The Oral Inactivated Porcine Epidemic Diarrhea Virus Presenting in the Intestine Induces Mucosal Immunity in Mice with Alginate–Chitosan Microcapsules

✅ 全文

口服灭活猪流行性腹泻病毒经肠递送海藻酸钠-壳聚糖微囊在小鼠中诱导黏膜免疫的研究

作者 Ziliang Qin; Zida Nai; Gang Li; Xinmiao He; Wentao Wang; Jiqiao Xia; Wang Chao; Lu Li; Xinpeng Jiang; Di Liu 期刊 Animals 发表日期 2023 卷/期/页码 Vol. 13(5) ISSN 2076-2615 DOI 10.3390/ani13050889 类型 原创研究 (Original Research)

📄 中文摘要 Chinese Abstract

中文
猪流行性腹泻病毒(PEDV)是一种高度传染性疾病,主要感染出生后7天内仔猪的小肠上皮细胞,三日龄仔猪的死亡率高达70%至100%。通过肌肉或皮下途径接种灭活疫苗或减毒疫苗诱导的母体抗体,在到达肠道前常被胃酸和胃蛋白酶消化,无法提供有效保护。黏膜免疫,特别是分泌型IgA(sIgA),比全身免疫对肠道感染提供更有效的保护。然而,如何将灭活的PEDV运送至肠道以激活黏膜免疫仍是一个未解决的难题。本研究探索了海藻酸-壳聚糖微胶囊作为口服疫苗递送系统的应用,以保护病毒免受胃部降解,并在肠道中释放以刺激小鼠的黏膜免疫应答。

📋 英文结构化总结 English Structured Summary

全文整理

EN

Background:

Porcine epidemic diarrhea virus (PEDV) is a highly contagious disease that infects the small intestinal epithelial cells of piglets during the first seven days of birth, with mortality rates ranging from 70% to 100% in three-day-old piglets. Maternal antibodies induced by inactivated or attenuated vaccines through intramuscular or subcutaneous routes are often digested by gastric acid and pepsin before reaching the intestine, failing to provide effective protection. Mucosal immunity, particularly secretory IgA (sIgA), provides more effective protection against intestinal infections than systemic immunity. However, the challenge of transporting inactivated PEDV into the intestine to activate mucosal immunity remains unsolved. This study explores the use of alginate–chitosan microcapsules as an oral vaccine delivery system to protect the virus from gastric degradation and release it in the gut to stimulate mucosal immune responses in mice.

Methods:

Inactivated PEDV was encapsulated in sodium alginate–chitosan microcapsules using ionic gelation. The microcapsules were characterized for encapsulation efficiency, protein content, and in vitro release in different saline solutions (PBS, normal saline, and hydrochloric acid) and storage tolerance at room temperature. SPF mice were divided into five groups and immunized orally with PBS, empty microcapsules, inactivated PEDV, low-dose PEDV microcapsules (6 × 10^6 PFU), or high-dose PEDV microcapsules (6 × 10^7 PFU). Serum, feces, and intestinal lavage samples were collected to measure specific IgG and IgA levels by ELISA. Neutralization assays were performed using Vero cells. T-cell proliferation, flow cytometry for dendritic cells (CD11b+, CD11c+) and B cells (B220+, CD23+), and cytokine expression (IFN-γ, IL-4, IL-1, TNF-α, IL-17, IL-10, TGF-β) were analyzed.

Results:

The microcapsules showed excellent release profiles in saline solutions (>50% release within 3 days) and acid stability, with 63.2% release in hydrochloric acid after 18 days. Storage tolerance was maintained for up to 5 months at room temperature. Both low- and high-dose PEDV microcapsule groups significantly increased specific IgA and IgG levels in serum and intestinal mucus compared to the inactivated PEDV group, in a dose-dependent manner. Neutralization assays confirmed that IgG and IgA from microcapsule groups effectively neutralized PEDV in Vero cells, with 50% neutralization titers of 1:256 (IgG) and 1:64 (IgA) for the high-dose group. T-cell proliferation indicated immune memory stimulation. Flow cytometry revealed enhanced differentiation of CD11b+ and CD11c+ dendritic cells and B220+ CD23+ B cells in microcapsule groups. Cytokine analysis showed increased anti-inflammatory cytokines (IL-10, TGF-β) and decreased pro-inflammatory cytokines (IL-1, TNF-α, IL-17) in microcapsule groups compared to the inactivated PEDV group.

Data Summary:

The microcapsule release rate reached 95% in PBS and 91% in normal saline after 18 days, but only 63.2% in hydrochloric acid. Storage stability remained above 83% release for the first 3 months and 41% at 15 months. Specific IgA levels in intestinal lavage were significantly higher in microcapsule groups (p < 0.05 on day 3; p < 0.01 on days 6 and 9). IgG levels in serum followed a similar trend. Neutralization titers for the high-dose microcapsule group were 1:256 (IgG) and 1:64 (IgA), compared to 1:128 (IgG) and 1:32 (IgA) for the low-dose group. Dendritic cell markers (CD11c+) increased from 4.3% (PBS) to 34.6% (high-dose microcapsules). B cell markers (B220+ CD23+) were elevated in microcapsule groups (45–47.7%) compared to inactivated PEDV (46.6%).

Conclusions:

Alginate–chitosan microcapsules effectively protect inactivated PEDV from gastric degradation and release it in the gut, stimulating both mucosal and systemic immune responses in mice. The microcapsules act as an oral adjuvant, enhancing dendritic cell and B cell differentiation, promoting anti-inflammatory cytokine expression, and inhibiting pro-inflammatory responses. This study demonstrates the potential of microencapsulation as an oral vaccine delivery system for PEDV, providing a reference for future research in pigs.

Practical Significance:

This research offers a promising strategy for developing oral vaccines against PEDV, which could improve protection in piglets by inducing mucosal immunity at the site of infection. The microcapsule system’s stability, low cost, and ease of production make it a practical candidate for large-scale application in swine farming, potentially reducing economic losses from PEDV outbreaks.

📋 中文结构化总结 Chinese Structured Summary

中文

背景:

猪流行性腹泻病毒(PEDV)是一种高度传染性疾病,主要感染出生后7天内仔猪的小肠上皮细胞,三日龄仔猪的死亡率高达70%至100%。通过肌肉或皮下途径接种灭活疫苗或减毒疫苗诱导的母体抗体,在到达肠道前常被胃酸和胃蛋白酶消化,无法提供有效保护。黏膜免疫,特别是分泌型IgA(sIgA),比全身免疫对肠道感染提供更有效的保护。然而,如何将灭活的PEDV运送至肠道以激活黏膜免疫仍是一个未解决的难题。本研究探索了海藻酸-壳聚糖微胶囊作为口服疫苗递送系统的应用,以保护病毒免受胃部降解,并在肠道中释放以刺激小鼠的黏膜免疫应答。

方法:

采用离子凝胶法将灭活的PEDV包封于海藻酸钠-壳聚糖微胶囊中。对微胶囊的包封率、蛋白含量以及在不同盐溶液(PBS、生理盐水和盐酸)中的体外释放特性和室温储存耐受性进行表征。将SPF级小鼠分为五组,分别口服PBS、空微胶囊、灭活PEDV、低剂量PEDV微胶囊(6×10^6 PFU)或高剂量PEDV微胶囊(6×10^7 PFU)。采集血清、粪便和肠灌洗液样本,通过ELISA检测特异性IgG和IgA水平。使用Vero细胞进行中和试验。分析T细胞增殖、树突状细胞(CD11b+、CD11c+)和B细胞(B220+、CD23+)的流式细胞术检测以及细胞因子表达(IFN-γ、IL-4、IL-1、TNF-α、IL-17、IL-10、TGF-β)。

结果:

微胶囊在盐溶液中表现出优异的释放特性(3天内释放率>50%),在酸性条件下稳定性良好,在盐酸中18天后释放率为63.2%。室温储存耐受性可维持长达5个月。与灭活PEDV组相比,低剂量和高剂量PEDV微胶囊组血清和肠黏液中特异性IgA和IgG水平均显著升高,且呈剂量依赖性。中和试验证实,微胶囊组的IgG和IgA能有效中和Vero细胞中的PEDV,高剂量组的50%中和滴度分别为IgG 1:256和IgA 1:64。T细胞增殖表明免疫记忆被激活。流式细胞术显示微胶囊组CD11b+和CD11c+树突状细胞以及B220+ CD23+ B细胞的分化增强。细胞因子分析显示,与灭活PEDV组相比,微胶囊组抗炎细胞因子(IL-10、TGF-β)升高,促炎细胞因子(IL-1、TNF-α、IL-17)降低。

数据总结:

微胶囊在PBS中18天后的释放率达到95%,在生理盐水中为91%,而在盐酸中仅为63.2%。储存稳定性在前3个月保持在83%以上释放率,15个月时为41%。肠灌洗液中特异性IgA水平在微胶囊组显著更高(第3天p<0.05;第6天和第9天p<0.01)。血清中IgG水平呈现相似趋势。高剂量微胶囊组的中和滴度为IgG 1:256和IgA 1:64,而低剂量组为IgG 1:128和IgA 1:32。树突状细胞标志物(CD11c+)从PBS组的4.3%增加到高剂量微胶囊组的34.6%。B细胞标志物(B220+ CD23+)在微胶囊组中升高(45%-47.7%),而灭活PEDV组为46.6%。

结论:

海藻酸-壳聚糖微胶囊能有效保护灭活的PEDV免受胃部降解,并在肠道中释放,刺激小鼠的黏膜和全身免疫应答。微胶囊作为口服佐剂,增强树突状细胞和B细胞分化,促进抗炎细胞因子表达,并抑制促炎反应。本研究证明了微胶囊化作为PEDV口服疫苗递送系统的潜力,为未来在猪中的研究提供了参考。

实际意义:

本研究为开发针对PEDV的口服疫苗提供了有前景的策略,通过在感染部位诱导黏膜免疫来提高对仔猪的保护效果。微胶囊系统的稳定性、低成本和易于生产的特点使其成为养猪业大规模应用的实用候选方案,有望减少PEDV暴发造成的经济损失。

