh industrial conditions—such as high temperatures, organic solvents, and extreme pH—often destabilize enzymes, reducing their catalytic efficiency and limiting their applications. Thermostable enzymes (thermozymes) are therefore highly desirable, as they maintain activity under high-temperature conditions, offering advantages like faster reaction rates and reduced microbial contamination. Developing such enzymes involves either discovering novel thermostable variants from extremophiles or engineering existing mesophilic enzymes using protein engineering strategies.

Methods:

This review systematically analyzes approaches to obtain thermostable enzymes, including isolation from extreme environments (e.g., hot springs, deep-sea vents), metagenomics, genome sequencing, and recombinant expression in mesophilic hosts like *E. coli* or yeast. It also evaluates protein engineering strategies—rational design, semi-rational design, directed evolution, and *de novo* design—for enhancing enzyme thermostability. Key methodologies include sequence alignment, disulfide bond engineering, proline/glycine substitutions, surface charge optimization, B-factor analysis, and free energy calculations using computational tools such as FoldX, PoPMuSiC, and Disulfide by Design (DbD).

Results:

Thermophilic enzymes exhibit 40–85% sequence similarity with mesophilic counterparts but share highly similar tertiary structures and catalytic mechanisms. Key stabilizing forces include hydrogen bonds, salt bridges, hydrophobic interactions, aromatic ring interactions (π-π and cation-π), and disulfide bonds. Enzymes with higher thermostability display increased rigidity, better packing efficiency, lower unfolding entropy, and enhanced α-helix stability. Rational design strategies have successfully improved thermostability: for example, introducing disulfide bonds in phytase increased its half-life 3.8-fold at 60 °C; proline substitutions in luciferase extended its half-life 1.4-fold at 35 °C; and B-factor-guided mutagenesis of α-L-rhamnosidase increased half-life up to 2.3-fold at 70 °C.

Data Summary:

Quantitative improvements include: a xylanase mutant (Xyn376) showing an 820-fold longer half-life at 70 °C; a lipase mutant (6s) with Tm increased by 22.53 °C and T50 by 31.23 °C; a nitrilase mutant (AcN-T201F) with 13.5-fold longer half-life; and a D-allulose 3-epimerase mutant with Tm increased by 17.54 °C. Sequence alignment of thermophilic and mesophilic enzymes reveals conserved stabilizing residues, while computational tools predict ΔΔG values to guide mutations. Over 20 software platforms (e.g., FoldX, DbD, B-FITTER) support thermostability engineering.

Conclusions:

Thermostable enzymes can be effectively developed through both bioprospecting in extreme environments and advanced protein engineering. Rational design, guided by structural insights and computational modeling, enables targeted improvements in thermostability without compromising catalytic activity. Key strategies—such as introducing disulfide bonds, optimizing surface charges, reducing conformational entropy via proline substitutions, and enhancing hydrophobic packing—are proven effective. Integration of bioinformatics, molecular dynamics, and high-throughput screening accelerates the development of robust industrial biocatalysts.

Practical Significance:

Enhancing enzyme thermostability expands their utility in industrial processes requiring high temperatures, such as biofuel production, food processing, textile treatment, and pharmaceutical synthesis. Stable enzymes reduce operational costs, improve process efficiency, and enable greener chemistry by replacing harsh chemical catalysts. This advances sustainable manufacturing across multiple sectors, supporting the transition toward bio-based economies.

📋 中文结构化总结 Chinese Structured Summary

中文

背景:

工业酶由于其底物特异性和环境友好性,被广泛应用于食品、制药、纺织、生物炼制和饲料等行业。然而,恶劣的工业条件——如高温、有机溶剂和极端pH值——往往会使酶失稳,降低其催化效率并限制其应用。因此,热稳定酶(thermozymes)备受青睐,因为它们能在高温条件下保持活性,具有反应速率更快和微生物污染减少等优势。开发此类酶的方法包括:从嗜极生物中发现新型热稳定变体,或利用蛋白质工程策略改造现有的常温酶。

方法:

本综述系统分析了获取热稳定酶的方法,包括从极端环境(如温泉、深海热泉)中分离、宏基因组学、基因组测序,以及在*E. coli*或酵母等常温宿主中的重组表达。本文还评估了用于增强酶热稳定性的蛋白质工程策略——理性设计、半理性设计、定向进化和从头设计(*de novo* design)。关键方法包括序列比对、二硫键工程、脯氨酸/甘氨酸替换、表面电荷优化、B因子分析,以及使用FoldX、PoPMuSiC和Disulfide by Design (DbD)等计算工具进行自由能计算。

结果:

嗜热酶与常温酶的序列相似性为40%–85%,但具有高度相似的三级结构和催化机制。关键的稳定力包括氢键、盐桥、疏水相互作用、芳香环相互作用(π-π和阳离子-π)以及二硫键。具有较高热稳定性的酶表现出刚性增加、堆积效率更好、解折叠熵更低以及α-螺旋稳定性增强。理性设计策略已成功提高了热稳定性:例如,在植酸酶中引入二硫键使其在60 °C下的半衰期提高了3.8倍;荧光素酶中的脯氨酸替换使其在35 °C下的半衰期延长了1.4倍;基于B因子引导的α-L-鼠李糖苷酶突变使其在70 °C下的半衰期最高提高了2.3倍。

数据总结:

定量的改进包括:一种木聚糖酶突变体(Xyn376)在70 °C下的半衰期延长了820倍;一种脂肪酶突变体(6s)的Tm值升高了22.53 °C,T50值升高了31.23 °C;一种腈水解酶突变体(AcN-T201F)的半衰期延长了13.5倍;一种D-阿洛酮糖3-差向异构酶突变体的Tm值升高了17.54 °C。嗜热酶与常温酶的序列比对揭示了保守的稳定残基,而计算工具则通过预测ΔΔG值来指导突变。超过20个软件平台(如FoldX、DbD、B-FITTER)支持热稳定性工程。

结论:

通过在极端环境中的生物勘探和先进的蛋白质工程,均可有效开发热稳定酶。在结构洞察和计算建模指导下的理性设计,能够在不损害催化活性的前提下实现对热稳定性的靶向提升。关键策略——如引入二硫键、优化表面电荷、通过脯氨酸替换降低构象熵以及增强疏水堆积——已被证明是有效的。生物信息学、分子动力学和高通量筛选的整合加速了稳健工业生物催化剂的开发。

实际意义:

增强酶的热稳定性拓展了其在需要高温的工业过程中的应用,如生物燃料生产、食品加工、纺织品处理和药物合成。稳定的酶可降低操作成本、提高工艺效率,并通过替代苛刻的化学催化剂实现更绿色的化学过程。这推动了多个领域的可持续制造,支持了向生物基经济的转型。

📖 英文全文 English Full Text

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Overview of strategies for developing high thermostability industrial enzymes: Discovery, mechanism, modification and challenges

Hao Wu, Qiuming Chen, Wenli Zhang & Wanmeng Mu To cite this article: Hao Wu, Qiuming Chen, Wenli Zhang & Wanmeng Mu (2021):

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Overview of strategies for developing high thermostability industrial enzymes: Discovery, mechanism, modification and challenges

Hao Wua , Qiuming Chena, Wenli Zhanga and Wanmeng Mua,b aState Key Laboratory of Food Science and Technology, Jiangnan University, Wuxi, Jiangsu, China; bInternational Joint Laboratory on Food

Safety, Jiangnan University, Wuxi, Jiangsu, China ABSTRACT

Biocatalysts such as enzymes are environmentally friendly and have substrate specificity, which are preferred in the production of various industrial products. However, the strict reaction conditions in industry including high temperature, organic solvents, strong acids and bases and other harsh environments often destabilize enzymes, and thus substantially compromise their catalytic functions, and greatly restrict their applications in food, pharmaceutical, textile, bio-refining and feed industries.

Therefore, developing industrial enzymes with high thermostability becomes very important in industry as thermozymes have more advantages under high temperature. Discovering new thermostable enzymes using genome sequencing, metagenomics and sample isolation from extreme environments, or performing molecular modification of the existing enzymes with poor thermostability using emerging protein engineering technology have become an effective means of obtaining thermozymes. Based on the thermozymes as biocatalytic chips in industry, this review systematically analyzes the ways to discover thermostable enzymes from extreme environment, clarifies various interaction forces that will affect thermal stability of enzymes, and proposes different strategies to improve enzymes’ thermostability. Furthermore, latest development in the thermal stability modification of industrial enzymes through rational design strategies is comprehensively introduced from structure-activity relationship point of view. Challenges and future research perspectives are put forward as well.

1.  Introduction As an effective alternative to traditional chemical catalysts, thermozymes have been widely applied in food, pharma- ceutical, textile, bio-refining, and feed industries (Han et al.

2019). A good enzyme often meets industrial requirements like high substrate specificity, high catalytic efficiency, and high thermal stability, among which the thermal stability of enzyme is particularly important because of the resistance to the severe environment and maintenance of long-term catalysis at high temperatures (Karnaouri et al. 2019; Suresh et al. 2021). During the preparation of industrial products in industry, the chemical reaction often occurs in the system with high temperature owing to many merits, such as higher reaction rate, lower risk of microbial contamination (Wu,

Zhang, and Mu 2019; Kumar et al. 2019). Enzymes exert the best biological activities in the living systems during the long-term natural evolution (Liu, Xun, and Feng et al.

2019). However, most enzymes are derived from the meso- philic bacteria, and the tolerance is poor, severely restricting the broad industrial application (Atalah et al. 2019).

Therefore, new enzymes with high thermostability or mod- ification of the available mesophilic enzymes are significant for industrial application. In addition, it is necessary to establish an efficient molecular modification method to improve the thermal stability of enzymes.

The evaluation of the thermostability of enzymes from the perspective of structure and energy usually uses ther- modynamic stability and kinetic stability as parameters.

Thermodynamic stability is used to characterize the ten- dency of protein unfolding. In such a situation, the protein structure is in a relatively stable energy state determined by the entropy and enthalpy, and the unfolding trend is not spontaneous. Natural enzymes often evolve into a thermo- dynamically stable state to adapt to environmental tempera- ture (Rothschild and Mancinelli 2001). Thermodynamic stability of a protein is usually assessed by free energy of unfolding (ΔGu), melting temperature (Tm), and unfolding equilibrium constant (Ku). Kinetic stability refers to the time or temperature required for a protein to maintain half activ- ity when undergoing irreversibility (Polizzi et al. 2007). The measurement of kinetic stability requires detecting the res- idue activity of enzymes after incubating at specific condi- tions. Generally, Topt (the optimal temperature), T50 (the temperature when enzyme loses half activity), t1/2 (the time when enzyme loses half activity), and kd,obs (observed deac- tivation rate constant) (Bommarius and Paye 2013) should be measured.