📖 英文全文 English Full Text

EN

pmc Animals (Basel) Animals (Basel) 2763 animals animals Animals : an Open Access Journal from MDPI 2076-2615 Multidisciplinary Digital Publishing Institute (MDPI) PMC10000104 PMC10000104.1 10000104 10000104 36899746 10.3390/ani13050889 animals-13-00889 1 Article The Oral Inactivated Porcine Epidemic Diarrhea Virus Presenting in the Intestine Induces Mucosal Immunity in Mice with Alginate–Chitosan Microcapsules Qin Ziliang Formal analysis Data curation 1 † Nai Zida Writing – original draft 1 † Li Gang Formal analysis 1 He Xinmiao Resources 2 Wang Wentao Methodology 2 Xia Jiqiao Formal analysis 1 Chao Wang Formal analysis 2 Li Lu 2 https://orcid.org/0000-0003-1128-2157 Jiang Xinpeng Writing – original draft Writing – review & editing 1 * Liu Di Data curation 2 * Wang Yue Academic Editor 1 College of Animal Science and Technology, Northeast Agricultural University, Harbin 150030, China 2 Key Laboratory of Combining Farming and Animal Husbandry, Ministry of Agriculture, Animal Husbandry Research Institute, Heilongjiang Academy of Agricultural Sciences, No. 368 Xuefu Road, Harbin 150086, China * Correspondence: jiangxinpeng@neau.edu.cn (X.J.); liudi1963@163.com (D.L.); Tel.: +86-451-55190722 (X.J. & D.L.) † Co-first authors. 28 2 2023 3 2023 13 5 430977 889 01 12 2022 20 2 2023 21 2 2023 28 02 2023 11 03 2023 02 05 2024 © 2023 by the authors. 2023 https://creativecommons.org/licenses/by/4.0/ Licensee MDPI, Basel, Switzerland. This article is an open access article distributed under the terms and conditions of the Creative Commons Attribution (CC BY) license ( https://creativecommons.org/licenses/by/4.0/ ). Simple Summary Porcine epidemic diarrhea virus (PEDV) is an α coronavirus that causes major disease outbreaks, producing up to 100% mortality rates in piglets during the first 7 days after birth. In this study, we used microcapsules with inactivated PEDV fed to mice by oral administration to improve the effectiveness of the oral delivery method for protection against PEDV infection, and avoided digestive degradation in the acidic environment of the stomach. In addition, the PEDV microcapsules displayed remarkable storage tolerance to maintain the quality of the PEDV antigen. The PEDV microcapsules delivered the inactivated virus into the gut, stimulating the specific mucosal immune response in mice, which could directly neutralize the enterovirus. Abstract The porcine epidemic diarrhea virus, PEDV, which causes diarrhea, vomiting and death in piglets, causes huge economic losses. Therefore, understanding how to induce mucosal immune responses in piglets is essential in the mechanism and application against PEDV infection with mucosal immunity. A method of treatment in our research was used to make an oral vaccine that packaged the inactive PEDV with microencapsulation, which consisted of sodium alginate and chitosan, and adapted the condition of the gut in mice. The in vitro release experiment of microcapsules showed that inactive PEDV was not only easily released in saline and acid solutions but also had an excellent storage tolerance, and was suitable for use as an oral vaccine. Interestingly, both experimental groups with different doses of inactive virus enhanced the secretion of specific antibodies in the serum and intestinal mucus, which caused the effective neutralization against PEDV in the Vero cell by both IgG and IgA, respectively. Moreover, the microencapsulation could stimulate the differentiation of CD11b+ and CD11c+ dendritic cells, which means that the microencapsulation was also identified as an oral adjuvant to help phagocytosis of dendritic cells in mice. Flow cytometry revealed that the B220 + and CD23 + of the B cells could significantly increase antibody production with the stimulation from the antigens’ PEDV groups, and the microencapsulation could also increase the cell viability of B cells, stimulating the secretion of antibodies such as IgG and IgA in mice. In addition, the microencapsulation promoted the expression of anti-inflammatory cytokines, such as IL-10 and TGF-β. Moreover, proinflammatory cytokines, such as IL-1, TNF-α, and IL-17, were inhibited by alginate and chitosan in the microencapsulation groups compared with the inactivated PEDV group. Taken together, our results demonstrate that the microparticle could play the role of mucosal adjuvant, and release inactivated PEDV in the gut, which can effectively stimulate mucosal and systemic immune responses in mice. microcapsules PEDV mucosal immunity alginate chitosan National Natural Science Foundation of China 31902169 Heilongjiang Province Science Fund for Excellent Young Scholars YQ2020C008 Young Talents” Project of Northeast Agricultural University 18QC39 This work was supported by the National Natural Science Foundation of China (Grant number:31902169), the Heilongjiang Province Science Fund for Excellent Young Scholars (Grant number: YQ2020C008), Young Talents” Project of Northeast Agricultural University (Grant number: 18QC39. pmc-status-qastatus 0 pmc-status-live yes pmc-status-embargo no pmc-status-released yes pmc-prop-open-access yes pmc-prop-olf no pmc-prop-manuscript no pmc-prop-legally-suppressed no pmc-prop-has-pdf yes pmc-prop-has-supplement yes pmc-prop-pdf-only no pmc-prop-suppress-copyright no pmc-prop-is-real-version no pmc-prop-is-scanned-article no pmc-prop-preprint no pmc-prop-in-epmc yes pmc-license-ref CC BY 1. Introduction Porcine epidemic diarrhea virus, PEDV, is a highly contagious disease that infects the small intestinal epithelial cells of piglets during the first seven days of birth, and the mortality rate can range from 70% to 100% in three-day-old piglets [ 1 ]. At the first week of birth, the major immune protection of piglets is dependent on maternal antibodies and innate immunity. The maternal antibody is induced by the inactivated and attenuated vaccines of PEDV through the intramuscular route or subcutaneous injection in the pregnant sow, but the maternal antibody is digested by gastric acid and pepsin before entering the intestine, which cannot effectively protect against PEDV infection. However, mucosal immunity can be built no more than three days after birth, and provides more effective protection than systemic immunity in piglets. Some studies have demonstrated that the first line of defense by IgA in the intestine would be more effective than that by IgG for neutralizing the infection of intestinal diseases [ 2 ]. However, the problem of how to transport the inactivated PEDV virus into the intestine and activate mucosal immunity has not yet been solved. Moreover, the mechanism of mucosal immunity to PEDV in the gut of fetal pigs remains unclear. The process of specialized M-cells taking up and presenting PEDV to the dendritic cells and lymphoid follicles also needs to be better understood to learn how antigens arrive at the inductive sites for T-cell- and B-cell-dependent activation of IgG and IgA production. One interesting strategy is packaging vaccines to look like microcapsules, which have different properties for oral immunity, such as size, shape, and surface molecule organization [ 3 ]. Chitosan and alginate are mixed to coagulate the ionic gel, which is a potential candidate vehicle for their main constituents due to their intrinsic immunomodulatory properties. Alginate is one of the most widely used carriers for the controlled release of different types of active agents. Moreover, sodium alginate, which is derived from marine brown algae and bacteria, has received attention as an antimicrobial in the food industry because of its unique physicochemical properties and biological activity. Chitosan (CS), also called poly glucosamine, is widely used to enhance the mucosal immune response due to its biocompatibility, biodegradability, and mucoadhesive properties [ 4 ]. The production method of alginate–chitosan microcapsules by using ionic gelation is an interesting approach to compound oral delivery systems for inactivated PEDV vaccines. The classic technique involves first mixing the antigen of inactivated PEDV and alginate solution and then pouring it slowly into a solution of calcium chloride and chitosan. Finally, the alginate microcapsules are collected by decanting the supernatant and are washed with water. Hence, the preparation method of PEDV alginate microcapsules is very simple. The manufacture of microencapsulations showed that they used simple machinery, had a low cost, and a good safety profile, making them an attractive approach to oral immunization. In a previous study of the mucosal immune system, oral vaccination with recombinant Lactobacillus was more promising for stimulating specific immunization against pathogens in the first contact with mucosal surfaces [ 5 , 6 , 7 ]. To improve the effectiveness of the oral vaccination delivery method, which protects against PEDV infection, avoiding digestive degradation in the acidic environment of the stomach is crucial (oral vaccination with alginate microsphere systems). There is also a novel microencapsulation method for rotavirus with anionic polymers and amines, including sodium alginate and spermine hydrochloride, which increases the antibody titers against rotavirus infection [ 8 ]. Similarly, microencapsulations of PEDV can arrive at the gut of piglets and release the virus in an alkaline environment. Moreover, they can be taken up by mucosa-associated lymphoid tissues to activate mucosal immune responses against encapsulated PEDV, and be processed by Peyer’s patches and M-cells in the small intestine [ 9 ]. In this study, inactivated PEDV packaged in microencapsulations was used to explore an efficient oral vaccine delivery system to release the virus into the gut, which would be better for protecting against PEDV-induced specific mucosal immunity in mice. In addition, mucosal and systemic immune responses were monitored for specific antibodies, such as IgA and IgG, in the feces and serum of mice, and then used to analyze the neutralizing activity against PEDV. Most importantly, the micro-encapsulations of PEDV were used with the antigen of complete enterovirus particles to present into the mucosal immune cells in the gut. The functional immune cells in the specific immune response, such as dendritic cells and B cells, were studied to focus on the mechanism of complete virus particles in the recognition, presentation, and antigen processing with oral mucosal immunity against enterovirus infection in vivo. 2. Materials and Methods 2.1. Cell and Virus PEDV strain LJB/03 was previously isolated from diarrheic piglets in China and purified in our laboratory [ 10 ]. Vero cells were cultured in Dulbecco’s modified Eagle’s medium (DMEM, Gibco) supplemented with 10% fetal bovine serum (FBS, Gibco) at 37 °C with 5% CO 2 . A PEDV strain (LJB/03) was isolated and stored in our laboratory. Confluent Vero cells grown in a 5 mL tissue culture flask were washed with PBS three times and inoculated with 1 mL of a mixture solution containing trypsin at a concentration of 10 µg/mL, PEDV inoculation culture (3 × 10 4 PFU), and DMEM without any serum. After incubating at 37 °C for 1 h, 4 mL of DMEM with trypsin at a concentration of 8 µg/mL was added. Before 70% cytopathic effects, the cells were maintained at 37 °C under 5% CO 2 and monitored daily. Finally, the diseased cells were subjected to three rounds of freezing and thawing, and then the supernatants were collected after centrifugation for 10 min at 12,000 rpm. The virus titers were measured with the method of TCID50, and the PEDV titer was approximately 6.3 × 10 7 PFU. PEDV was inactivated with 0.1 M binary ethylenimine (BEI) to a final volume of 5%, which was incubated at 37 °C for 24 h. In addition, sodium thiosulfate was used to neutralize the excess BEI at 37 °C for 2 h. Inactivated PEDV virus was stored at −80 °C until use. 2.2. The Production of Microcapsules The inactivated PEDV (6 × 10 6 PFU and 6 × 10 7 PFU) and sodium alginate solution at 1.5% (wt/vol) were obtained by dissolving and passing the solution. The CaCl 2 -chitosan solution was obtained by adding CaCl 2 and sodium alginate to final concentrations of 4% and 1% (wt/vol), respectively. After completely mixing the PEDV and the sodium alginate solution, the mixture was dropped at a constant speed (approximately 60–90 drops/min) through a medical 9-gauge syringe into a solution of calcium chloride and chitosan acetic acid. A suspension of sodium alginate–chitosan microcapsules was obtained after thorough stirring at a constant rate of approximately 300 r/min at room temperature for 30 min. The particle size was approximately 7.54 ± 2.87 μm, which was measured under a light microscope. Finally, the samples were separated, filtrated, and washed repeatedly with distilled water, precooled at −80 °C for 1 h, and freeze-dried. 2.3. Analysis of Encapsulation Efficiency and Protein Content The 100 mg freeze-dried microcapsules were weighed into a 50 mL centrifuge tube with 10 mL trisodium citrate solution (0.06 mol/L) and incubated at room temperature for 10 min. The microcapsules were ultrasonicated and centrifuged at 10,000 rpm for 10 min. Finally, approximately 1 mL of the supernatant (filtrated processing if there was another matter) was collected to determine the total protein content by the Bradford Protein Assay Kit (Coomassie Brilliant Blue) [ 11 ]. The encapsulation efficiency (B) and the amount of carrier protein (Z) of the microcapsule were calculated according to the formula [ 12 ]: B = W/J × 100% (1)