© 2021 Taylor & Francis Group, LLC CONTACT Wenli Zhang wenlizhang@jiangnan.edu.cn https://doi.org/10.1080/10408398.2021.1970508

KEYWORDS Thermostability; protein engineering; industrial enzymes; extreme environment; interaction force

2 H. WU ET AL.

The recent development of bioinformatics and sequencing technology has promoted the discovery of new coding sequences of enzymes (Wang, Nie, and Xu 2019). More and more thermophilic enzymes have been isolated or cloned from hyperthermophilic and thermophilic strains. It was found that the sequence similarity between thermophilic enzymes and mesophilic enzymes could reach about 40%–85% (Vieille and Zeikus 2001), while the tertiary structure of which was also highly similar, and the catalytic mechanism was the same, indicating that there were other mechanisms and factors affecting enzymes’ thermal stability. Extensive studies have revealed that there are many interaction forces being in the amino acid residues of enzymes which are including hydrophobic interactions, salt bridges, aromatic ring interactions, disulfide bonds and hydrogen bonds, and these interaction forces play a very pivotal role in maintaining the conformational stability of enzymes. Additionally, enzymes with better thermal stability tend to have a more stable con- formation, such as higher rigidity, higher stacking efficiency, lower de-folding entropy, and alpha-helix stability (Vieille and

Zeikus 2001). Higher thermostability makes enzymes more competitive and desirable in the industrial application.

In the past few decades, continuous efforts have been made to obtain desired industrial enzymes with high thermostability through two main ways. One way is to screen hyperthermo- philic and thermophilic organisms from extreme environment (Figure 1). However, this screening process is complicated and tedious, and the enzyme activity is relatively low. The other way is to improve the thermostability of existing industrial enzymes derived from mesophilic organisms through advanced protein engineering strategies like rational design, semi-rational design, directed evolution and de novo design (Liu, Xun, and

Feng et al. 2019). Additionally, the computational tools for enzyme engineering are widely used aiding this process to better understand the thermostability mechanism of industrial enzymes (Chen et al. 2020). However, rational design requires a comprehensive understanding of the relationship of the structure, function, catalytic mechanisms of enzymes.

Semi-rational design involves mutations based on sequence, structure or computational models, followed by small-scale mutagenesis and screening methods (Zhang, Geary, and

Simpson 2019). Directed evolution requires the construction of a large mutant library and efficient high throughput screen- ing (HTS) methods. De novo protein design explores the full sequence space, guided by the physical principles that underlie protein folding (Huang, Boyken, and Baker 2016).

This review systematically summarizes some achievements in the thermal stability of industrial enzymes applied in food, pharmaceutical, textile, bio-refining and feed indus- tries. The mechanisms and factors affecting the thermosta- bility of enzymes are discussed in detail. Then, strategies for developing high thermostability enzymes including how to obtain enzymes and how to modify the molecular struc- ture of existing enzymes with weak thermal stability through advanced protein engineering techniques are proposed as well. Mature methods to improve the thermal stability of enzymes through rational design are analyzed.

2.  Factors affecting protein thermal stability 2.1.  Hydrogen bond

Hydrogen bonding is an important non-covalent interaction in protein structure, which not only exists between the

Figure 1.  The flow chart of obtaining thermostable enzymes from extreme environment using different separation strategies.

Critical Reviews in Food Science and Nutrition 3 amino acid residues in the protein but also manifests in the interaction between the protein and the surrounding water molecules (Figure 2). This is because there are many hydrogen donors and hydrogen acceptors between the water molecules inside and around the protein. Generally, the distance of hydrogen donors and hydrogen acceptors is not more than 3 Å and the angle is less than 90 degrees. The energy provided by each pair of hydrogen bonds formed in the protein is about 0.6 kcal/mol (Li, Zhou, and Lu 2005).

Vogt et al., have found that the thermostability of protein is closely related to the number of hydrogen bonds after comparing different families of proteins in terms of their respective fractional polar atom surface areas (Vogt, Woell, and Argos 1997). Vieira et al., have dealt with two struc- turally similar family 11 xylanases, BCX (mesophilic xylanse from Bacillus circulans) and TLX (thermophilic xylanase from Thermomyces lanuginosus) by molecular dynamics simulations, and demonstrated that the intramolecular hydrogen bonds and salt bridges were key factors for the maintenance of the backbone rigidity at high temperatures (Vieira and Degrève 2009). Later research has reaffirmed the conclusion that thermophilic enzymes have more hydro- gen bonds than mesophilic enzymes (Tompa, Gromiha, and

Saraboji 2016). Besides, Ishak et al., have found that the melting temperature (Tm) of recombinant lipase mutants

D43E and E226D from Geobacillus zalihae increased up to

76 °C and 77.4 °C, respectively, while that of the wild-type enzymes were 70.9 °C (Ishak et al. 2020). Further structural investigations about G. zalihae lipase mutants D43E and

E226D have indicated that the improvement of lipase sta- bility was attributed to the additional hydrogen bonds and ion-pair interactions. Interestingly, the introduction of inter- chain hydrogen bonds at the interface regions also contrib- uted to the thermostability and structural stability of

D-allulose 3-epimerase from Dorea sp. CAG317 with Tm increased by 17.54 °C compared to wild type (Zhang et al. 2018).

2.2.  Salt bridge Salt bridge is formed through the electrostatic attraction of amino acid residues with opposite charges (Figure 2). As a driving force for maintaining the structure thermostability of protein at high temperatures, salt bridge frequently appears on the surface of proteins (Xu, Cen et al. 2020). Thermophilic proteins tend to possess more surface salt bridges than homologous mesophilic proteins at high temperatures (de

Bakker, Hünenberger, and McCammon 1999; Szilágyi and

Závodszky 2000). Also, salt bridge is considered as a more important factor than hydrogen bond in thermophilic pro- teins. The molecular dynamics simulation results illustrated that high temperature would lead to more intra-protein

Figure 2.  Factors and characteristics affecting the thermal stability of industrial enzymes.

4 H. WU ET AL. interaction energy due to the tightening of salt bridges, which also explained that the reason why salt bridges may stabilize hyperthermophilic proteins at elevated temperatures rather than at room temperature. Another reason was that the large desolvation penalty incurred by the association of two charged residues forming a salt bridge was not com- pensated by intra-protein interaction at room temperature (Szilágyi and Závodszky 2000). Therefore, introduction of a desirable salt bridge remains a very difficult task as some- times it will result slight stabilization or destabilization of proteins. Additionally, Szilágyi and Závodszky have compiled a non-redundant data set, comprising high-quality structures of thermophilic proteins and the mesophilic homologues to draw general evolution of the heat stability of proteins (Szilágyi and Závodszky 2000). It was found that the number of salt bridges was a significant factor affecting the stability of proteins, and the number of salt bridges in thermophilic proteins was higher than that of mesophilic proteins. To increase the thermostability of 1,4-α-glucan branching enzymes from Geobacillus thermoglucosidans (GtGBE), Ban et al., have introduced additional local salt bridges into

GtGBE and results showed that five separately introduced mutants, namely, Q231R-D227, Q231K-D227, T339E-K335,

T339D-K335, and I571D-R569 had longer half-life of 17% to 51% than that of wild-type (Ban et al. 2020). Further circular dichroism and intrinsic fluorescence experiments indicated that the improved thermostability of GtGBE mutants may be ascribed to the enhanced rigidity in newly formed salt bridge networks. Chan et al., have investigated how salt-bridge influenced protein stability with the research on the pair-wise interaction energy and ΔCp (heat capacity change of unfolding) (Chan et al. 2011), and the results indicated that extra salt-bridges enhanced the thermostability of proteins by reducing ΔCp, which would make protein stability curves rise and widen.

2.3.  Hydrophobic interaction Many studies have confirmed that hydrophobic interaction plays an important role in maintaining protein stability and forming protein tertiary structure, where the hydrophobic environment is the major factor affecting the stability of thermophilic proteins when compared with other interac- tions, such as salt bridges and hydrogen bonds. The hydro- phobicity content has also been proposed to be informative for discriminating between mesophilic and thermophilic proteins (Modarres, Mofrad, and Sanati-Nezhad 2016).

Gromiha et al., have found that 80% of thermophilic pro- teins show higher hydrophobicity than mesophilic ones based on a dataset of 373 protein families (Gromiha et al.

2013). The interaction force is generated mainly due to the cluster and hydrophobic amino acid side chains which instinctively repels the contact with water (Folch, Rooman, and Dehouck 2008). Therefore, the hydrophobic amino acids (nonpolar amino acids) in aqueous solutions are usually buried inside proteins, forming a hydrophobic core, whereas polar amino acids are distributed in the hydrophilic envi- ronment on the protein surface. It was reported that the stable protein could obtain 1.3 ± 0.5 kcal/mol when every additional −CH2− group was buried in the protein (Figure

2) (Pace 1992). By introducing a methyl group into the hydrophobic core of E. coli ribonuclease H1, Ishikawa et al., have successfully achieved the thermostability of the enzyme (Ishikawa et al. 1993). This can be explained by the later research findings that more hydrophobic interaction would make the unfolding rate slower in thermostable pro- teins (Okada et al. 2010). Relevant literature had reported that the thermostability of D-allulose 3-epimerase from

Rhodopirellula baltica was enhanced to a Δt1/2 of 50.4 min,

ΔTm of 12.6 °C, and ΔT50 60 of 22 °C after the site-directed mutation of L144F (Mao et al. 2020). Further detailed anal- ysis of the structure indicated that a new hydrophobic inter- action was produced in the mutation protein. A similar result was also observed in the double point mutant T130M/

E133F of (R)-selective amine transaminase from Aspergillus terreus, with 3.3-fold in t1/2 at 40 °C and 5 °C higher in

T1/2 10

min thermal stability than wild type enzyme, which was due to the newly formed hydrophobic interactions and hydrogen bonds (Huang, Xie, and Feng 2017). Furthermore, when error-prone PCR and rational design based on

B-factors were used, the thermostability of optimal variant

Xyn376 from GH 11 family showed a half-life 820-fold higher than that of the wild-type enzyme at 70 °C (Xing et al. 2021). The hydrogen bonds and hydrophobic interactions were the major forces for improved thermostability by the structural analysis.

2.4.  Aromatic ring interaction Aromatic ring interaction is also an important driving force for protein thermostability, mainly including the interaction of cation (positively charged amino acids, such as Lys, Arg and protonated His) and aromatic ring (cation-π), or aromatic-aromatic interaction (π-π). The cation-π interaction was a general, strong and non-covalent binding force, pro- viding the energy twice as strong as that of salt bridges (Chakravarty and Varadarajan 2002; Dougherty 2007). The interaction of aromatic ring amino acids (Try, Tyr and Phe) mainly occurs when the distance between the phenyl ring centroids is less than 7.0 Å (Figure 2). A π-π interaction usually stabilizes a protein molecule by 0.6–1.3 kcal/mol when the preferential distance of the centroids of the two aromatic rings are 5.5 Å (Ohmura et al. 2001). However, the aromatic interactions happen when the orientation of aro- matic rings is in offset stacked or edge-face, which results in some challenges to design aromatic interactions. To sys- tematically clarify the contribution of aromatic interactions to the thermostability of proteins, Kannan et al., have inves- tigated a dataset of 24 protein families with known crystal structures from the thermophilic and the mesophilic homo- logues, and found that 17 thermophilic protein families possessed additional aromatic clusters or enlarged aromatic networks located on the protein surface than the corre- sponding mesophilic homologues (Kannan and Vishveshwara

2000). Yoneda et al., have revealed that the higher thermo- stability of B. smithii indio reductase was due to the

Critical Reviews in Food Science and Nutrition 5 intersubunit aromatic interactions (F105-F172′ and F172 and F105′), and F105 played a governing role in these aromatic interactions (Yoneda et al. 2020). The additional aromatic interaction of Y11-Y16 could increase the stability of the N-terminal part of mesophilic family 11 xylanase from Streptomyces sp. S38, which increased Tm by 9 °C, indi- cating that adding π-π interaction at the appropriate place could improve the thermostability of the protein (Georis et al. 2000). A recent study has declared that half-lives of the nitrilase mutants AcN-T201F and AcN-T201W constructed by error-prone PCR were 13.5- and 10.8-fold longer than that of wild-type AcN, respectively (Xu et al. 2018). The molecular modeling suggested that W201 or F201 residue of nitrilase mutant not only improved the stability of the dimer interface but also formed π-π interaction with W165 residue to stabilize the substrate binding pocket, indirectly enhancing the thermostability.

2.5.  Disulfide bond Disulfide bonds are formed between the cysteine residues (Cys) with the distance of the alpha carbon atoms in space ranging from 4 to 9 Å (Figure 2). This process is one of the posttranslational modifications dependent on the con- formation of proteins and requires a specific redox envi- ronment and chaperones proteins (Creighton 1984). Disulfide bonds, as covalent interactions, which stabilize the structure of proteins by reducing conformational entropy, play a vital role in the folding and activity of proteins. Compared with the non-covalent interactions forces, such as hydrogen bonds, salt bridges, hydrophobic interactions and aromatic interactions, disulfide bonds provide the greatest energy for protein stability. It has been reported that the average sep- aration between Cys forming a disulfide cross-link is 15 residues for natural protein, which can provide 3.0 kcal/mol energy if assuming negligible effect on the folded form (Kazlauskas 2018). However, many factors should be taken into account to construct disulfide bonds. To figure out the factors that may affect the successful construction of disul- fide bonds, Dani et al., have reevaluated and refined an automated procedure for modeling the disulfide bonds in proteins through a computational MODIP program (Dani,

Ramakrishnan, and Varadarajan 2003), and found that the stabilized disulfide bonds were associated with the proper stereochemistry, lower depth regions, relatively higher mobil- ity (higher B-factors) and longer loop lengths (25–75 resi- dues). To effectively improve the protein stability and modify functional properties, a software named Disulfide by Design (DbD) and an accessible web server hosting site (http:// cptweb.cpt.wayne.edu/DbD2/) have been developed by Craig and Dombkowski to auxiliary predict pairs of residues that would likely form a disulfide bond if mutated to Cys (Craig and Dombkowski 2013). Compared with other non-covalent interaction forces including hydrogen bonds and hydropho- bic forces, it seems to be a more convenient and simple method to design disulfide bonds assisting by computational calculation programs and software. However, the formation and correct folding of disulfide bonds are also full of uncertainty due to the redox instability which is not fit for enzymes that function in reducing environment.

Extensive studies have been carried out to enhance the thermostability of enzymes by introducing disulfide bonds (Vasudevan et al. 2019). A recent study had successfully enhanced the thermostability of phytase from B. licheni- formis WHU by DbD v2.05 program coupled with homology models analysis, whose mutant G197C/A358C was 3.8-fold than wild type enzyme in half-life at 60 °C (Zhang et al.

2020). Molecular dynamics results indicated that the ther- mostability mechanism of this G197C/A358C mutant was that the newly formed disulfide bonds might anchor the

C-terminus of phytase and reinforce the local packing rigid- ity. In the study of Tang et al., two disulfide bonds had been separately constructed, namely Xyn2C14–52 and Xyn2C59–

149, between the N-terminal and α-helix to the β-sheet core of Xyn2 using site-directed mutagenesis at the corresponding residues, respectively, and resulted 2.5- and 1.8-fold longer half-lives than the wild type Xyn2 at 60 °C (Tang et al.

2017). The newly formed disulfide bonds effectively stabi- lized the Xyn2 structure by preventing the structure from unfolding, which may be the mechanism for the improved thermostability. Li et al., have engineered different regional multiple disulfide bonds to improve the thermostability of lipase from Yarrowia lipolytica (Li, Zhang et al. 2019). The sextuple mutant 6 s showed that Tm and T50

15 (Temperature that the activity loss half at 15 min) increased by 22.53 °C and 31.23 °C, respectively, due to more rigidified enzyme structures and longer unfolding times after introducing addi- tional disulfide bonds.

2.6.  Protein packaging efficiency Protein packaging efficiency, which is related to the thermal stability of a protein, is defined as the ratio of the hydro- phobic surface area to the total area of the protein surface (Vieille and Zeikus 2001) (Figure 2). Karshikoff et al., had analyzed the structures of 80 non-homologous mesophilic proteins, 20 thermophilic proteins and 4 hyperthermophilic proteins, and found that thermophilic proteins often had higher protein packaging efficiency (Karshikoff and

Ladenstein 1998). An improvement in the inner packing effectively enhances protein stability since an increase in buried cavities destabilizes protein structure (Eriksson et al.

1992; Xu et al. 1998). Abraham et al., had chosen 43 resi- dues of Lipase A from B. subtilis with exposure ratio below

5% and packing value below 0.55 as first-round mutant candidates and found that less-packed residues with no water-contact were good target sites for enhancing thermo- stability (Abraham et al. 2005). Based on the strategies of

Gly mutation to Ala, and Ala mutation to Val, six mutants, namely, A38V, A75V, G80A, A105V, A146V and G172A were obtained with higher thermostability than that of wild-type. Among them, half-lives of A38V, G80A, and

G172A mutant increased 64- to 70-fold than wild type lipase

A. One study has also shown that reducing the hydrophobic surface area of flavodoxin by changing the hydrophobic amino acids on the surface into hydrophilic amino acids

6 H. WU ET AL. could significantly improve the thermal stability of the pro- tein (Ayuso-Tejedor, Abián, and Sancho 2011).

3.  Discovery natural enzymes with high thermostability

It is believed that the properties of enzymes are closely related to the environment in which the host lives owing to the long-term natural evolution (Ueno, Ibarra, and

Gojobori 2016). Accordingly, it is reasonable to think that microorganisms that grow in a high-temperature environ- ment may secrete enzymes with good thermal stability (Table

1). Previous studies have revealed that extremophiles sur- vived in extreme conditions could secrete novel enzymes with various properties, which could be applied in chemical, food and pharmaceutical industries. Therefore, extremophiles have gained much research attention (Chettri et al. 2021;

Herbert 1992; van den Burg 2003; Verma, Meghwanshi, and

Kumar 2021), and thermostable enzymes can be obtained by novel proteins from extremophiles such as hyperthermo- philes or thermophiles (Figure 1).

At present, only a minor fraction of microorganisms that can resist extreme heat have been reported, and most of which belong to archaea. Many of these available microor- ganisms that grow in extreme conditions, such as deep-sea, hot-spring environment, are difficult to be cultivated in the laboratory environment, which makes the production of enzymes from extremophiles infeasible through fermentation technology. Nonetheless, the development of genome sequencing, molecular biology and metagenomics has accel- erated the gene mining, discovery and identification of enzymes, such as xylanase (Chadha et al. 2019; Ferrer et al. 2016; Lorenz and Eck 2005; Mhiri et al. 2020; Patel et al. 2019). Besides, many plasmid vectors and mature expres- sion systems allow the extremophiles-derived enzymes to be cloned and expressed in the mesophilic hosts that are easy to be cultivated in the laboratory with mature molec- ular biotechnology. Furthermore, many prokaryote systems such as Escherichia coli, Bacillus, Lactobacillus, and eukary- otic systems such as Pichia, Saccharomyces cerevisiae, and

Candida have been developed as selectable expressing hosts for producing different source enzymes (Peng et al. 2021).

For example, both the D-lyxose isomerase from Thermoprotei archaeon and L-aminoacylase from Thermococcus litoralis have been successfully cloned, expressed and characterized in E. coli hosts (Toogood et al. 2002; Wu et al. 2020). The β-glycosidase from extreme thermoacidophilic archaeon

Sulfolobus solfataricus has been expressed in yeast systems (D’Auria et al. 1996). Fortunately, the majority of hyperther- mophilic enzymes expressed in these expressing systems retain all of the native enzymes’ biochemical properties, including proper folding and thermostability (Ebaid et al.

2019; Grättinger et al. 1998; Shi et al. 2019; Vieille and

Zeikus 2001).

4.  Protein engineering strategies for developing thermostable enzyme

4.1.  Rational design In recent years, with the rapid development of bioinformatics technology and structural biology, rational design strategies have become important means to modify the properties of proteins (Table 2). A practical rational design is based on the comprehensive understanding of the protein structure, function and structure-activity relationship, and then pur- poseful modification of the specific sites of the protein through selective substitution, insertion or truncation, and further experimental analysis of the property changes of the designed protein. However, the application range of rational

Table 1.  Different strategies used to discovery natural enzymes with high thermostability.