Z = W/M (2) (W: protein content in the microcapsules; J: total amount of protein; M: total amount of microcapsules.) 2.4. In Vitro Release Experiment of Microcapsules in Different Saline Solutions, pH Values, and Room Temperature Storage Tolerances Three 50 mL centrifuge tubes containing 100 mg of PEDV microcapsules were added to 10 mL of pH 7.4 PBS solution, 0.75% physiological saline solution, and pH 2.3 hydrochloric acid solution, and then placed in the Oven-Controlled Crystal Oscillator at 37 °C and a speed of 100 r/m. The release of protein content in the solution was measured at 1 h, 3 h, 9 h, 1 d, 3 d, 6 d, 12 d, and 18 d. The protein content was analyzed by the Coomassie Brilliant Blue method [ 13 ], and then the release rate (RT) curve was drawn. The PEDV microcapsules of freeze-dried particles were stored without any media in the dark at room temperature for 5 months, and the storage performance was evaluated by measuring the changes in the PEDV protein release rate every month. The concrete method of PEDV protein release rate refers to analysis of encapsulation efficiency and protein content. The release rate (RT) was calculated according to the formula: RT = R/W. (R: release amount of PEDV protein; W: the protein content in the microcapsule) [ 3 ]. 2.5. Immunization of Microcapsules in SPF Mice A total of 50 SPF mice, 5 weeks old, with approximately 18 g of body weight, were randomly divided into five groups. Each group contained 10 mice. The immunization regimen is shown in Table 1 . The first group, the negative control group, was immunized with PBS buffer through oral administration. The second group was immunized with microcapsules without virus through oral administration. The third group was immunized with inactivated PEDV without encapsulation through oral administration. The fourth group was immunized with the encapsulated PEDV vaccine through oral administration, which encapsulated approximately 6 × 10 6 PFU of PEDV. The fifth group was immunized with approximately 6 × 10 7 PFU of encapsulated PEDV through oral administration, which encapsulated 100 μL of PEDV. All the groups were used to immunize mice via an intragastric route on Days 1 and 3 twice. On Days 0 (preimmunization), 3, 6, and 9, 200 mg serum samples and feces samples were collected from both the tail vein and the anus. The fecal samples were subsequently homogenized for 30 min in 400 μL of sterile PBS (pH 7.4) containing 0.01 mol/L EDTA-Na 2 and then incubated for 12 h at 4 °C. The extracted supernatants of all fecal samples were collected by centrifugation at 15,000× g for 10 min and stored at −80 °C [ 6 ]. The feces were supplemented with protease inhibitors for the subsequent ELISA analysis. The serum was stored at −80 °C for the subsequent ELISA and neutralization analyses. Intestinal lavage samples (mucus) were obtained from the intestine of euthanized mice. The mucus was suspended in 400 μL of sterile PBS (pH 7.4) containing 0.01 mol/L EDTA-Na 2 for 2 h at 4 °C. Then, all mucus samples were collected by centrifugation at 15,000× g for 10 min, and the supernatant was stored at −80 °C with protease inhibitors for neutralization analysis. 2.6. Enzyme-Linked Immunosorbent Assay (ELISA) The ELISA plates were coated for 18 h at 4 °C with PEDV (6.3 × 10 7 PFU), which was previously cultured from Vero cells in the previous section. After the plates were blocked with 5% skim milk in PBS for 1.5 h at 37 °C, they were washed 3 times with PBST (PBS + 0.1% Tween 20). Sera and fecal samples (supernate of fecal) were added into wells in triplicate and used to test specific antibodies such as IgG and IgA. The sera and fecal samples were incubated for 1 h at 37 °C and washed as before. Goat anti-mouse IgG and IgA antibodies–HRP (Invitrogen) were added to each well (1:5000) and incubated for 1 h at 37 °C. After the final round of washing with PBST three times, the TMB substrate was used for color development, and the absorbance was measured at 490 nm. 2.7. PEDV Neutralization Assay The serum of mice fed with PEDV microcapsules and inactivated PEDV was collected to determine the neutralization ability of antibodies. The serum and intestinal lavage of mucus were obtained from the previously described immunization, and were filtered with a 0. 45 µm filter membrane. The concrete method was as follows: 50 µL samples (serum and intestinal lavage) were taken to a constant dilution from 1:2 to 1:512 and then added to a 96-well plate for eight replications with Vero cells. PEDV at a titer of 5 × 10 5 PFU was mixed within the DMEM culture medium, and 10% heat-inactivated bovine serum albumin was added to the cell plate, which was coated with the diluted serum and fecal sample solution and then incubated with the antibody and virus at 37 °C for 1 h. Then, 100 µL of Vero cells were added to the antibody–virus mixture and incubated in a 5% CO 2 incubator at 37 °C for 3 days. Finally, the covered medium was discarded, and the wells were washed three times with sterile PBS (pH = 7.4) and dyed with 1% crystal violet solution. The quantity variance of plaque was analyzed to demonstrate their antibody level. 2.8. T-Cell Proliferation Five mice were dissected from each group on the seventh day after the second immunization. Single-lymphocyte suspensions were prepared from the spleen after the second immunization, as previously described [ 5 ]. Lymphocytes were isolated from the spleens of five mice dissected from each group and incubated in triplicate in 96-well plates at 5 × 10 5 cells/well with Roswell Park Memorial Institute 1640 medium (RPMI-1640) plus 20% fetal calf serum (FCS) at 37 °C in a 5% CO 2 incubator. Then, the cells were stimulated for 48 h with 0.5 and 1 μg/mL inactive PEDV in the experimental group (specific antigen stimulation) and control group (without antigen stimulation). Based on the manufacturer’s instructions (Promega), the Cell Titer 96 Aqueous Non-Radioactive Cell Proliferation Assay was used to evaluate T-cell proliferation. The solution of A thiazolyl blue (MTT) was pipetted (10 µL) into each well to develop the color. The plates were incubated for 4 h before reading the OD 490 values of the plate using the Magellan plate reader, and then the average was taken of the PEDV stimulation data to compare with that of the negative control wells. The proliferation rate was analyzed with the stimulation index: SI = (OD490 experiment group − OD490 culture media)/(OD490 control group − OD490 culture media) 2.9. Flow Cytometry and Cell Sorting The suspensions of single lymphocytes were derived from the spleens of immunizing mice that were dissected from each group on the seventh day of the second immunization [ 14 ]. The isolated spleen T-cells (5 × 10 5 cells/mL) were cultured in RPMI 1640 culture media for flow cytometry staining. The incubated single-lymphocyte suspensions were stained with anti-CD11c (PE-conjugated) and anti-CD11b (FITC-conjugated) antibodies and anti-CD23 (APC-conjugated) and anti-B220 (PE-conjugated) antibodies in RPMI 1640 culture media without serum. All antibodies were purchased from Miltenyi Biotec. Single lymphocyte cells were stained with CD11c (PE-conjugated) and CD11b (FITC-conjugated) antibodies and sorted with FACStar to prepare CD11c + and CD11b + cells. The same method was used to prepare CD23 + B220 + cells and B220 + cells. All the samples were tested with FACSCanto (BD Biosciences) and analyzed by CellQuest software [ 15 ]. In all cases, the purity of FACStar-sorted cells was >98%. The cells were sorted by FACSAria (BD Biosciences) into CD11c + , CD11b + , CD23 + B220 + , and B220 + populations in complete medium (RPMI, 1% penicillin-streptomycin, 1% glutamine, 50 mM b-mercaptoethanol). 2.10. Cytokine Assays Real-time qRT-PCR was used to determine the levels of cytokine genes and intestinal tight junction gene products in splenic lymphocyte and intestinal samples from immunized mice using a CFX96TM Real-Time PCR Detection System (Bio-Rad, Hercules, CA, USA). Total RNA was extracted from intestinal tissues and spleen with total RNA extraction kits (TaKaRa, Dalian, China) according to the manufacturer’s instructions [ 16 ]. Total RNA was converted to cDNA using the PrimeScript TM RT reagent Kit with gDNA Eraser (TaKaRa, Dalian, China) [ 17 ]. The cDNA products were used for real-time PCR with a SYBR Premix Ex Taq TM II reagent kit (TaKaRa, Dalian, China), and the specific primers used are listed in the Table S1 [ 18 ]. The Livak method (2 −∆∆CT method) was used to calculate the fold change compared to β-actin gene controls [ 19 , 20 ]. 2.11. Statistical Analysis All the samples and experiments were analyzed in triplicate, and all the groups were examined as independent measurements to support adequate statistics in the experiments. The average duration of recovery and colonization over time were compared between groups using repeated measures analysis of variance with Bonferroni’s correction using SPSS software (IBM, New York, USA). Data between the different groups were analyzed with one-way repeated measures analysis of variance (ANOVA) and the least significant difference (LSD) test with GraphPad software. Statistically significant effects ( p < 0.05) were further analyzed [ 21 ]. 2.12. Ethical Statement All animals were housed in negative-pressure isolators with HEPA filters in a BSL2. The protocols for animal experiments were approved by the Institutional Committee of Northeast Agricultural University (2018NEAU-131, 12 September 2018) and complied with the guidelines of the Northeast Agricultural University Administrative Committee of Laboratory Animals. 3. Results 3.1. The Excellent Storage Tolerances of Microcapsules in Different Saline Solutions, pH Values, and Room Temperature As a biomedical material, the ability of microcapsules to be released in saline and acid solutions is crucial in clinical applications. The release rates in different saline solutions, pH values, and storage times are shown in Figure 1 . The trend of the in vitro release ability of microcapsules in the PBS group and normal saline group was similar, and the release rate was more than 50% on the 3rd day; on the 18 th day, the release rate reached 95% and 91%, respectively. However, that of the hydrochloric acid group was only 37.5% on the 3rd day and just 63.2% on the 18th day. These results indicated that the microcapsules were easily released in saline solution, but most importantly, they were acid-stable. The release ability after different months of storage showed that the release rate remained higher than 83% in the first three months, and they still maintained the lowest release rate of 41% in the fifteenth month. These results indicated that the microcapsules have excellent storage tolerance in the dark at room temperature for 5 months. 3.2. The Microcapsules Stimulate the Specific Humoral and Mucosal Immunity The specific antibodies in intestinal lavage and serum were detected by ELISA at the end of the immunization. The ELISA results showed that with increasing days, the specific antibody level in both the inactivated PEDV and microcapsule groups continuously increased, as shown in Figure 2 . For specific IgA, the PEDV (low) and PEDV (high) microcapsule groups had significantly higher levels than the inactivated group on the third day ( p < 0.05), and the PEDV (high) microcapsules group had remarkably higher levels than the PEDV (low) microcapsules group ( p < 0.05). The PEDV (low) microcapsules group had significantly higher levels than the inactivated PEDV ( p < 0.05) on the sixth day, while the PEDV (high) microcapsules group had significantly higher levels than the inactivated group ( p < 0.01). At the end of the detection on the ninth day, both PEDV microcapsules groups had significantly higher levels than the inactivated group ( p < 0.01). Most importantly, the empty microcapsule group did not have detectable IgA antibodies during the whole immunization period. Figure 2 B shows that the specific IgG levels in both PEDV microcapsules showed the same trend as the intestinal lavage results and were significantly higher than those in the inactivated PEDV group on the third day ( p < 0.05). The specific IgG levels in the PEDV microencapsulated groups were significantly higher than those in the inactivated PEDV group on the sixth and ninth days ( p < 0.01). These results suggest that the PEDV microcapsules have the ability to activate specific mucosal and systemic immune responses in a dose-dependent manner in mucosal immunity. 3.3. The Specific IgG and IgA Neutralized PEDV The neutralization of IgG ( Figure 3 A) and IgA ( Figure 3 B) is shown in Figure 3 . The results indicated that the neutralization of IgG in the PEDV (high) microcapsule group was more effective than that in the PEDV (low) microcapsule group after the 1:8 dilution point against PEDV infection in the in vitro experiment. The 50% neutralization with IgG of the high PEDV group was probably 1:256, while the PEDV (low) microcapsule group was 1:128. The 50% neutralization of the PEDV (high) microcapsule group was higher than the PEDV (low) microcapsule group in the neutralization. The neutralization of IgA in both the PEDV (high) and PEDV (low) microcapsule groups was higher than that in the inactivated PEDV group, inhibiting PEDV infection in the in vitro experiment. The 50% neutralization of IgA for the inactivated PEDV group, PEDV (low) microcapsule group, and PEDV (high) microcapsule group gradually increased against PEDV infection in Vero cells at dilutions of 1:16, 1:32, and 1:64, respectively. The neutralization ability of IgG and IgA in the PEDV (high) microcapsule group was higher than that in the PEDV (low) microcapsule group. The neutralization of PEDV microcapsules was also dose-dependent, which indicated that the PEDV (high) microcapsule group had better systemic and mucosal immunity than the PEDV (low) microcapsule group. 3.4. PEDV Microcapsules Stimulated Immune Memory To further analyze whether microcapsules influence cell-mediated immunity, T-cell proliferation was analyzed to study immune memory with PEDV from five immunized mice for 29 days after the third immunization to obtain a single-cell suspension of lymphocytes for the in vitro experiment ( Table 2 ). The suspension was stimulated with PBS (as a control), microcapsules (without PEDV), inactivated PEDV, PEDV (low) microcapsules, and PEDV (high) microcapsules. Different doses of 0.5 μg/mL and 1.0 μg/mL PEDV were used to simultaneously stimulate lymphocyte proliferation. At a dose of 0.5 μg/mL PEDV, the number of PEDV (low) microcapsules was significantly higher than that in the PBS group; moreover, the number of PEDV (high) microcapsules was significantly higher than that in the PBS group. There was no significant difference between the microcapsule groups, inactivated group, and PBS group with regard to the specific antibodies. With the stimulating dose of 1 μg/mL PEDV, both PEDV microcapsule groups were significantly higher than the PBS group. The microcapsules and inactivated group were not significantly different from the PBS group. The lymphocyte proliferation results indicated that both 0.5 μg/mL and 1 μg/mL PEDV could stimulate T-cell proliferation with immune memory for the immune response of PEDV microcapsules. Single-lymphocyte suspensions were isolated from animals after the last boost, plated as triplicates in a 96-well plate, and stimulated in vitro for 72 h with PEDV and con A as a positive control. T rate was analyzed with stimulation index: SI = (OD490 experiment group − OD490 culture media)/(OD490 control group − OD490 culture media). The differences between means were considered significant at * p < 0.05 and very significant at ** p < 0.01. 3.5. Microcapsules Enhanced the B Cell Differentiation CD11b and CD11c are cell surface markers of dendritic cells which were detected by flow cytometric analysis ( Figure 4 A) from different groups of immunizations. The results showed that PBS, microcapsules, and inactivated PEDV stimulated approximately 2.2% of CD11b+ cells, and PEDV (low) microcapsules and PEDV (high) microcapsules stimulated CD11b+ cells. Conversely, the trend in CD11c+ cells gradually increased from the PBS group (4.3%) to PEDV (high) microcapsules (34.6%). The results of CD23 and B220 cell markers ( Figure 4 B) indicated that all B220+ cells were stimulated for differentiation in addition to the inactivated PEDV group, and the PBS and microcapsule groups reached 57.4% and 54.4%, respectively. Research on B220+ cells indicated that inactivated PEDV could better inhibit antibody production with oral immunization compared with other groups. Most importantly, the percentage of B220+ cells in both the PEDV (low) microcapsule and the PEDV (high) microcapsule groups was higher than that in the inactivated PEDV group. Nevertheless, B220+ and CD23+ cells were significantly increased by stimulation with PEDV; moreover, the percentages of these three groups were slightly different from those of the inactivated PEDV group (46.6%), the PEDV (low) microcapsules (45%) and the PEDV (high) microcapsules (47.7%). 3.6. Microcapsules Inhibit the Inflammation To validate the results of inflammation after immunization, qRT-PCR was performed to analyze cytokine expression at the mRNA level ( Figure 5 ). Compared to the samples from the different groups, our qRT-PCR results revealed significant differences in the expression of genes, such as IFN-γ, IL-4, IL-1, TNF-α, IL-17, IL-10, TGF-β, occluding, and ZO-1. The expression analysis was clustered by hierarchical clustering using the complete linkage algorithm and Pearson correlation metric in R for the heat map with GraphPad software. The heat map results indicated that the IFN-γ expression in the microcapsule group, PEDV (low) microcapsule group, and PEDV (high) microcapsule group was significantly higher than that in the inactivated group, and IFN-γ expression increased with increasing doses of PEDV. IL-4 expression showed a similar trend in the microcapsule group, PEDV (low) microcapsule group, and PEDV (high) microcapsule group, which stimulated the Th2 immune response. IL-4 expression in the inactivated group was different from IFN-γ expression, which indicated that the microcapsules could stimulate Th1 immune response. However, the two PEDV microcapsule groups exhibited different Th1 immune responses compared with the inactivated group. The microcapsules could effectively inhibit the inflammation stimulated by the inactivated virus, which could decrease the expression of IL-1, TNF-a, and IL-17 in the microcapsule groups. The anti-inflammatory cytokines IL-10 and TGF-b were significantly increased in the microcapsules groups compared with the inactivated group. The relative tight junction genes also showed the same expression trend in various groups. 4. Discussion The PEDV outbreak of 2013–2014 led to annual losses among worldwide swine producers. The loss of productivity from enteric diseases of PEDV in neonatal piglets costs swine producers millions of dollars [ 2 , 22 ]. Previous development of live and attenuated vaccines for another diarrheal virus of pigs, transmissible gastroenteritis virus (TGEV), provided insights into the mechanisms of mucosal immunity with IgA and piglet protection [ 5 , 23 ]. A previous study showed that the inactive PEDV was effective in stimulating the specific antibody of IgA in an immunized sow with attenuated vaccines protecting the piglets for lactogenic immunity [ 24 ]. Lactogenic immunity from pregnant sows is induced via the gut–mammary gland secretory IgA (sIgA) axis, which is also a promising and effective way to protect suckling piglets from PEDV infection [ 25 ]. Therefore, a successful PEDV vaccine must induce sufficient maternal or self-reproductive IgA antibodies [ 26 , 27 ]. However, the PEDV did not use the same route as the TGEV immune plan. The main reason is that the antibody titers of PEDV did not reach the titers of TGEV to boost a successful immune response. More research has focused on recombinant vaccines with different delivery vectors to protect antigens not digested by gastric acid [ 28 ]. However, the exposure dose of antigen was too low to stimulate specific antibodies, such as IgA and IgG. The antigen expressed by the recombinant vaccine was very exclusive. We explored a new form of possibility to deliver the virus into the gut, stimulating the specific mucosal immune response, which could directly neutralize the enterovirus at the site of infection. Alginate microcapsules using ionic gelation represent a new and interesting approach to oral delivery systems for inactivating PEDV carriers. The microcapsules could efficiently capsulate the inactive PEDV antigen, and the whole virus particle was contained in the microcapsule. The microcapsules had good release profiles of the virus particles in saline solutions, such as PBS and normal saline, and the release rate was higher than 50% within three days. Studies have shown that the specific antibodies of IgA reach a peak in the second after immunization [ 29 ]. The most important feature was the microcapsules protecting the integrity of virus particles in hydrochloric acid, which prevents the virus particles from being released and subsequently digested in gastric acid [ 30 ]. Phage encapsulation and subsequent release kinetics revealed that the microcapsules possess pH-responsive characteristics with phage release triggered in an intestinal pH range suitable for therapeutic purposes [ 31 ]. A number of previous studies have used alginate as the main encapsulating agent either on its own or in combination with chitosan [ 32 , 33 ]. The chitosan–alginate microspheres effectively protected the virus in simulated gastric conditions, showing the remaining viral titers. The chitosan–alginate microspheres acted as an acid barrier in the simulated gastric conditions, helping the virus arrive at the M cell in the intestinal mucosal immune system. With storage at room temperature, the PEDV microcapsules displayed a remarkably low loss of antigen in the first three months, and they had good storage tolerance, thus maintaining the quality of the PEDV antigen. Tan reported that tocotrienols encapsulated in chitosan–alginate microcapsules have effective storage tolerance in the yogurt matrix [ 34 ]. PEDV initially attacks neonatal intestinal epithelial cells in piglets and the intestinal tract system, inducing diarrhea clinical signs, but systemic lymphoid organs cannot provide the effective antibody IgG to neutralize this virus in the neonatal pig. They mainly depend on the innate immunity of maternal antibodies. Thus, we chose microcapsules carrying inactive PEDV to stimulate the mucosal immune system of neonatal piglets. The specific antibodies against IgA and IgG showed that the microcapsules stimulated the mucosal and systemic immune systems producing specific antibodies, such as IgA and IgG [ 5 ]. In the first mouse immunization experiment, the microcapsule groups had higher levels of antibodies than the inactivated PEDV group. Most importantly, the immunization of microcapsules in specific antibody production was dose-dependent, and the levels of specific IgA and IgG in the high-dose microcapsule group were significantly higher than those in the low-dose microcapsule group. There was a close connection between the specific neutralization of antibody titers and the dose dependence of microcapsules arriving at the mucosal surface. The results of 50% neutralization with specific IgG and IgA were also found during microcapsule immunization, and PEDV (high) microcapsule groups had better neutralizing activity than PEDV (low) microcapsule groups. The specific antibody of IgA had a greater efficiency of neutralization than the specific antibody of IgG in the same group. The main reason was that chitosan–alginate microcapsules stimulate humoral immunity at the mucosal area, which is mainly mediated by IgA antibodies as the predominant immunoglobulin, and serum-derived IgG also contributes to immune defense [ 35 ]. Specific antibody experiments have indicated that microcapsules stimulate specific mucosal and systemic immunity in mice. However, the mice are not the infecting hosts of PEDV, which means there is just the possibility of an immune response in piglets. There are many differences in immunization and infection between mice and neonatal pigs. Virus particle carriers have shown higher potential as oral delivery systems of proteins and peptides, which are taken up by M-cells of Peyer’s patches in the gut [ 35 ]. As seen in the qRT-PCR results, the microcapsules of PEDV, which have been reported to immunize with microcapsules, were associated with higher levels of IFN-γ production related to the T helper 1 (Th1)-type immune response [ 36 ]. In contrast, immunization with microcapsules without PEDV promoted IL-4 secretion related to the Th2-type immune response. IFN-γ production was higher than IL-4 production after PEDV microcapsule immunization. The cellular immune response (Th1) and humoral immune response (Th2) were disrupted, and the Th1 type immune response was predominant [ 6 ]. In particular, the high-dose PEDV microcapsules enhance IFN-γ expression, which means that the PEDV microcapsule immunization mediates the T helper 1 (Th1)-type immune response, and the chitosan–alginate plays an immunoregulatory role in extroversion to the cellular immune response. The mouse oral immunization of recombinant Lactobacillus casei expressing the Dendritic Cell-Targeting Peptide Fusing COE Protein of PEDV also mediated the Th1 immune response in piglets [ 37 ]. The cytokine response was also analyzed to compare the inflammation, cellular and humoral immunity in oral immunization with PEDV microcapsules. IL-1 and TNF-α were also used to analyze the safety and inflammation with immunization, which did not stimulate the inflammatory response when using the oral PEDV microcapsules. Many more studies have demonstrated the chitosan–alginate induction of the Th1-type immune response for oral vaccination in mice, and studies on the effects of chitosan have indicated that chitosan-fed farm animals showed higher weight gains but a lower incidence of disease than unfed animals [ 38 , 39 , 40 ]. DC-specific delivery has been considered a promising strategy for facilitating the efficient recognition, processing, and presentation of antigens by DCs, leading to enhanced antigen-specific immunity. The dendritic cell-targeted chitosan nanoparticles for nasal DNA immunization suggest that targeted pDNA delivery through a noninvasive intranasal route can be a strategy for designing low-dose vaccines [ 41 ]. Without adjuvant immunization, the increase in CD11c+ during vaccination promotes germinal center induction and robust humoral responses [ 42 ]. When injected, these alginate ‘vaccination nodes’ containing activated DCs attracted both host dendritic cells and a large number of T-cells to the injection sites in mice, while some of the inoculated DCs trafficked to the draining lymph nodes [ 43 ]. Compared with the inactivated PEDV group, chitosan–alginate groups, such as high-dose PEDV microcapsules and low-dose PEDV microcapsules, significantly stimulated the CD11c+ increase after the last immunization. Taking the advantage of CD11c+ in vivo DC targeting into consideration, chitosan–alginate could presumably induce in vivo DC maturation more robustly than inactivated PEDV. The chitosan–alginate could first effectively induce DC maturation of CD11c+ through the interaction with immunoregulation of chitosan–alginate in the gut, which enhanced the specific immune response, inducing subsequent humoral immunity with mucosal immunity and the systemic immune response. 5. Conclusions The oral microencapsulation was packaged with different titers of inactivated PEDV, which consisted of alginate and chitosan arriving and presenting to the gut in mice. It induced specific humoral and mucosal immunity. Specific antibodies from immunized mice, such as IgA and IgG, neutralized PEDV in vitro. Oral immunization also stimulated immunologic memory in mice. Alginate and chitosan not only act as capsule wall materials but also enhance the viability of immune cells such as DCs and B cells with the function of adjuvants. To the best of our knowledge, this study of microencapsulation is the first to package enterovirus in the immunization of mice even though the host of PEDV is pigs. Therefore, the host animals, pigs, should be studied with inactivated and microencapsulated PEDV. All the data derived from this study can be an important reference point for further research in this area. Acknowledgments Student Innovation Practical Training of NEAU. Disclaimer/Publisher’s Note: The statements, opinions and data contained in all publications are solely those of the individual author(s) and contributor(s) and not of MDPI and/or the editor(s). MDPI and/or the editor(s) disclaim responsibility for any injury to people or property resulting from any ideas, methods, instructions or products referred to in the content. Supplementary Materials The following supporting information can be downloaded at: https://www.mdpi.com/article/10.3390/ani13050889/s1 , Table S1. Primers used for q-RT PCR for inflammatory and functional analyses. Click here for additional data file. Author Contributions Data curation, Z.Q.; Formal analysis, Z.Q., G.L., J.X. and L.L.; Methodology, W.W., W.C. and X.J.; Resources, X.H.; Writing—original draft, Z.N. and X.J.; Writing—review and editing, X.J. and D.L. All authors have read and agreed to the published version of the manuscript. Institutional Review Board Statement Animals were housed in negative-pressure isolators with HEPA filters in a BSL2. Protocols for animal experiments were approved by the Institutional Committee of Northeast Agricultural University (2016NEAU-219, 13 September 2016) and complied with the guidelines of Northeast Agricultural University laboratory animal welfare and ethics of Northeast Agricultural University Administrative Committee of Laboratory Animals. Informed Consent Statement Not applicable. Data Availability Statement Once this manuscript is accepted, the data supporting the results of this study will be made publicly available in any publicly accessible repository. Conflicts of Interest The authors declare no financial or commercial conflict of interest. References 1.