Microorganisms Sources Microorganism Topt (°C) Methods

Production Enzymes Topt (°C) Thermostable ability References

Pyrococcus furiosus DSM 3638 Shallow thermal waters near

Vulcano Island, Italy 100 Sample isolation Native α-amylase

106 Retain approximately 30% of initial activity after 8 h at 98 °C (Brown,

Costantino, and Kelly 1990) Thermococcus sp.

Hot-spring environment 85 Sample isolation Native cyclomaltodextrin glucanotransferase

110 40 min half-life at 110 °C (Tachibana et al. 1999)

T. aggregans Deep-sea from the Guaymas Basin 85 Cloning and expression in

Escherichia coli Recombinant pullulan hydrolase III

100 2.5 h half-life at 100 °C (Niehaus et al.

2000) P. furiosus DSM 3638 Shallow thermal waters near

Vulcano Island, Italy 100 Cloning and expression in E. coli

Recombinant esterase 100 50 min half-life at 126 °C (Ikeda and

Clark 1998) NS Offshore oil reservoir on the Norwegian

Continental Shelf NR Metagenome isolation Recombinant esterase

NR 90 °C for 1 h without any notable decrease in activity (Lewin et al.

2016) NS Compost NR Metagenome isolation Recombinant endoglucanase

85 Retain full activity after 24 h at 60 °C (Jensen et al.

2018) NR, not reported; NS, not specified.

Critical Reviews in Food Science and Nutrition 7 design is restricted due to a limited understanding of the catalytic mechanism and thermostability mechanism.

Currently, the rational design strategies that have been suc- cessfully applied mainly include homologous sequence align- ment, protein surface charge engineering, disulfide bonds design, proline and glycine design, free energy of protein unfolding design, temperature factor design and anchoring of unstable regions (Figure 3).

4.1.1.  Based on homologous sequence alignment The primary structure of a protein is defined as the sequence of amino acid residues in the polypeptide chain of the protein, determining other high-level structures of the protein.

Therefore, the sequence alignment of proteins with various thermal stabilities would provide useful amino acid residues affecting the proteins’ functions. Previous studies have reported that the sequence similarity of thermophilic enzymes and mesophilic enzymes could reach 40%–85% (Vieille and Zeikus

2001). Accordingly, the amino acid sites related to thermal stability could be found by sequence alignment between pro- teins with high or poor thermal stability, and then possible mutation sites could be selected or designed to improve the thermal stability of proteins (Table 3). Based on homologous sequence alignment, Xiao et al., have successfully improved the thermostability of pectase lyase from Xanthomonas camp- estris, with Tm increasing by 6 °C and half-life being 23-fold longer at 45 °C (Xiao et al. 2008). Similarly, G312 and K436 have been selected as the site-directed mutagenesis targets to improve the thermostability of maltogenic amylase from

Bacillus sp. US149 by sequence alignments and homology modeling (Mabrouk et al. 2011). The maltogenic amylase dou- ble point mutant G312A/K436R displayed Topt and half-life time increased by 5 °C and 10 min at 55 °C, respectively. Based on the multiple sequence alignment of D-psicose 3-epimerase from various organisms, t1/2 value of mutant G109P from

Clostridium bolteae ATCC BAA-613 increased by 2.1-fold to that of wild-type enzyme (Zhang et al. 2016).

4.1.2.  Based on protein surface charge engineering

Protein surface charge engineering is a powerful tool to change some enzyme properties (Zhou et al. 2019). Almost all natural proteins contain charged amino acids which are distributing on the surface of the protein to increase the stability of the protein through the interaction between charges. Optimizing the charged amino acids on the protein surface is a promising method to improve the thermal stability of protein (Strickler et al. 2006; Zouari Ayadi et al. 2015). As expected, this engineering successfully improved the activity, thermostability and ionic liquid tol- erance of B. subtilis lipase A, further convincing it a pow- erful approach in surface charge engineering to enhance thermostability (Zhou et al. 2019). It has also been reported the remarkable significance of protein surface charge engi- neering in strengthening the thermostability of endogluca- nase II from Penicillium verruculosum and stability in

1-butyl-3-methylimidazolium chloride (Dotsenko et al.

2020). Through analysis of protein surface topography, mul- tiple sequence alignment and ΔG calculations, it was found that the half-life time of endoglucanase mutant E70S and

V150L increased by 1.2 and 1.4-fold at 80 °C, respectively (Table 3). In addition, the thermal activation and T50 of laccase mutant E188K from Bacillus HR03 were 3-fold and

5 °C higher than wild type enzyme, respectively, by intro- ducing positive charge on its surface loop (Mollania et al.

2011; Liu et al. 2020).

4.1.3.  Based on disulfide bonds design Disulfide bond is a kind of interaction force formed by the covalent bonding of two Cysteines (Figure 3). The DbD

Table 2.  Some of the popular softwares applied in the protein engineering for improving thermostability.

Software Input Function Output Access websites References

FoldX Structure A force filed for energy calculations and protein design (ΔΔG) between the final state (the mutant) and the reference state (the wild-type protein) http://foldx.embl.de/ (Schymkowitz et al.

2005) PoPMuSiC Structure Predicting stability changes (ΔΔG) between the final state (the mutant) and the reference state (the wild-type protein) http://dezyme.com/. (Dehouck et al. 2009)

B-FITTER Structure Predicting the flexibility of protein structure based on B-factor

A ranked classification of all the residues according to the B-factor http://www.kofo.mpg.de/ en/research/ biocatalysis. (Reetz and Carballeira

2007) Disulfide by Design Structure Predicting pairs of residues that will likely form a disulfide bond

A series of potential disulfide bonds pairs, including bond energy, angle and B factor values http://cptweb.cpt.wayne. edu/DbD2/. (Craig and

Dombkowski 2013) Molecular dynamic simulation Structure

Performing dynamic properties of a protein at atomic level during a period of time.

Root mean square fluctuation (RMSF), Root mean square deviation (RMSD), Radius of rotation (Rg)

Gromacs, Amber, NAMD or Charmm (Zeiske, Stafford, and

Palmer 2016) Swiss-model Sequence Building a three-dimensional structure of protein

Generating a three-dimensional structure of target protein based on the available homologous crystal protein structure https://swissmodel.expasy. org/interactive. (Waterhouse et al.

2018) HotSpot Wizard 3.0 Sequence/ Structure Automated prediction of hotspots and the design of smart libraries in semi-rational protein design

Single-point mutant or multiple-point mutant or smart library https://loschmidt.chemi. muni.cz/ hotspotwizard/. (Sumbalova et al.

2018) 8 H. WU ET AL. software provides a convenient pathway to identify potential disulfide bonds to improve the thermal stability of the pro- tein based on the integration analysis of bonding energy, bonding dihedral angles, bonding distances, bonding geom- etry and values of temperature factor (B-factor) (Craig and

Dombkowski 2013). Currently, extensive studies have paid much attention on disulfide bond strategy to alter the ther- mostability of proteins (Table 3). For example, the thermo- stability of diisopropyl-fluorophosphatase mutant V24C/C76 at 60 °C was successfully enhanced after using the disulfide bond engineering, because the designed V24C/C76 displayed the lowest energy (0.33 kcal/mol) and a lower B-factor (15.07) which were predicted by DbD software (Mohammadi et al. 2018). Samson et al. have found that the thermosta- bility of catalase from B. pumilus was strengthened by intro- ducing a disulfide bond between S286C and D289C with the half-life showing 48 min longer than that of the wild type at 60 °C (Samson et al. 2018). Furthermore, the con- structed glucose dehydrogenase mutant, V149C/G190C, showed a 110 min half-life of thermal inactivation at 45 °C, which was 13-fold greater than that of the wild-type enzyme, and that the mutant’s catalytic activity and kinetic param- eters were not affected (Sakai et al. 2015).

4.1.4.  Based on proline and glycine design It was reported that the mutation of Xaa to Proline or

Glycine to Xaa could increase the stability of protein because these substitutions could decrease the unfolding entropy of proteins (Matthews, Nicholson, and Becktel 1987). Proline has a pyrrolidine ring on the side chain, and the rotation of N-Cα is restricted, contributing to a smaller degree of conformational freedom and conformational rigidity increase (Figure 3) (Dotsenko et al. 2019). Nonetheless, only the replacement of proline at the appropriate site could improve the thermal stability of the protein (Tian et al. 2010; Zhou,

Xue, and Ma 2010). The decreasing content of glycine is also beneficial for the stability of proteins because glycine has high conformational entropy (Xu, Cen et al. 2020). For example, the mutation of Gly to Ala within the α-helix could improve the protein thermostability because of high helical propensity and low conformational entropy (Scott et al. 2007). Interestingly, Yi et al., have reported that intro- ducing glycine to the protein surface would improve the thermostability of endoglucanase CelA from Clostridium thermocellum (Yi, Pei, and Wu 2011). Previous study has indicated that the substitutions of Xaa to proline located in regions of the β-turn and the N-cap of the α-helix were

Figure 3.  Different strategies to improve thermal stability of enzymes.

Critical Reviews in Food Science and Nutrition 9 Table 3.  Different protein engineering strategies to improve the thermostability of various industrial enzymes.

Enzymes Microorganisms or Plasmids Strategies Mutants

Results (than wild type) Thermostable mechanisms Applications

References Pectase lyase Xanthomonas campestris Sequence alignment strategy of mesophilic and thermophilic proteins

R236F Half-life: 23-fold at 45 °C Tm: 6 °C higher Hydrophobic desolvation analyzed by structure analysis and computational methods

Hemp fiber-processing, fruit ripening (Xiao et al. 2008)

Maltogenic amylase Bacillus sp. US149 Sequence alignments and homology modeling

G312A/K436R Half-life: 10 min higher at 55 °C Topm: 5 °C higher

Hydrophobic interactions, salt bridges, hydrogen bonds

Bread, baking industry (Mabrouk et al.

2011) Endoglucanase II Penicillium verruculosum Protein surface topography, multiple sequence alignment and ΔΔG calculations

A52K, E70S, and V150L Half-life: 1.3–1.6 fold at 70 °C

Half-life: 1.2–1.4 fold at 80 °C NR Wood industry (Dotsenko et al.

2020) Laccase Bacillus HR03 Introducing positive charge on the surface loop

E188K T50: 5 °C higher Higher tightness of the enzyme structure

Beverages, wastewater treatment, drug analysis, bioremediation (Mollania et al.

2011) Diisopropyl- fluorohosphatase (DFPase) Loligo vulgaris

Introducing disulfide bridges V24C/C76 Thermostability is higher at 60 °C

More stable secondary structures, Rigidifying flexible regions

Medicine (Mohammadi et al.

2018) Catalase Bacillus pumilus ML413 Introducing disulfide bridges

S286C/D289C Half-life: 48 min higher at 60 °C Generating long inter-residues interactions

Food, textile, healthcare (Samson et al.

2018) Luciferase NR Proline substitutions within flexible regions

H489P Half-life: 1.4-fold at 35 °C Rigidifying flexible regions

487–495 Diagnostic, therapeutic application (Yu et al. 2015)

Feruloyl esterase Aspergillus niger Calculating the folding free energy change

D93G/S187F Half-life: 9.6-fold at 50 °C Lower conformational energy

Agrifood, pharmaceutical industries (Zhang and Wu 2011)

Transglutaminase Streptomyces hygroscopicus Calculating the folding free energy change

P132I Half-life: 31% higher at 50 °C Increased hydrogen bonds,

Stronger internal hydrophobicity Food, textile (Tong et al. 2018)

Tyrosinase Streptomyces kathirae SC-1 Calculating the folding free energy change

R95Y/G123W Half-life: 1.5-fold at 60 °C Additional hydrogen bonds

Medicine, cosmetic, food, environmental protection (Guo et al. 2017)

Lipase Rhizopus chinensis Calculating the folding free energy change

S142A/D217V/ Q239F/S250Y Half-life: 41.7-fold at 60 °C,

Topm: 5 °C higher T50 30: 15.8 °C higher Decreased solvent accessible surface area, newly formed salt bridges, increased folding free energy

Food, oil, pharmaceuticals, paper, leather, detergent, cosmetics (Wang et al. 2020) α-L-Rhamnosidase

Aspergillus terreus B-factor-saturation mutagenesis strategy

G827K/D594Q Half-life: 2.3-fold at 70 °C Newly formed hydrogen bonds and salt bridges

Food, pharmaceutical industries (Ge et al. 2018) Feruloyl esterase

Aspergillus usamii B-factor, folding free energy, iterative saturation mutagenesis

S33E/N92R Half-life: 3.96-fold at 50 °C Tm: 4.7 °C higher

Additional hydrogen bonds Food, textile, pharmaceutical industries (Yin et al. 2015)

Lipase B Candida antarctica B-factor, RosettaDesign, packing analysis tool “Voronoia”

R249L Tm: 2.3 °C higher Decreasing number of cavities

Dairy, nutrition, cosmetics, pharmaceutical (Kim, Le, and Kim

2010) Xylanase 2 Trichoderma reesei Introducing disulfide bonds between

N-terminus and β-sheet F14C/Q52C Half-life: 2.5-fold at 70 °C

Decreasing the entropy of unfolded state Food, feed, pulp, biofuel (Tang et al. 2017) (Continued)

10 H. WU ET AL.

Xylanase Thermomyces lanuginosus Introducing disulfide bond into

N-terminal region Q1C-Q24C Half-life: 20-fold at 70 °C

Tm: 8 °C higher Rigidifying flexible regions Animal feeding, pulp bleaching, baking (Wang et al. 2012)

Transglutaminase Streptomyces mobaraensis Directed evolution based on error-prone PCR

E164L Half-life: 1.66-fold at 50 °C Weakened the interactions between the two loop regions adjacent

Food, textile (Liu, Huang et al.

2019) Phospholipase D Streptomyces halstedii Directed evolution based on error-prone PCR

S163F Half-life: 3.04-fold at 50 °C Topt: 10 °C higher

Newly formed salt bridges, stronger hydrophobic interactions

Pharmaceutical, food, cosmetic industries (Huang et al. 2020)

Xylanase pET28a vector Directed evolution based on error-prone PCR and rational design guided by B-factor analysis

L28V/N30S/ K133E/ G172D/ Q14H/A29S/ A203V/N30P/ T31H/A52L

Half-life: 820-fold at 70 °C Newly formed hydrogen bonds

Animal feeding, pulp bleaching, baking (Xing et al. 2021)

Chitinase Paenibacillus pasadenensis Sequence- and structure-based semi-rational design in combination with introduction of disulfide bond

S244C-I139C/ T259P Half-life: 26.3-fold at 50 °C Topt: 7.5 °C higher

Stabilized folding form Agrifood, biological control, medical rehabilitation (Xu, Ni et al. 2020)

Lipase Lip2 Yarrowia lipolytica Directed evolution based on error-prone PCR, semi-rational design based on B-factor iterative test and site-directed mutagenesis

A103S/T117G and T117G/ F237C Half-life: 7-fold at 50 °C

Anchoring the flexible loop region Food, oil, pharmaceuticals, paper, leather, detergent, cosmetics (Wen, Tan, and

Zhao 2012) NR, not reported.

T50 30: Temperature at which the enzyme remained 50% of its activity after 30 min of heat-treatment; Topt: Optimal temperature; Tm: Melting temperature; T50: Temperature at which 50% of the initial activity is retained after 30 min incubation.

Enzymes Microorganisms or Plasmids Strategies Mutants

Results (than wild type) Thermostable mechanisms Applications

References Table 3. (Continued) Critical Reviews in Food Science and Nutrition

11 highly effective for increasing the stability of proteins (Wang et al. 2014). Besides, the comparative analysis of mesophilic and thermophilic alcohol dehydrogenases had revealed that a higher number of conserved proline residues existed in the two most stable enzymes, horse liver alcohol dehydro- genase (HLADH) and Thermoanaerobacter brockii alcohol dehydrogenase (TBADH), and these prolines residues were responsible for the increased thermostability of HLADH and

TBADH by rigidifying the loop regions (Barzegar et al.

2009). Similar result was also obtained to enhance the ther- mostability of luciferase and α-glucosidase by introducing proline to rigidify flexible regions (Zhou, Xue, and Ma 2010;

Yu et al. 2015). The half-life time of the improved luciferase

H489P mutant was 1.4-fold longer than that of wild type, further proving that proline strengthened the overall rigidity of proteins (Yu et al. 2015).

4.1.5.  Based on the folding free energy of protein design

Unfolding free energy is the difference in free energy between the folded state and the unfolded state of the protein. The higher the unfolding free energy, the more energy needed to destroy the higher-level structure of the protein, indicating the more stable the protein. Protein folding free energy is consid- ered as an important characteristic related to the thermal stability of protein (Zhang et al. 2012). Some bioinformatic softwares like FoldX (Guerois, Nielsen, and Serrano 2002;

Schymkowitz et al. 2005) and PoPMuSiC were adopted to predict the effect of protein mutants on the folding free energy based on the protein sequence or three-dimensional structure (Table 2) (Zhang and Wu 2011). By predicting the folding free energy change of amino acid substitutions using PoPMuSiC algorithm, four positive mutants of feruloyl esterase A from

Aspergillus niger, namely S92A, D93G, D174A and S187F, were found to have the most stabilizing effect (Zhang and Wu

2011). Especially, half-life of the double point mutant D93G/

S187F increased by 9.6-fold at 50 °C when compared with that of the wild type (Table 3). By employing the same algorithm, the half-life of the transglutaminase mutant P132I from S. hygroscopicus reached 5.0 min at 50 °C, which was 31% higher than that of the wild type (Tong et al. 2018). The tyrosinase double point mutant R95Y/G123W from S. kathirae increased by 5 °C higher Topt and 1.5-fold half-life at 60 °C when com- pared with that of the wild type (Guo et al. 2017). Moreover, the combining use of FoldX and molecular dynamics simula- tions approaches also significantly enhanced the thermostability of Rhizopus chinensis lipase (Wang et al. 2020). The quadru- plemutation m31 (S142A/D217V/Q239F/S250Y) mutant exhib- ited a half-life at 60 °C 41.7-fold longer, a Topt 5 °C higher and a T50

30 of 15.8 °C higher than that of the wild type r27RCL.

Further analysis revealed that the thermostability mechanism was improved due to the decreased solvent accessible surface area, newly formed salt bridge and increased folding free energy of m31.

4.1.6.  Based on temperature factor design The temperature factor (B-factor) is often used to reflect the conformational state of amino acid residues in the protein (Figure 3). The higher the B-factor value means the more flexibility in the conformation of the corresponding part (Yu and Huang 2014). Sun et al., have comprehensively reviewed the exploitation of B-factors in protein science in terms of the application in interpreting rigidity, flexibility, and internal motion and engineering thermostability (Sun et al. 2019), and declared that B-factor analyses could provide structural and mechanistic insights when combined with other exper- imental and computational techniques. The B-FITTER pro- gram was considered to be effective in predicting the flexible residues and calculating the amino acid B-factor of proteins, but available crystal structure information was required since

B-factor was obtained from X-ray data (Reetz and Carballeira

2007). Using the B-factor-saturation mutagenesis strategy, the half-life of D594Q and G827K/D594Q mutants of α-L-rham- nosidase from A. terreus increased by 2.1- and 2.3-fold, respectively, compared to that of the wild type at 70 °C, which was due to the newly formed hydrogen bonds and salt bridges (Ge et al. 2018). The Tm and half-life at 35 °C of levansucrase mutant E404L increased by 2.8 °C and

12.5-fold to that of wild type, respectively (Xu et al. 2019).

Similarly, according to B-factor analyzed by B-FITTER and folding free energy predicted by PoPMuSiC algorithm, S33 and N92 of type A feruloyl esterase from A. usamii were chosen for further iterative saturation mutagenesis (Yin et al. 2015). The S33E/N92R mutant displayed a Tm 4.7 °C higher and a half-life 3.96-fold longer at 50 °C compared with that of the wild type (Table 3). Moreover, Tm of mutant

R249L lipase B from Candida antarctica increased to 56.8 °C through in silico design after employing B-factor and

RosettaDesign approach (Kim, Le, and Kim 2010).