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Injectable dendritic cell-carrying alginate gels for immunization and immunotherapy Biomaterials 2008 29 3671 3682 10.1016/j.biomaterials.2008.05.033 18565578 Figure 1 The stability of microcapsules shown by the release rate in ( A ) PBS, normal saline, hydrochloric acid, and release ability in different months ( B ). The differences between means were considered significant at * p < 0.05 and very significant at ** p < 0.01. Figure 2 Enzyme-linked immunosorbent assay measures of antibodies IgA and IgG in feces ( A ) and serum ( B ) after the final immunity. The differences between means were considered significant at * p < 0.05 and very significant at ** p < 0.01. Figure 3 The results of antibody neutralization activity of IgG ( A ) and IgA ( B ). Both neutralization percentages of IgA and IgG in the intestinal mucosa and serum. Figure 4 The flow cytometric analysis results for the percentage of CD11b+ and CD11c+ cell for immunization ( A ). ( B ) indicates the percentage of B220+ and CD23+ cell with the flowcytometric analysis. Figure 5 The expression analysis of genes by qRT-PCR analysis. For the expression analysis of genes, blue and red indicate decreased and increased expression, respectively. For qRT-PCR analysis of the expression of randomly selected novel genes from the immune and tight junction, data are presented as mean ± S.D. (n = 3). animals-13-00889-t001_Table 1 Table 1 Immunization regime of mice. Groups (n) Type of Vaccine 1st Vaccination 2nd Vaccination Route Dose Route Dose PBS (10) Negative control of PBS buffer O/A 0.2 mL O/A 0.2 mL Microcapsules (10) PBS encapsulated in alginate and chitosan O/A 0.2 mL O/A 0.2 mL Inactivated PEDV(10) Inactivated PEDV vaccine O/A 0.2 mL O/A 0.2 mL PEDV (low) microcapsule (10) PEDV vaccine encapsulated in alginate and chitosan with low titer virus (6 × 10 6 PFU) O/A 0.2 mL O/A 0.2 mL PEDV (high) microcapsule (10) PEDV vaccine encapsulated in alginate and chitosan with high titer virus (6 × 10 7 PFU) O/A 0.2 mL O/A 0.2 mL n = number of mice; O/A = oral administration. animals-13-00889-t002_Table 2 Table 2 Lymphocyte proliferation index. Groups Stimulation Index Value 0.5 μg/mL PEDV 1 μg/mL PEDV PBS(Control) 1.054 ± 0. 13 1.025 ± 0.11 Microcapsules 1.272 ± 0. 149 1.231 ± 0.156 Inactivated PEDV 1.349 ± 0.151 1.358 ± 0.166 PEDV (low) microcapsule 1.721 ± 0.171 * 2.529 ± 0.183 ** PEDV (high) microcapsule 1.987 ± 0.177 ** 3.161 ± 0.191 **