4.1.7.  Based on the anchoring of unstable regions

Loops and N- and C-termini, the regions with the highest thermal factors in a protein crystal structure (Figure 3), are considered to be closely related to protein stability. Many studies have found that anchoring these regions can enhance the thermal stability of proteins (Ben Ali et al. 2011; Sun et al. 2005; Tang et al. 2017). To improve the thermostability of a mesophilic family 11 xylanase A from A. niger (AnxA), researchers have tried to replace AnxA’s N-terminus with the corresponding region of thermostable xylanase A from

Thermomonospora fusca (TfxA) (Sun et al. 2005). The newly hybrid xylanase ATx was more thermostable than AnxA, and it was similar to that of TfxA, demonstrating the important role of the N-terminus of TfxA in the thermo- stability of ATx. This work has also proved the feasibility of N-terminus replacement to improve the thermal stability of the protein. Thermostability of Trichoderma reesei xylanase

2 (Xyn2) is also reported to be enhanced by introducing disulfide bonds between N-terminus and β-sheet, with

2.5-fold higher half-life at 60 °C (Tang et al. 2017). Likewise,

Tm and half-life time of GH11 xylanase from Thermomyces lanuginosus increased about 8 °C and 20-fold, respectively, after introducing disulfide bond Q1C-Q24C into the

N-terminal region of the enzyme (Wang et al. 2012).

However, most studies have declared that the modification of the N-terminus sometimes decreased the activity of the

12 H. WU ET AL. enzyme (Liu et al. 2015; Sun et al. 2005). Accordingly, the

C-terminal modification might be an alternative to alter the enzyme properties. Coincidently, Li et al., have reported that the thermostability of A. fumigatus Z5 xylanase could be enhanced by introducing a poly-threonine region located in a linker region of the C-terminus between catalytic domain and carbohydrate-binding module domain (Li, Chen et al. 2019).

4.2.  Directed evolution strategy Directed evolution is a very important means of non-rational design to change the properties of proteins, such as thermal stability, substrate specificity and catalytic reaction efficiency (Figure 3). Since proposed in the 1990s, this technology has been significant in protein engineering and has been broadly adopted in the enzyme fields (Chen et al. 1991; Zhang,

Geary, and Simpson 2019). Directed evolution is an accel- erated process that mimics the evolution of enzymes in nature by artificially creating a large number of mutants in vitro. Although directed evolution does not need to a prior understanding of the structure, catalytic mechanism and structure-activity relationship of the enzyme, the successful implementation of this technique requires, firstly to con- struct highly efficient mutant library by random mutagenesis such as error-prone PCR or DNA-shuffling techniques, and secondly to create high-throughput screening (HTS) method based on the chromogenic substrate or fluorescent color or physical and chemical properties of the products (Ladevèze et al. 2013; Liu, Xun, and Feng et al. 2019).

Transglutaminase has been widely used in the food and textile industry due to the cross-linking modification of proteins. To meet industrial requirements, three mutants with enhanced activity and thermostability were obtained from 5700 mutant libraries via directed evolution using two round error-prone PCR, and the E164L mutant of

Streptomyces mobaraensis transglutaminase showed a half-life

1.66-fold longer than that of the wild type at 50 °C (Liu,

Huang et al. 2019). The thermal stability of the mutant lipase (ep-231-51) from B. licheniformis was 13.5-fold higher than that of the wild type (Madan and Mishra 2014).

Besides, an enhancement thermostability S163F mutant of

Streptomyces halstedii phospholipase D was produced from

7700 random mutagenesis clones generated by error-prone

PCR strategy, showing a Topt 10 °C higher and a half-life at

50 °C 3.04-fold longer than that of wild type enzyme (Huang et al. 2020). Although directed evolution can achieve the modification of the thermal stability of protein, this process is labor-intensive and time-consuming. The blind charac- teristic of random mutations will generate a large number of unexpected and useless mutants, which require to be further screened.

4.3.  Semi-rational design strategy Rational design requires an in-depth understanding of

­protein structure and function relationship, whereas directed evolution needs to establish a huge mutant library and HTS methods (Figure 3). The semi-rational design provides a new direction for mutation according to the structural/ sequence-based information and the feasible HTS system because this strategy integrates the advantages of the other two methods (Kapoor, Rafiq, and Sharma 2017). With the aid of bioinformatics and computational predictive algo- rithms, the mutation sites of semi-rational design are con- centrated to one or a few sites, which will be further mutated using random mutation, site-directed mutation or site-directed saturation mutation technology, thereby creating a high-quality and small-scale mutagenesis library (Liu, Xun, and Feng et al. 2019). There are several feasible tools, such as FoldX (Schymkowitz et al. 2005), PoPMuSiC (Dehouck et al. 2009) and MultiMutate (Deutsch and Krishnamoorthy

2007), for predicting changes in protein stability following point mutation.

Xing et al. have employed the directed evolution based on error-prone PCR and rational design guided by B-factor analysis to improve the thermostability of GH11 xylanase (Table 3) (Xing et al. 2021). After conducting two rounds of error-prone PCR, site-directed mutagenesis, site-saturation mutagenesis and B-factor analysis, the mutant Xyn376 (L28V/N30S/K133E/G172D/Q14H/A29S/A203V/N30P/T31H/

A52L) was screened from 30,000 clones in the random mutagenesis library with a half-life of 410 min at 70 °C, which was 820-fold higher than that of the wild type enzyme (Table 3). The chitinase from Paenibacillus pasadenensis was also engineered to improve its thermostability and activity through semi-rational design from sequence- and structure-based strategy analysis (Xu, Ni et al. 2020). The obtained mutant (S244C-I139C/T259P) displayed 26.3-fold longer half-life at 50 °C and a Topt 7.5 °C higher than that of the wild type. Furthermore, the thermostability of lipase

Lip2 from Yarrowia lipolytica was significantly enhanced with a half-life 7-fold longer than that of the wild type using error-prone PCR based on directed evolution and

B-factor iterative test based on semi-rational design and site-directed mutagenesis (Wen, Tan, and Zhao 2012).

5.  Challenges and future perspectives Comparing with chemical catalysts, biocatalysts such as enzymes have unparalleled advantages in terms of catalytic efficiency, substrate specificity and environmental friendli- ness, and are widely used in food, pharmaceutical, textile, bio-refining and feed industries. The high thermostability of enzymes is the prerequisite for industrial application. The ways to obtain highly thermostable enzymes include metag- enomic screening, genome sequencing of extremophiles from extreme environments and employing protein engineering methods to modify available enzymes with poor function.

It is the goal for all biologists and enzyme engineers to optimize and modify proteins’ properties to meet industrial requirements. The developed protein engineering technolo- gies, such as rational design, directed evolution and semi-rational design, have made great progress in protein function modification, and have been widely adopted in the

Critical Reviews in Food Science and Nutrition 13 industrial enzyme fields. There are still many challenges in engineering the properties of enzymes. The rational design based on sequence or structure information of protein requires an in-depth understanding of the structure, function and structure-activity relationship. In most cases, the obtained three-dimensional structure of a target protein is usually provided by homology modeling construction according to primary sequences. Accordingly, obtaining the crystal structure of the target enzyme is an urgent challenge to be overcome. Directed evolution does not rely on the three-dimensional structure of protein, but it requires the construction of a large number of mutant libraries and HTS methods. However, it is relatively difficult to establish a corresponding index correlation between the enzyme’s ther- mal stability and activity. During the screening process, the mutants generally need to be heat-treated in advance and then subject to high-throughput detection of enzyme activity.

Actually, the whole screening process is complex and time-consuming. When performing protein engineering for a specific enzyme, the aforementioned factors should be fully considered, and appropriate molecular modification strategies should be flexibly selected. Fortunately, the devel- opment of hadoop-driven artificial intelligence and compu- tational biology has greatly accelerated protein engineering design. The intelligent computational design of proteins will be a new trend in future development.

Disclosure statement The authors declare that they do not have any actual or potential conflict of interest including any financial, personal or other relation- ships with other people or organizations within five years of beginning the submitted work that could inappropriately influence, or be per- ceived to influence, their work.

Funding This work was funded by National Natural Science Foundation of

China (No. 31801583 and 31922073), the Natural Science Foundation of Jiangsu Province (No. BK20180607), the Key Technology R&D

Program of Jiangsu Province (BE2019629), Tianjin Synthetic

Biotechnology Innovation Capacity Improvement Project (TSBICIP-KJGG-003), and the Key-Area Research and Development

Program of Guangdong Province (2020B020226007).

ORCID Hao Wu http://orcid.org/0000-0002-5532-6564 Wenli Zhang http://orcid.org/0000-0002-7861-0170

Wanmeng Mu http://orcid.org/0000-0001-6597-527X References

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好的,遵照您的指令,我将以OWL的身份,将提供的学术英文段落翻译成中文,并确保技术术语的准确性。

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**获取和使用的完整条款与条件可在以下网址找到:** https://www.tandfonline.com/action/journalInformation?journalCode=bfsn20 **《食品科学与营养学评论》** ISSN: (印刷版) (在线版) 期刊主页: https://www.tandfonline.com/loi/bfsn20 **开发高耐热性工业酶的策略综述:发现、机制、改造与挑战** 吴浩,陈秋明,张文利 & 穆万孟 引用本文:吴浩,陈秋明,张文利 & 穆万孟 (2021): 开发高耐热性工业酶的策略综述:发现、机制、改造与挑战,《食品科学与营养学评论》,DOI: 10.1080/10408398.2021.1970508 链接到本文:https://doi.org/10.1080/10408398.2021.1970508 在线发表:2021年8月26日。 提交您的文章到本期刊 文章浏览:836次 查看相关文章 查看交叉标记数据 综述 《食品科学与营养学评论》 **开发高耐热性工业酶的策略综述:发现、机制、改造与挑战** 吴浩a,陈秋明a,张文利a 和 穆万孟a,b a江南大学食品科学与技术国家重点实验室,中国江苏无锡;b江南大学食品安全国际联合实验室,中国江苏无锡 **摘要** 酶等生物催化剂具有环境友好性和底物特异性,在多种工业产品的生产中备受青睐。然而,工业中严格的反应条件,包括高温、有机溶剂、强酸强碱和其他恶劣环境,常常会使酶不稳定,从而严重影响其催化功能,并极大地限制了其在食品、制药、纺织、生物炼制和饲料工业中的应用。因此,开发具有高耐热性的工业酶在工业中变得非常重要,因为耐热酶在高温下更具优势。利用基因组测序、宏基因组学和从极端环境分离样品来发现新的耐热酶,或利用新兴的蛋白质工程技术对现有耐热性差的酶进行分子改造,已成为获得耐热酶的有效手段。本文以耐热酶作为工业中的生物催化芯片,系统分析了从极端环境中发现耐热酶的方法,阐明了影响酶热稳定性的各种相互作用力,并提出了提高酶耐热性的不同策略。此外,还从结构与活性关系的角度,全面介绍了通过理性设计策略改造工业酶耐热性的最新进展。最后,提出了挑战和未来的研究方向。 1. 引言 作为传统化学催化剂的有效替代,耐热酶已广泛应用于食品、制药、纺织、生物炼制和饲料工业(Han et al. 2019)。一种好的酶通常需要满足工业要求,如高底物特异性、高催化效率和高耐热性,其中酶的热稳定性尤为重要,因为它能抵抗恶劣环境并在高温下维持长期催化(Karnaouri et al. 2019; Suresh et al. 2021)。在工业产品的制备过程中,由于高温具有反应速率更高、微生物污染风险更低等诸多优点,化学反应通常在高温体系中进行(Wu, Zhang, and Mu 2019; Kumar et al. 2019)。酶在长期的生物进化过程中,在活体系统中发挥最佳的生物学活性(Liu, Xun, and Feng et al. 2019)。然而,大多数酶来源于嗜温细菌,耐受性差,严重限制了其广泛的工业应用(Atalah et al. 2019)。因此,获得具有高耐热性的新酶或改造现有的嗜温酶对工业应用具有重要意义。此外,有必要建立一种高效的分子改造方法来提高酶的热稳定性。 从结构和能量角度评估酶的热稳定性,通常使用热力学稳定性和动力学稳定性作为参数。热力学稳定性用于表征蛋白质变性的趋势。在这种情况下,蛋白质结构处于由熵和焓决定的相对稳定的能量状态,变性趋势不是自发的。天然酶通常进化到热力学稳定状态以适应环境温度(Rothschild and Mancinelli 2001)。蛋白质的热力学稳定性通常通过变性自由能(ΔGu)、熔解温度(Tm)和变性平衡常数(Ku)来评估。动力学稳定性是指蛋白质在发生不可逆变化时维持一半活性所需的时间或温度(Polizzi et al. 2007)。动力学稳定性的测量需要在特定条件孵育后检测酶的残余活性。通常,应测量Topt(最适温度)、T50(酶失去一半活性时的温度)、t1/2(酶失去一半活性所需的时间)和kd,obs(观察到的失活速率常数)(Bommarius and Paye 2013)。 © 2021 Taylor & Francis Group, LLC 联系方式:张文利 wenlizhang@jiangnan.edu.cn https://doi.org/10.1080/10408398.2021.1970508 **关键词** 热稳定性;蛋白质工程;工业酶;极端环境;相互作用力 2 H. WU ET AL. 近年来,生物信息学和测序技术的发展促进了新的酶编码序列的发现(Wang, Nie, and Xu 2019)。越来越多的耐热酶从超嗜热和嗜热菌株中分离或克隆出来。研究发现,耐热酶与嗜温酶的序列相似性可达约40%–85%(Vieille and Zeikus 2001),而它们的三级结构也高度相似,催化机制相同,表明存在其他影响酶热稳定性的机制和因素。大量研究表明,酶的氨基酸残基之间存在多种相互作用力,包括疏水相互作用、盐桥、芳香环相互作用、二硫键和氢键,这些相互作用力在维持酶的构象稳定性方面起着非常重要的作用。此外,具有较好热稳定性的酶往往具有更稳定的构象,例如更高的刚性、更高的堆积效率、更低的去折叠熵和α-螺旋稳定性(Vieille and Zeikus 2001)。更高的热稳定性使酶在工业应用中更具竞争力和吸引力。 在过去的几十年里,人们通过两种主要方式不断努力获得具有所需高耐热性的工业酶。一种方式是从极端环境中筛选超嗜热和嗜热生物(图1)。然而,这一筛选过程复杂且繁琐,且酶活性相对较低。另一种方式是通过先进的蛋白质工程策略,如理性设计、半理性设计、定向进化和从头设计,提高来源于嗜温生物的现有工业酶的热稳定性(Liu, Xun, and Feng et al. 2019)。此外,酶工程的计算工具被广泛用于辅助这一过程,以更好地理解工业酶的热稳定性机制(Chen et al. 2020)。然而,理性设计需要对酶的结构、功能和催化机制之间的关系有全面的了解。半理性设计涉及基于序列、结构或计算模型的突变,然后进行小规模突变和筛选方法(Zhang, Geary, and Simpson 2019)。定向进化需要构建大型突变文库和高效的高通量筛选(HTS)方法。从头蛋白质设计探索完整的序列空间,由蛋白质折叠的物理原理指导(Huang, Boyken, and Baker 2016)。 本综述系统总结了食品、制药、纺织、生物炼制和饲料工业中应用的工业酶热稳定性方面的一些成就。详细讨论了影响酶热稳定性的机制和因素。然后,提出了开发高耐热性酶的策略,包括如何获得酶以及如何通过先进的蛋白质工程技术改造热稳定性弱的现有酶的分子结构。还分析了通过理性设计提高酶热稳定性的成熟方法。 2. 影响蛋白质热稳定性的因素 2.1. 氢键 氢键是蛋白质结构中一种重要的非共价相互作用,它不仅存在于蛋白质内部的氨基酸残基之间,也表现在蛋白质与周围水分子的相互作用中(图2)。这是因为蛋白质内部和周围的水分子之间存在许多氢供体和氢受体。通常,氢供体和氢受体之间的距离不超过3 Å,角度小于90度。蛋白质中每对氢键提供的能量约为0.6 kcal/mol(Li, Zhou, and Lu 2005)。Vogt等人通过比较不同蛋白质家族的各自极性原子分数表面积,发现蛋白质的热稳定性与氢键的数量密切相关(Vogt, Woell, and Argos 1997)。Vieira等人通过分子动力学模拟研究了两种结构相似的11家族木聚糖酶,BCX(来自环状芽孢杆菌的嗜温木聚糖酶)和TLX(来自嗜热真菌的嗜热木聚糖酶),并证明了分子内氢键和盐桥是维持高温下骨架刚性的关键因素(Vieira and Degrève 2009)。后来的研究再次证实了耐热酶比嗜温酶具有更多的氢键(Tompa, Gromiha, and Saraboji 2016)。此外,Ishak等人发现,来自Geobacillus zalihae的重组脂肪酶突变体D43E和E226D的熔解温度(Tm)分别提高到76 °C和77.4 °C,而野生型酶为70.9 °C(Ishak et al. 2020)。对G. zalihae脂肪酶突变体D43E和E226D的进一步结构研究表明,脂肪酶稳定性的提高归因于额外的氢键和离子对相互作用。有趣的是,在界面区域引入链间氢键也有助于提高来自Dorea sp. CAG317的D-阿洛酮糖3-差向异构酶的热稳定性和结构稳定性,其Tm比野生型提高了17.54 °C(Zhang et al. 2018)。 2.2. 盐桥 盐桥是由带相反电荷的氨基酸残基之间的静电吸引形成的(图2)。作为在高温下维持蛋白质结构热稳定性的驱动力,盐桥经常出现在蛋白质表面(Xu, Cen et al. 2020)。嗜热蛋白质在高温下往往比同源的嗜温蛋白质具有更多的表面盐桥(de Bakker, Hünenberger, and McCammon 1999; Szilágyi and Závodszky 2000)。此外,盐桥被认为是嗜热蛋白质中比氢键更重要的因素。分子动力学模拟结果表明,高温会导致盐桥收紧,从而增加蛋白质内相互作用能,这也解释了为什么盐桥可能在高温下而不是在室温下稳定超嗜热蛋白质。另一个原因是,在室温下,两个带电残基形成盐桥时产生的大溶剂化惩罚不能通过蛋白质内相互作用来补偿(Szilágyi and Závodszky 2000)。因此,引入理想的盐桥仍然是一项非常困难的任务,有时它会导致蛋白质的轻微稳定或不稳定。此外,Szilágyi和Závodszky编制了一个非冗余数据集,包含嗜热蛋白质及其嗜温同源物的高质量结构,以总结蛋白质热稳定性的总体演变(Szilágyi and Závodszky 2000)。结果发现,盐桥的数量是影响蛋白质稳定性的一个重要因素,嗜热蛋白质中的盐桥数量高于嗜温蛋白质。为了提高来自Geobacillus thermoglucosidans的1,4-α-葡聚糖分支酶(GtGBE)的热稳定性,Ban等人将额外的局部盐桥引入GtGBE,结果表明,五个单独引入的突变体,即Q231R-D227、Q231K-D227、T339E-K335、T339D-K335和I571D-R569,其半衰期比野生型长17%至51%(Ban et al. 2020)。进一步的圆二色性和内在荧光实验表明,GtGBE突变体热稳定性的提高可能归因于新形成的盐桥网络中增强的刚性。Chan等人通过研究成对相互作用能和ΔCp(变性的热容变化),研究了盐桥如何影响蛋白质稳定性(Chan et al. 2011),结果表明,额外的盐桥通过降低ΔCp来增强蛋白质的热稳定性,这将使蛋白质稳定性曲线升高和变宽。 2.3. 疏水相互作用 许多研究证实,疏水相互作用在维持蛋白质稳定性和形成蛋白质三级结构中起着重要作用,其中疏水环境是与盐桥和氢键等其他相互作用相比,影响嗜热蛋白质稳定性的主要因素。疏水性含量也被提出可作为区分嗜温蛋白质和嗜温蛋白质的信息指标(Modarres, Mofrad, and Sanati-Nezhad 2016)。Gromiha等人基于373个蛋白质家族的数据集发现,80%的嗜热蛋白质比嗜温蛋白质具有更高的疏水性(Gromiha et al. 2013)。