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# 翻译

**动物(巴塞尔)** 动物(巴塞尔)2763 动物 动物 **动物**:MDPI开放获取期刊 2076-2615 多学科数字出版研究所(MDPI)PMC10000104 PMC10000104.1 10000104 10000104 36899746 10.3390/ani13050889 animals-13-00889 1 论文 **口服海藻酸-壳聚糖微胶囊递送的肠道呈灭活猪流行性腹泻病毒在小鼠中诱导黏膜免疫**

**作者:** 秦子良(形式分析、数据整理)1 † 乃子达(初稿撰写)1 † 李刚(形式分析)1 何新苗(资源提供)2 王雯韬(方法学)2 夏继桥(形式分析)1 王超(形式分析)2 李璐 2 https://orcid.org/0000-0003-1128-2157 蒋新鹏(初稿撰写、审校编辑)1 * 刘迪(数据整理)2 * 王悦(学术编辑)1

1 东北农业大学动物科学技术学院,哈尔滨 150030,中国 2 黑龙江省农业科学院畜牧兽医研究所,农业农村部种养结合重点实验室,哈尔滨 150086,中国

* 通讯作者:jiangxinpeng@neau.edu.cn(蒋新鹏);liudi1963@163.com(刘迪);电话:+86-451-55190722(蒋新鹏 & 刘迪) † 共同第一作者

2023年2月28日 2023年3月 13 5 430977 889 2022年12月1日 2023年2月20日 2023年2月21日 2023年2月28日 2023年3月11日 2024年5月2日

© 2023 作者。2023 https://creativecommons.org/licenses/by/4.0/ 许可方:MDPI,巴塞尔,瑞士。本文为根据知识共享署名(CC BY)许可条款和条件分发的开放获取文章(https://creativecommons.org/licenses/by/4.0/)。

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**简单摘要**

猪流行性腹泻病毒(PEDV)是一种α冠状病毒,可引起重大疫情暴发,在出生后7天内的仔猪中致死率高达100%。在本研究中,我们使用含有灭活PEDV的微胶囊对小鼠进行口服免疫,以提高口服递送方法在预防PEDV感染方面的有效性,并避免在胃酸环境中的消化降解。此外,PEDV微胶囊表现出优异的储存耐受性,可维持PEDV抗原的质量。PEDV微胶囊将灭活病毒递送至肠道,刺激小鼠的特异性黏膜免疫反应,可直接中和肠道病毒。

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**摘要**

猪流行性腹泻病毒(PEDV)可引起仔猪腹泻、呕吐和死亡,造成巨大的经济损失。因此,了解如何在仔猪中诱导黏膜免疫反应对于PEDV感染的黏膜免疫机制和应用至关重要。本研究采用一种治疗方法,制备了以海藻酸钠和壳聚糖为微囊化材料包裹灭活PEDV的口服疫苗,并适应了小鼠的肠道环境。微胶囊的体外释放实验表明,灭活PEDV不仅在盐溶液和酸溶液中易于释放,而且具有优异的储存耐受性,适合作为口服疫苗使用。有趣的是,不同剂量的灭活病毒实验组均增强了血清和肠黏液中特异性抗体的分泌,分别通过IgG和IgA在Vero细胞中实现了对PEDV的有效中和。此外,微囊化可刺激CD11b⁺和CD11c⁺树突状细胞的分化,这意味着微囊化也被鉴定为一种口服佐剂,有助于小鼠树突状细胞的吞噬作用。流式细胞术结果显示,在PEDV抗原组的刺激下,B细胞的B220⁺和CD23⁺可显著增加抗体产生,微囊化还可提高B细胞的活力,刺激小鼠中IgG和IgA等抗体的分泌。此外,微囊化促进了抗炎细胞因子如IL-10和TGF-β的表达。与灭活PEDV组相比,微囊化组中的海藻酸钠和壳聚糖抑制了促炎细胞因子如IL-1、TNF-α和IL-17的表达。综上所述,我们的结果表明,微粒可发挥黏膜佐剂的作用,在肠道中释放灭活PEDV,有效刺激小鼠的黏膜和全身免疫反应。

**关键词:** 微胶囊;PEDV;黏膜免疫;海藻酸盐;壳聚糖

**资助:** 国家自然科学基金(31902169);黑龙江省优秀青年科学基金(YQ2020C008);东北农业大学"青年人才"项目(18QC39)。本研究得到国家自然科学基金(项目编号:31902169)、黑龙江省优秀青年科学基金(项目编号:YQ2020C008)和东北农业大学"青年人才"项目(项目编号:18QC39)的资助。

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## 1. 引言

猪流行性腹泻病毒(PEDV)是一种高度传染性疾病,在仔猪出生后前七天感染小肠上皮细胞,三日龄仔猪的死亡率可达70%至100%[1]。在出生的第一周,仔猪的主要免疫保护依赖于母源抗体和先天免疫。母源抗体是通过肌肉注射或皮下注射途径对妊娠母猪接种PEDV灭活疫苗和弱毒疫苗诱导产生的,但母源抗体在进入肠道前被胃酸和胃蛋白酶消化,无法有效预防PEDV感染。然而,黏膜免疫可在出生后三天内建立,为仔猪提供比全身免疫更有效的保护。一些研究表明,肠道中IgA构成的第一道防线在中和肠道疾病感染方面比IgG更为有效[2]。然而,如何将灭活PEDV病毒转运至肠道并激活黏膜免疫的问题尚未解决。此外,胎猪肠道中针对PEDV的黏膜免疫机制仍不清楚。 specialized M细胞摄取PEDV并将其呈递给树突状细胞和淋巴滤泡的过程也需要更好地理解,以了解抗原如何到达诱导位点,实现T细胞和B细胞依赖性激活以产生IgG和IgA。

一种有趣的策略是将疫苗包装成微胶囊,微胶囊具有不同的口服免疫特性,如大小、形状和表面分子组织[3]。壳聚糖和海藻酸盐混合凝固离子凝胶,由于其内在的免疫调节特性,是作为主要成分的潜在候选载体。海藻酸盐是最广泛使用的载体之一,用于控制释放不同类型的活性剂。此外,海藻酸钠来源于海洋褐藻和细菌,因其独特的理化性质和生物活性,在食品工业中作为抗菌剂受到关注。壳聚糖(CS),也称为聚葡萄糖胺,因其生物相容性、生物降解性和黏膜黏附特性,被广泛用于增强黏膜免疫反应[4]。利用离子凝胶化制备海藻酸盐-壳聚糖微胶囊是复合口服递送系统用于灭活PEDV疫苗的一种有趣的方法。经典技术包括首先将灭活PEDV的抗原与海藻酸盐溶液混合,然后缓慢倒入氯化钙和壳聚糖溶液中。最后,通过倾析上清液收集海藻酸盐微胶囊并用水洗涤。因此,PEDV海藻酸盐微胶囊的制备方法非常简单。微囊化制备表明,它们使用简单的机械,成本低,安全性好,使其成为口服免疫的一种有吸引力的方法。

在黏膜免疫系统的先前研究中,口服重组乳酸菌疫苗在首次接触黏膜表面时刺激针对病原体的特异性免疫更有前景[5,6,7]。为了提高口服疫苗接种递送方法的有效性以预防PEDV感染,避免在胃酸环境中的消化降解至关重要(使用海藻酸盐微球系统的口服疫苗接种)。还有一种使用阴离子聚合物和胺(包括海藻酸钠和盐酸精胺)对轮状病毒进行微囊化的新方法,可增加针对轮状病毒感染的抗体滴度[8]。同样,PEDV的微囊化可到达仔猪的肠道,并在碱性环境中释放病毒。此外,它们可被黏膜相关淋巴组织摄取,激活针对包封PEDV的黏膜免疫反应,并由小肠中的派伊尔斑(Peyer's patches)和M细胞加工[9]。

在本研究中,将包封在微囊化中的灭活PEDV用于探索一种高效的口服疫苗递送系统,将病毒释放到肠道中,从而更好地保护小鼠免受PEDV诱导的特异性黏膜免疫。此外,监测了黏膜和全身免疫反应,检测小鼠粪便和血清中特异性抗体如IgA和IgG,然后用于分析对PEDV的中和活性。最重要的是,PEDV的微囊化与完整肠道病毒颗粒的抗原一起使用,呈递至肠道中的黏膜免疫细胞。研究了特异性免疫反应中的功能免疫细胞,如树突状细胞和B细胞,重点关注完整病毒颗粒在体内口服黏膜免疫中对肠道病毒感染的识别、呈递和抗原加工机制。

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## 2. 材料与方法

### 2.1. 细胞与病毒

PEDV毒株LJB/03此前从中国腹泻仔猪中分离并在本实验室纯化[10]。Vero细胞在添加10%胎牛血清(FBS,Gibco)的Dulbecco改良Eagle培养基(DMEM,Gibco)中,于37°C、5% CO₂条件下培养。PEDV毒株(LJB/03)在本实验室分离和保存。将生长在5 mL组织培养瓶中的汇合Vero细胞用PBS洗涤三次,接种1 mL含有浓度为10 µg/mL的胰蛋白酶、PEDV接种培养物(3×10⁴ PFU)和无血清DMEM的混合溶液。在37°C孵育1小时后,加入4 mL含有浓度为8 µg/mL胰蛋白酶的DMEM。在出现70%细胞病变效应之前,将细胞在37°C、5% CO₂条件下维持并每天观察。最后,将病变细胞进行三轮冻融,然后在12,000 rpm离心10分钟后收集上清液。用TCID₅₀方法测定病毒滴度,PEDV滴度约为6.3×10⁷ PFU。用0.1 M双乙烯亚胺(BEI)将PEDV灭活至终体积的5%,在37°C孵育24小时。此外,用硫代硫酸钠在37°C中和过量BEI 2小时。灭活的PEDV病毒在-80°C保存直至使用。

### 2.2. 微胶囊的制备

将灭活PEDV(6×10⁶ PFU和6×10⁷ PFU)与1.5%(wt/vol)海藻酸钠溶液混合,通过溶解和过滤获得。通过将CaCl₂和海藻酸钠分别添加至终浓度4%和1%(wt/vol)获得CaCl₂-壳聚糖溶液。将PEDV与海藻酸钠溶液完全混合后,通过医用9号注射器以恒定速度(约60-90滴/分钟)将混合物滴入氯化钙和壳聚糖乙酸溶液中。在室温下以约300 r/min的恒定速率充分搅拌30分钟后,获得海藻酸钠-壳聚糖微胶囊悬浮液。在光学显微镜下测量粒径约为7.54±2.87 µm。最后,将样品分离、过滤并用蒸馏水反复洗涤,在-80°C预冷1小时,然后冷冻干燥。

### 2.3. 包封效率和蛋白质含量分析

将100 mg冷冻干燥的微胶囊称入含有10 mL柠檬酸钠溶液(0.06 mol/L)的50 mL离心管中,在室温下孵育10分钟。将微胶囊超声处理并在10,000 rpm离心10分钟。最后,收集约1 mL上清液(如有其他物质则进行过滤处理),使用Bradford蛋白质测定试剂盒(考马斯亮蓝)测定总蛋白质含量[11]。根据公式计算微胶囊的包封效率(B)和载体蛋白量(Z)[12]:

B = W/J × 100% (1) Z = W/M (2)

(W:微胶囊中的蛋白质含量;J:蛋白质总量;M:微胶囊总量。)

### 2.4. 不同盐溶液、pH值和室温储存耐受性中微胶囊的体外释放实验

将三个含有100 mg PEDV微胶囊的50 mL离心管分别加入10 mL pH 7.4 PBS溶液、0.75%生理盐水和pH 2.3盐酸溶液,然后置于37°C、100 r/m速率的恒温晶体振荡器中。在1 h、3 h、9 h、1 d、3 d、6 d、12 d和18 d测定溶液中蛋白质含量的释放。通过考马斯亮蓝法分析蛋白质含量[13],然后绘制释放率(RT)曲线。将PEDV微胶囊的冷冻干燥颗粒在无介质、室温避光条件下储存5个月,通过每月测量PEDV蛋白质释放率的变化来评估储存性能。PEDV蛋白质释放率的具体方法参见包封效率和蛋白质含量的分析。释放率(RT)根据公式计算:RT = R/W。(R:PEDV蛋白质的释放量;W:微胶囊中的蛋白质含量)[3]。

### 2.5. SPF小鼠的微胶囊免疫

将50只5周龄、体重约18 g的SPF小鼠随机分为五组,每组10只。免疫方案见表1。第一组为阴性对照组,通过口服给予PBS缓冲液免疫。第二组通过口服给予不含病毒的微胶囊免疫。第三组通过口服给予未包封的灭活PEDV免疫。第四组通过口服给予包封的PEDV疫苗免疫,包封约6×10⁶ PFU的PEDV。第五组通过口服给予约6×10⁷ PFU的包封PEDV免疫,包封100 µL PEDV。所有组均在第1天和第3天通过灌胃途径免疫小鼠两次。在第0天(免疫前)、第3天、第6天和第9天,从尾静脉和肛门分别采集200 mg血清样本和粪便样本。将粪便样本在400 µL含有0.01 mol/L EDTA-Na₂的无菌PBS(pH 7.4)中匀浆30分钟,然后在4°C孵育12小时。所有粪便样本的提取上清液通过15,000×g离心10分钟收集,并在-80°C保存[6]。粪便中添加蛋白酶抑制剂用于后续ELISA分析。血清在-80°C保存用于后续ELISA和中和分析。从安乐死小鼠的肠道获得肠灌洗样本(黏液)。将黏液悬浮在400 µL含有0.01 mol/L EDTA-Na₂的无菌PBS(pH 7.4)中,在4°C孵育2小时。然后,所有黏液样本通过15,000×g离心10分钟收集,上清液在-80°C与蛋白酶抑制剂一起保存用于中和分析。