这种相互作用力主要是由于疏水氨基酸侧链的聚集,本能地排斥与水的接触(Folch, Rooman, and Dehouck 2008)。因此,水溶液中的疏水氨基酸(非极性氨基酸)通常被包裹在蛋白质内部,形成疏水核心,而极性氨基酸则分布在蛋白质表面的亲水环境中。据报道,当每个额外的-CH2-基团被包裹在蛋白质中时,稳定的蛋白质可以获得1.3 ± 0.5 kcal/mol的能量(图2)(Pace 1992)。通过将甲基引入大肠杆菌核糖核酸酶H1的疏水核心,Ishikawa等人成功地实现了该酶的热稳定性(Ishikawa et al. 1993)。这可以用后来的研究结果来解释,即在耐热蛋白质中,更多的疏水相互作用会使变性速率变慢(Okada et al. 2010)。相关文献报道,来自Rhodopirellula baltica的D-阿洛酮糖3-差向异构酶在L144F位点定向突变后,其热稳定性得到提高,Δt1/2为50.4 min,ΔTm为12.6 °C,ΔT50 60为22 °C(Mao et al. 2020)。进一步的结构分析表明,突变蛋白质中产生了新的疏水相互作用。在来自土曲霉的(R)-选择性胺转氨酶的双点突变体T130M/E133F中也观察到类似的结果,其在40 °C下的t1/2是野生型的3.3倍,T1/2 10 min热稳定性比野生型高5 °C,这是由于新形成的疏水相互作用和氢键(Huang, Xie, and Feng 2017)。此外,当使用易错PCR和基于B因子的理性设计时,来自GH 11家族的最佳变体Xyn376的热稳定性在70 °C下表现出比野生型酶高820倍的半衰期(Xing et al. 2021)。结构分析表明,氢键和疏水相互作用是提高热稳定性的主要作用力。 2.4. 芳香环相互作用 芳香环相互作用也是蛋白质热稳定性的重要驱动力,主要包括阳离子(带正电荷的氨基酸,如赖氨酸、精氨酸和质子化的组氨酸)与芳香环(阳离子-π)的相互作用,或芳香-芳香相互作用(π-π)。阳离子-π相互作用是一种普遍的、强的非共价结合力,提供的能量是盐桥的两倍(Chakravarty and Varadarajan 2002; Dougherty 2007)。芳香环氨基酸(色氨酸、酪氨酸和苯丙氨酸)的相互作用主要发生在苯基环中心之间的距离小于7.0 Å时(图2)。当两个芳香环的优先距离为5.5 Å时,π-π相互作用通常以0.6–1.3 kcal/mol的能量稳定蛋白质分子(Ohmura et al. 2001)。然而,当芳香环的取向为偏移堆叠或边对面时,芳香相互作用就会发生,这给设计芳香相互作用带来了一些挑战。为了系统地阐明芳香相互作用对蛋白质热稳定性的贡献,Kannan等人研究了24个蛋白质家族的数据集,这些家族具有来自嗜热和嗜温同源物的已知晶体结构,发现17个嗜热蛋白质家族比相应的嗜温同源物具有额外的芳香簇或位于蛋白质表面的扩增芳香网络(Kannan and Vishveshwara 2000)。Yoneda等人揭示了B. smithii吲哚还原酶的较高热稳定性是由于亚基间的芳香相互作用(F105-F172′和F172和F105′),并且F105在这些芳香相互作用中起主导作用(Yoneda et al. 2020)。在嗜温11家族木聚糖酶的N端部分添加Y11-Y16的额外芳香相互作用,可以提高其稳定性,Tm增加9 °C,表明在适当位置添加π-π相互作用可以提高蛋白质的热稳定性(Georis et al. 2000)。最近的一项研究宣布,通过易错PCR构建的腈水解酶突变体AcN-T201F和AcN-T201W的半衰期分别比野生型AcN长13.5倍和10.8倍(Xu et al. 2018)。分子模型表明,腈水解酶突变体的W201或F201残基不仅提高了二聚体界面的稳定性,还与W165残基形成π-π相互作用以稳定底物结合口袋,间接增强了热稳定性。 2.5. 二硫键 二硫键在氨基酸残基半胱氨酸(Cys)之间形成,其α碳原子在空间中的距离范围为4至9 Å(图2)。这个过程是依赖于蛋白质构象的翻译后修饰之一,需要特定的氧化还原环境和伴侣蛋白(Creighton 1984)。二硫键作为共价相互作用,通过降低构象熵来稳定蛋白质结构,在蛋白质的折叠和活性中起着至关重要的作用。与氢键、盐桥、疏水相互作用和芳香相互作用等非共价相互作用力相比,二硫键为蛋白质稳定性提供了最大的能量。据报道,形成二硫键的半胱氨酸之间的平均距离为15个残基,如果假设对折叠形式的影响可以忽略不计,则可以提供3.0 kcal/mol的能量(Kazlauskas 2018)。然而,构建二硫键需要考虑许多因素。为了找出可能影响二硫键成功构建的因素,Dani等人通过计算MODIP程序重新评估和细化了蛋白质中二硫键建模的自动化程序(Dani, Ramakrishnan, and Varadarajan 2003),发现稳定的二硫键与适当的立体化学、较低的深度区域、相对较高的流动性(较高的B因子)和较长的环长度(25-75个残基)有关。为了有效地提高蛋白质稳定性和改变功能特性,Craig和Dombkowski开发了一个名为Disulfide by Design (DbD)的软件和一个可访问的Web服务器托管站点(http://cptweb.cpt.wayne.edu/DbD2/),以辅助预测如果突变为半胱氨酸可能形成二硫键的残基对(Craig and Dombkowski 2013)。与包括氢键和疏水作用力在内的其他非共价相互作用力相比,借助计算程序和软件设计二硫键似乎是一种更方便、更简单的方法。然而,二硫键的形成和正确折叠也充满了不确定性,因为氧化还原不稳定性不适合在还原环境中发挥作用的酶。 大量研究通过引入二硫键来提高酶的热稳定性(Vasudevan et al. 2019)。最近的一项研究通过DbD v2.05程序结合同源模型分析,成功地提高了来自B. licheniformis WHU的植酸酶的热稳定性,其突变体G197C/A358C在60 °C下的半衰期是野生型酶的3.8倍(Zhang et al. 2020)。分子动力学结果表明,该G197C/A358C突变体的热稳定性机制可能是新形成的二硫键锚定了植酸酶的C端并增强了局部堆积刚性。在Tang等人的研究中,使用定点突变在Xyn2的N端和α-螺旋到β-折叠核心之间分别构建了两个二硫键,即Xyn2C14–52和Xyn2C59–149,结果在60 °C下的半衰期比野生型Xyn2长2.5倍和1.8倍(Tang et al. 2017)。新形成的二硫键通过防止结构展开,有效地稳定了Xyn2结构,这可能是热稳定性提高的机制。Li等人改造了不同的区域多个二硫键,以提高来自Yarrowia lipolytica的脂肪酶的热稳定性(Li, Zhang et al. 2019)。六重突变体6 s显示,Tm和T50 15(在15分钟内活性损失一半的温度)分别提高了22.53 °C和31.23 °C,这是由于引入额外的二硫键后酶结构更加刚性化和更长的变性时间。 2.6. 蛋白质包装效率 蛋白质包装效率与蛋白质的热稳定性有关,定义为蛋白质表面的疏水性表面积与总表面积之比(Vieille and Zeikus 2001)(图2)。Karshikoff等人分析了80种非同源嗜温蛋白质、20种嗜热蛋白质和4种超嗜热蛋白质的结构,发现嗜热蛋白质通常具有更高的蛋白质包装效率(Karshikoff and Ladenstein 1998)。内部堆积效果的改善有效地增强了蛋白质稳定性,因为埋藏空腔的增加会破坏蛋白质结构(Eriksson et al. 1992; Xu et al. 1998)。Abraham等人选择了B. subtilis脂肪酶A中暴露率低于5%且包装值低于0.55的43个残基作为第一轮突变候选者,发现没有水接触的包装较差的残基是提高热稳定性的良好靶点(Abraham et al. 2005)。基于甘氨酸突变为丙氨酸和丙氨酸突变为缬氨酸的策略,获得了六个突变体,即A38V、A75V、G80A、A105V、A146V和G172A,其热稳定性高于野生型。其中,A38V、G80A和G172A突变体的半衰期比野生型脂肪酶A增加了64至70倍。一项研究还表明,通过将表面的疏水氨基酸改变为亲水氨基酸来降低黄素蛋白的疏水性表面积,可以显著提高蛋白质的热稳定性(Ayuso-Tejedor, Abián, and Sancho 2011)。 3. 发现具有高耐热性的天然酶 人们认为,酶的特性与宿主所处的环境密切相关,这是由于长期的生物进化(Ueno, Ibarra, and Gojobori 2016)。因此,可以合理地认为,在高温环境中生长的微生物可能分泌具有良好热稳定性的酶(表1)。先前的研究表明,在极端条件下生存的极端微生物可以分泌具有多种特性的新型酶,这些酶可应用于化学、食品和制药工业。因此,极端微生物受到了广泛的研究关注(Chettri et al. 2021; Herbert 1992; van den Burg 2003; Verma, Meghwanshi, and Kumar 2021),并且可以通过来自极端微生物(如超嗜热菌或嗜热菌)的新型蛋白质获得耐热酶(图1)。 目前,只有一小部分能够抵抗极端高温的微生物被报道,其中大多数属于古菌。许多在极端条件下生长的现有微生物,如深海、温泉环境,在实验室环境中难以培养,这使得通过发酵技术生产极端微生物来源的酶变得不可行。尽管如此,基因组测序、分子生物学和宏基因组学的发展加速了酶的基因挖掘、发现和鉴定,例如木聚糖酶(Chadha et al. 2019; Ferrer et al. 2016; Lorenz and Eck 2005; Mhiri et al. 2020; Patel et al. 2019)。此外,许多质粒载体和成熟的表达系统使得来源于极端微生物的酶可以在易于在实验室培养的嗜温宿主中克隆和表达,并具备成熟的分子生物学技术。此外,许多原核系统,如大肠杆菌、芽孢杆菌、乳杆菌,以及真核系统,如毕赤酵母、酿酒酵母和念珠菌,已被开发为可选的表达宿主,用于生产不同来源的酶(Peng et al. 2021)。例如,来自Thermoprotei古菌的D-木糖异构酶和来自Thermococcus litoralis的L-氨基酰化酶都已在大肠杆菌宿主中成功克隆、表达和表征(Toogood et al. 2002; Wu et al. 2020)。来自极端嗜热嗜酸古菌Sulfolobus solfataricus的β-糖苷酶已在酵母系统中表达(D’Auria et al. 1996)。幸运的是,在这些表达系统中表达的大多数超嗜热酶保留了所有天然酶的生化特性,包括正确的折叠和热稳定性(Ebaid et al. 2019; Grättinger et al. 1998; Shi et al. 2019; Vieille and Zeikus 2001)。 4. 开发耐热酶的蛋白质工程策略 4.1. 理性设计 近年来,随着生物信息学和结构生物学的快速发展,理性设计策略已成为改变蛋白质特性的重要手段(表2)。一个实用的理性设计是基于对蛋白质结构、功能和结构与活性关系的全面理解,然后通过选择性替换、插入或截短对蛋白质的特定位点进行有目的的改造,并进一步实验分析设计蛋白质的性质变化。然而,理性设计的应用范围 表1. 用于发现具有高耐热性的天然酶的不同策略。 微生物 来源 微生物 Topt (°C) 方法 生产 酶 Topt (°C) 耐热能力