### 2.6. 酶联免疫吸附测定(ELISA)

将ELISA板在4°C用PEDV(6.3×10⁷ PFU)包被18小时,PEDV事先在Vero细胞中培养(如前述章节所述)。用PBS中5%脱脂乳在37°C封闭1.5小时后,用PBST(PBS + 0.1% Tween 20)洗涤3次。将血清和粪便样本(粪便上清液)以复孔加入孔中,检测IgG和IgA等特异性抗体。将血清和粪便样本在37°C孵育1小时,如前洗涤。向每孔加入山羊抗小鼠IgG和IgA抗体-HRP(Invitrogen)(1:5000),在37°C孵育1小时。用PBST进行最后一轮洗涤三次后,使用TMB底物进行显色,在490 nm处测量吸光度。

### 2.7. PEDV中和试验

收集喂食PEDV微胶囊和灭活PEDV的小鼠血清以确定抗体的中和能力。从上述免疫中获得血清和肠灌洗黏液,用0.45 µm滤膜过滤。具体方法如下:取50 µL样本(血清和肠灌洗液)从1:2至1:512进行系列稀释,然后加入含有Vero细胞的96孔板中,设8个重复。将滴度为5×10⁵ PFU的PEDV与DMEM培养基混合,并向细胞板中加入10%热灭活牛血清白蛋白,用稀释的血清和粪便样本溶液包被,然后在37°C与抗体和病毒孵育1小时。然后,将100 µL Vero细胞加入抗体-病毒混合物中,在37°C、5% CO₂培养箱中孵育3天。最后,弃去覆盖的培养基,用无菌PBS(pH=7.4)洗涤三次,用1%结晶紫溶液染色。分析斑块数量的差异以证明其抗体水平。

### 2.8. T细胞增殖

在第二次免疫后第七天,从每组解剖五只小鼠。如前所述,从脾脏制备单淋巴细胞悬液[5]。从每组解剖的五只小鼠脾脏中分离淋巴细胞,在96孔板中以5×10⁵个细胞/孔在RPMI-1640培养基加20%胎牛血清(FCS)中于37°C、5% CO₂培养箱中复孔孵育。然后,在实验组(特异性抗原刺激)和对照组(无抗原刺激)中用0.5和1 µg/mL灭活PEDV刺激细胞48小时。根据制造商说明(Promega),使用Cell Titer 96水溶液非放射性细胞增殖测定法评估T细胞增殖。将噻唑蓝(MTT)溶液(10 µL)移液至每孔进行显色。将板孵育4小时,然后使用Magellan板读数器读取板的OD₄₉₀值,取PEDV刺激数据的平均值与阴性对照孔进行比较。用刺激指数分析增殖率:SI = (OD₄₉₀实验组 − OD₄₉₀培养基)/(OD₄₉₀对照组 − OD₄₉₀培养基)。

### 2.9. 流式细胞术和细胞分选

从每组免疫小鼠的脾脏中获得单淋巴细胞悬液,在第二次免疫后第七天解剖[14]。将分离的脾脏T细胞(5×10⁵个细胞/mL)在RPMI 1640培养基中培养用于流式细胞术染色。将孵育的单淋巴细胞悬液用抗CD11c(PE偶联)和抗CD11b(FITC偶联)抗体以及抗CD23(APC偶联)和抗B220(PE偶联)抗体在无血清的RPMI 1640培养基中染色。所有抗体均购自Miltenyi Biotec。用CD11c(PE偶联)和CD11b(FITC偶联)抗体染色单淋巴细胞,并用FACStar分选以制备CD11c⁺和CD11b⁺细胞。用相同方法制备CD23⁺B220⁺细胞和B220⁺细胞。所有样品用FACSCanto(BD Biosciences)检测,用CellQuest软件分析[15]。在所有情况下,FACStar分选细胞的纯度>98%。用FACSAria(BD Biosciences)将细胞分选到完全培养基(RPMI、1%青霉素-链霉素、1%谷氨酰胺、50 mM β-巯基乙醇)中的CD11c⁺、CD11b⁺、CD23⁺B220⁺和B220⁺群体中。

### 2.10. 细胞因子测定

使用CFX96™实时PCR检测系统(Bio-Rad,Hercules,CA,USA),通过实时qRT-PCR测定免疫小鼠脾淋巴细胞和肠道样本中细胞因子基因和肠道紧密连接基因产物的水平。按照制造商说明,使用总RNA提取试剂盒(TaKara,中国大连)从肠道组织和脾脏中提取总RNA[16]。使用PrimeScript™ RT试剂盒(含gDNA Eraser)(TaKara,中国大连)将总RNA转化为cDNA[17]。将cDNA产物用于SYBR Premix Ex Taq™ II试剂盒(TaKara,中国大连)的实时PCR,所用特异性引物列于表S1[18]。使用Livak方法(2⁻ΔΔCT方法)计算相对于β-actin基因对照的倍数变化[19,20]。

### 2.11. 统计分析

所有样本和实验均进行三次分析,所有组均作为独立测量进行检查,以支持实验中的充分统计学。使用SPSS软件(IBM,New York,USA),采用Bonferroni校正的重复测量方差分析比较各组随时间推移的恢复和定植平均持续时间。使用GraphPad软件,采用单因素重复测量方差分析(ANOVA)和最小显著差异(LSD)检验分析不同组之间的数据。对统计学显著效应(p < 0.05)进行进一步分析[21]。

### 2.12. 伦理声明

所有动物均饲养在BSL2级带HEPA过滤器的负压隔离器中。动物实验方案经东北农业大学机构委员会批准(2018NEAU-131,2018年9月12日),并符合东北农业大学实验动物管理委员会的实验动物指南。

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## 3. 结果

### 3.1. 微胶囊在不同盐溶液、pH值和室温下的优异储存耐受性

作为生物医学材料,微胶囊在盐和酸溶液中释放的能力在临床应用中至关重要。不同盐溶液、pH值和储存时间的释放率如图1所示。微胶囊在PBS组和生理盐水组中的体外释放能力趋势相似,第3天释放率超过50%;第18天释放率分别达到95%和91%。然而,盐酸组第3天仅37.5%,第18天仅63.2%。这些结果表明,微胶囊在盐溶液中易于释放,但最重要的是它们具有耐酸性。不同储存月数后的释放能力显示,前三个月释放率保持在83%以上,在第十五个月仍保持最低释放率41%。这些结果表明,微胶囊在室温避光条件下储存5个月具有优异的储存耐受性。

### 3.2. 微胶囊刺激特异性体液和黏膜免疫

在免疫结束时,通过ELISA检测肠灌洗液和血清中的特异性抗体。ELISA结果显示,随着天数增加,灭活PEDV组和微胶囊组的特异性抗体水平持续升高,如图2所示。对于特异性IgA,PEDV(低剂量)和PEDV(高剂量)微胶囊组在第3天的水平显著高于灭活组(p < 0.05),PEDV(高剂量)微胶囊组的水平显著高于PEDV(低剂量)微胶囊组(p < 0.05)。第6天,PEDV(低剂量)微胶囊组的水平显著高于灭活PEDV组(p < 0.05),而PEDV(高剂量)微胶囊组的水平极显著高于灭活组(p < 0.01)。在第9天检测结束时,两个PEDV微胶囊组的水平均极显著高于灭活组(p < 0.01)。最重要的是,空微胶囊组在整个免疫期间未检测到IgA抗体。

图2B显示,两个PEDV微胶囊组的特异性IgG水平呈现与肠灌洗结果相同的趋势,在第3天显著高于灭活PEDV组(p < 0.05)。第6天和第9天,PEDV微囊化组的特异性IgG水平极显著高于灭活PEDV组(p < 0.01)。这些结果表明,PEDV微胶囊能够以剂量依赖性方式激活黏膜免疫中的特异性黏膜和全身免疫反应。

### 3.3. 特异性IgG和IgA中和PEDV

IgG(图3A)和IgA(图3B)的中和结果如图3所示。结果表明,在体外实验中,PEDV(高剂量)微胶囊组在1:8稀释点后对PEDV感染的中和效果优于PEDV(低剂量)微胶囊组。高剂量PEDV组的50% IgG中和滴度可能为1:256,而PEDV(低剂量)微胶囊组为1:128。PEDV(高剂量)微胶囊组的中和50%滴度高于PEDV(低剂量)微胶囊组。PEDV(高剂量)和PEDV(低剂量)微胶囊组的IgA中和均高于灭活PEDV组,在体外实验中抑制PEDV感染。灭活PEDV组、PEDV(低剂量)微胶囊组和PEDV(高剂量)微胶囊组的IgA 50%中和滴度逐渐增加,在Vero细胞中对PEDV感染的稀释度分别为1:16、1:32和1:64。PEDV(高剂量)微胶囊组的IgG和IgA中和能力高于PEDV(低剂量)微胶囊组。PEDV微胶囊的中和也呈剂量依赖性,表明PEDV(高剂量)微胶囊组比PEDV(低剂量)微胶囊组具有更好的全身和黏膜免疫力。

### 3.4. PEDV微胶囊刺激免疫记忆

为进一步分析微胶囊是否影响细胞介导的免疫,分析T细胞增殖以研究免疫记忆。在第三次免疫后29天,从五只免疫小鼠中获得淋巴细胞单细胞悬液,用于体外实验(表2)。将悬液用PBS(作为对照)、微胶囊(不含PEDV)、灭活PEDV、PEDV(低剂量)微胶囊和PEDV(高剂量)微胶囊刺激。使用0.5 µg/mL和1.0 µg/mL不同剂量的PEDV同时刺激淋巴细胞增殖。在0.5 µg/mL PEDV剂量下,PEDV(低剂量)微胶囊组的数量显著高于PBS组;此外,PEDV(高剂量)微胶囊组的数量显著高于PBS组。微胶囊组、灭活组和PBS组在特异性抗体方面无显著差异。在1 µg/mL PEDV刺激剂量下,两个PEDV微胶囊组均显著高于PBS组。微胶囊组和灭活组与PBS组无显著差异。淋巴细胞增殖结果表明,0.5 µg/mL和1 µg/mL PEDV均可刺激具有免疫记忆的T细胞增殖,产生PEDV微胶囊的免疫反应。

从最后一次加强免疫后的动物中分离单淋巴细胞悬液,在96孔板中以复孔接种,在体外用PEDV和刀豆蛋白A(con A,作为阳性对照)刺激72小时。用刺激指数分析T细胞增殖率:SI = (OD₄₉₀实验组 − OD₄₉₀培养基)/(OD₄₉₀对照组 − OD₄₉₀培养基)。均值之间的差异在* p < 0.05时认为显著,在** p < 0.01时认为极显著。

### 3.5. 微胶囊增强B细胞分化

CD11b和CD11c是树突状细胞的表面标志物,通过流式细胞术分析检测(图4A),来自不同免疫组。结果显示,PBS、微胶囊和灭活PEDV刺激约2.2%的CD11b⁺细胞,PEDV(低剂量)微胶囊和PEDV(高剂量)微胶囊刺激CD11b⁺细胞。相反,CD11c⁺细胞的趋势从PBS组(4.3%)逐渐增加到PEDV(高剂量)微胶囊组(34.6%)。CD23和B220细胞标志物的结果(图4B)表明,除灭活PEDV组外,所有B220⁺细胞均被刺激分化,PBS组和微胶囊组分别达到57.4%和54.4%。对B220⁺细胞的研究表明,与其他组相比,灭活PEDV在口服免疫中更能抑制抗体产生。最重要的是,PEDV(低剂量)微胶囊组和PEDV(高剂量)微胶囊组中B220⁺细胞的百分比均高于灭活PEDV组。然而,PEDV刺激显著增加了B220⁺和CD23⁺细胞;此外,这三组的百分比与灭活PEDV组(46.6%)、PEDV(低剂量)微胶囊组(45%)和PEDV(高剂量)微胶囊组(47.7%)略有不同。

### 3.6. 微胶囊抑制炎症

为验证免疫后的炎症结果,进行qRT-PCR分析mRNA水平的细胞因子表达(图5)。与不同组的样本相比,我们的qRT-PCR结果显示基因表达存在显著差异,如IFN-γ、IL-4、IL-1、TNF-α、IL-17、IL-10、TGF-β、闭合蛋白(occludin)和ZO-1。使用R中的完全连锁算法和Pearson相关度量对热图进行层次聚类分析,使用GraphPad软件绘制。热图结果表明,微胶囊组、PEDV(低剂量)微胶囊组和PEDV(高剂量)微胶囊组中IFN-γ的表达显著高于灭活组,且IFN-γ表达随PEDV剂量增加而增加。IL-4表达在微胶囊组、PEDV(低剂量)微胶囊组和PEDV(高剂量)微胶囊组中呈现相似趋势,刺激Th2免疫反应。灭活组中IL-4表达与IFN-γ表达不同,表明微胶囊可刺激Th1免疫反应。然而,两个PEDV微胶囊组与灭活组相比表现出不同的Th1免疫反应。微胶囊可有效抑制灭活病毒刺激的炎症,降低微胶囊组中IL-1、TNF-α和IL-17的表达。与灭活组相比,微胶囊组中抗炎细胞因子IL-10和TGF-β显著增加。相对紧密连接基因在各种组中也表现出相同的表达趋势。

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## 4. 讨论

2013-2014年的PEDV暴发给全球养猪生产者造成了年度损失。PEDV在新生仔猪中引起的肠道疾病生产力损失使养猪生产者损失数百万美元[2,22]。此前针对另一种猪腹泻病毒——传染性胃肠炎病毒(TGEV)的活疫苗和弱毒疫苗的开发,为IgA和仔猪保护的黏膜免疫机制提供了见解[5,23]。先前的研究表明,灭活PEDV在刺激免疫母猪的特异性IgA抗体方面有效,通过弱毒疫苗保护仔猪获得泌乳免疫[24]。妊娠母猪的泌乳免疫通过肠道-乳腺分泌型IgA(sIgA)轴诱导,这也是保护哺乳仔猪免受PEDV感染的一种有前景且有效的方法[25]。因此,成功的PEDV疫苗必须诱导足够的母源或自泌IgA抗体[26,27]。然而,PEDV没有使用与TGEV免疫计划相同的途径。主要原因是PEDV的抗体滴度没有达到TGEV的滴度以激发成功的免疫反应。更多研究集中在具有不同递送载体的重组疫苗上,以保护抗原不被胃酸消化[28]。然而,抗原的暴露剂量太低,无法刺激特异性抗体如IgA和IgG。重组疫苗表达的抗原非常有限。我们探索了一种将病毒递送至肠道的新可能性形式,刺激特异性黏膜免疫反应,可直接在感染部位中和肠道病毒。

使用离子凝胶化的海藻酸盐微胶囊代表了灭活PEDV载体口服递送系统的一种新的有趣方法。微胶囊可有效包封灭活PEDV抗原,整个病毒颗粒包含在微胶囊中。微胶囊在PBS和生理盐水等盐溶液中具有良好的病毒颗粒释放特性,三天内释放率高于50%。研究表明,特异性IgA抗体在免疫后第二周达到峰值[29]。最重要的特征是微胶囊在盐酸中保护病毒颗粒的完整性,防止病毒颗粒在胃酸中释放后被消化[30]。噬菌体包封和随后的释放动力学表明,微胶囊具有pH响应特性,在适合治疗目的的肠道pH范围内触发噬菌体释放[31]。许多先前研究使用海藻酸盐作为主要包封剂,单独使用或与壳聚糖组合使用[32,33]。壳聚糖-海藻酸盐微球在模拟胃条件下有效保护病毒,显示残留病毒滴度。壳聚糖-海藻酸盐微球在模拟胃条件下充当酸屏障,帮助病毒到达肠道黏膜免疫系统的M细胞。在室温储存下,PEDV微胶囊在前三个月表现出极低的抗原损失,具有良好的储存耐受性,从而维持PEDV抗原的质量。Tan报道,包封在壳聚糖-海藻酸盐微胶囊中的生育三烯醇在酸奶基质中具有有效的储存耐受性[34]。

PEDV最初攻击仔猪的新生肠道上皮细胞和肠道系统,引起腹泻临床症状,但全身淋巴器官无法提供有效的抗体IgG来中和新生猪中的这种病毒。它们主要依赖母源抗体的先天免疫。因此,我们选择携带灭活PEDV的微胶囊来刺激新生仔猪的黏膜免疫系统。针对IgA和IgG的特异性抗体表明,微胶囊刺激黏膜和全身免疫系统产生特异性抗体,如IgA和IgG[5]。在第一次小鼠免疫实验中,微胶囊组的抗体水平高于灭活PEDV组。最重要的是,微胶囊免疫在特异性抗体产生中呈剂量依赖性,高剂量微胶囊组的特异性IgA和IgG水平显著高于低剂量微胶囊组。特异性中和抗体滴度与微胶囊到达黏膜表面的剂量依赖性之间存在密切关系。在微胶囊免疫期间也发现了特异性IgG和IgA的50%中和结果,PEDV(高剂量)微胶囊组的中和活性优于PEDV(低剂量)微胶囊组。特异性IgA抗体的中和效率高于同一组中特异性IgG抗体。主要原因是壳聚糖-海藻酸盐微胶囊在黏膜区域刺激体液免疫,主要由IgA抗体作为主要免疫球蛋白介导,血清来源的IgG也有助于免疫防御[35]。特异性抗体实验表明,微胶囊刺激小鼠的特异性黏膜和全身免疫。然而,小鼠不是PEDV的感染宿主,这意味着在仔猪中仅存在免疫反应的可能性。小鼠和新生猪在免疫和感染方面存在许多差异。

病毒颗粒载体作为蛋白质和肽的口服递送系统显示出更高的潜力,被肠道中派伊尔斑的M细胞摄取[35]。从qRT-PCR结果来看,已报道的PEDV微胶囊免疫与较高水平的IFN-γ产生相关,涉及T辅助1型(Th1)免疫反应[36]。相反,不含PEDV的微胶囊免疫促进与Th2型免疫反应相关的IL-4分泌。PEDV微胶囊免疫后IFN-γ产生高于IL-4产生。细胞免疫反应(Th1)和体液免疫反应(Th2)被打破,Th1型免疫反应占主导地位[6]。特别是,高剂量PEDV微胶囊增强IFN-γ表达,这意味着PEDV微胶囊免疫介导T辅助1型(Th1)免疫反应,壳聚糖-海藻酸盐在细胞免疫反应中发挥免疫调节作用。表达PEDV COE蛋白的靶向树突状细胞肽融合重组干酪乳杆菌的小鼠口服免疫也在仔猪中介导了Th1免疫反应[37]。还分析了细胞因子反应,以比较PEDV微胶囊口服免疫中的炎症、细胞和体液免疫。IL-1和TNF-α也用于分析免疫的安全性和炎症,口服PEDV微胶囊时未刺激炎症反应。更多研究证明了壳聚糖-海藻酸盐在小鼠口服疫苗接种中诱导Th1型免疫反应,壳聚糖效应的研究表明,饲喂壳聚糖的农场动物比未饲喂的动物体重增加更高,但疾病发生率更低[38,39,40]。

DC特异性递送被认为是一种有前景的策略,可促进DC对抗原的有效识别、加工和呈递,从而增强抗原特异性免疫。用于鼻内DNA免疫的靶向树突状细胞的壳聚糖纳米颗粒表明,通过非侵入性鼻内途径靶向pDNA递送可以成为设计低剂量疫苗的策略[41]。在没有佐剂免疫的情况下,疫苗接种期间CD11c⁺的增加促进生发中心诱导和强大的体液反应[42]。注射时,这些含有活化DC的海藻酸盐"疫苗接种节点"在小鼠注射部位吸引了宿主树突状细胞和大量T细胞,同时一些接种的DC迁移到引流淋巴结[43]。与灭活PEDV组相比,壳聚糖-海藻酸盐组(如高剂量PEDV微胶囊和低剂量PEDV微胶囊)在最后一次免疫后显著刺激了CD11c⁺的增加。考虑到体内DC靶向CD11c⁺的优势,壳聚糖-海藻酸盐可能比灭活PEDV更有效地诱导体内DC成熟。壳聚糖-海藻酸盐可首先通过壳聚糖-海藻酸盐在肠道中的免疫调节相互作用有效诱导CD11c⁺的DC成熟,增强特异性免疫反应,诱导黏膜免疫和全身免疫反应后的体液免疫。

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## 5. 结论

口服微囊化包裹了不同滴度的灭活PEDV,由海藻酸盐和壳聚糖组成,到达并呈递至小鼠肠道。它诱导了特异性体液和黏膜免疫。免疫小鼠的特异性抗体(如IgA和IgG)在体外中和了PEDV。口服免疫还刺激了小鼠的免疫记忆。海藻酸盐和壳聚糖不仅作为囊壁材料,还以佐剂功能增强DC和B细胞等免疫细胞的活力。据我们所知,这项微囊化研究是首次在免疫小鼠中包封肠道病毒,尽管PEDV的宿主是猪。因此,应使用灭活和微囊化的PEDV对宿主动物猪进行研究。本研究获得的所有数据可作为该领域进一步研究的重要参考。

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**致谢** 东北农业大学学生创新实践训练。

**免责声明/出版商说明:** 所有出版物中包含的陈述、观点和数据仅为作者和贡献者的个人观点,不代表MDPI和/或编辑的观点。MDPI和/或编辑对内容中提及的任何想法、方法、说明或产品可能造成的任何人身或财产损害不承担责任。

**补充材料** 以下支持信息可在https://www.mdpi.com/article/10.3390/ani13050889/s1下载:表S1。用于炎症和功能分析的qRT-PCR引物。点击此处获取额外数据文件。

**作者贡献** 数据整理,秦子良;形式分析,秦子良、李刚、夏继桥、李璐;方法学,王雯韬、王超、蒋新鹏;资源提供,何新苗;初稿撰写,乃子达、蒋新鹏;审校编辑,蒋新鹏、刘迪。所有作者均已阅读并同意手稿的发表版本。

**机构审查委员会声明** 动物饲养在BSL2级带HEPA过滤器的负压隔离器中。动物实验方案经东北农业大学机构委员会批准(2016NEAU-219,2016年9月13日),并符合东北农业大学实验动物福利伦理和东北农业大学实验动物管理委员会的指南。

**知情同意声明** 不适用。

**数据可用性声明** 一旦本手稿被接受,支持本研究结果的数据将在任何可公开访问的存储库中公开提供。

**利益冲突** 作者声明无财务或商业利益冲突。