EuNPs-mAb fluorescent probe based immunochromatographic strip for rapid and sensitive detection of porcine epidemic diarrhea virus

✅ 全文

基于EuNPs-mAb荧光探针的免疫层析试纸条用于猪流行性腹泻病毒的快速灵敏检测

作者 Fei Xu; Zhiyuan Jin; Siyi Zou; Chaoqun Chen; Qifang Song; Shengchao Deng; Wei Xiao; Xiaoli Zhang; Aiqing Jia; Yong Tang 期刊 Talanta 发表日期 2020 DOI 10.1016/j.talanta.2020.120865 类型 原创研究 (Original Research)

📄 英文摘要 English Abstract

EN

Porcine epidemic diarrhea (PED), induced by porcine epidemic diarrhea virus (PEDV) causes acute diarrhea, vomiting, dehydration and high mortality in neonatal piglets, resulting in significant economic losses in the pig industries. In this study, an immunochromatographic assay (ICA) based on a EuNPs-mAb fluorescent probe was developed and optimized for rapid detection of PEDV. The limit of detection (LOD) of the ICA was 0.218 μg/mL (2.725 × 103 TCID50/mL) and its linear detection range was 0.03125–8 μg/mL (3.91 × 102-105 TCID50/mL). The ICA was also validated for the detection of PEDV in swine stool samples. 60 swine stool samples from southern China were analyzed by the ICA and RT-PCR, and the results showed that the coincidence rate of the ICA to RT-PCR was 86.67%, which was significantly higher than that of AuNPs based ICA. The ICA is sensitive and specific and can achieve on-site rapid detection of swine stool samples. Therefore, the ICA has a great potential for PED diagnosis and prevention.

📄 中文摘要 Chinese Abstract

中文
鸭腺病毒3型(DAdV-3)感染对鸭类健康有严重影响,快速检测方法对于降低该病原体在临床实践中的发病率和死亡率至关重要。DAdV-3血清型属于DAdV-B,是影响水禽最严重的腺病毒。目前检测DAdV-3的方法包括聚合酶链式反应(PCR)、定量PCR(qPCR)、间接酶联免疫吸附试验(ELISA)和环介导等温扩增(LAMP)。前三种方法需要专用仪器和专业操作人员,限制了其在养殖场的应用。虽然LAMP方法可在60–65°C下实现快速扩增,但对引物要求较高且操作不便。因此,亟需一种快速、特异且可现场检测的方法来克服这些局限性。

📋 英文结构化总结 English Structured Summary

全文整理

EN

Background:

Duck adenovirus type-3 (DAdV-3) infections have severe effects on duck health, and rapid detection methods are crucial to reduce the morbidity and mortality associated with this pathogen in clinical practice. The DAdV-3 serotype belongs to DAdV-B and is the most severe adenovirus that affects waterfowl. Existing methods for the detection of DAdV-3 include polymerase chain reaction (PCR), quantitative PCR (qPCR), indirect enzyme-linked immunosorbent assay (ELISA), and loop-mediated isothermal amplification (LAMP). The first three methods require special instruments and professional operators, which limits their application in aquaculture farms. Although the LAMP method enables rapid amplification at 60–65°C, it has high requirements for primers and is not easy to operate. Thus, there is an urgent need for a rapid, specific, and on-site detection method to address these limitations.

Methods:

In this study, we established, optimized, and validated a novel recombinase polymerase amplification (RPA)-lateral flow dipstick (LFD) assay for the detection of DAdV-3. Next, we established a clinical infection model based on the pathogenicity of the DAdV-3 strain and tested the effectiveness of the RPA-LFD assay in controlling an outbreak of DAdV-3 infection. The assay can be performed within 30 min at 42°C. The 5′ ends of the upstream and downstream primers are labeled with fluorescein isothiocyanate (FITC) and biotin, respectively, and the double-labeled product formed after amplification is detected using a dipstick with fluorescent microspheres consisting of highly fluorescent europium (III) nanoparticles (EuNPs).

Results:

Specificity tests indicated no cross-reactivity with other viruses. The detection limit of the assay was 1×10¹ copies/μL. We evaluated 65 clinical samples using RPA-LFD and quantitative polymerase chain reaction (qPCR), and both methods showed a positivity rate of 33.8% and a coincidence rate of 100%. The kappa (κ) value of the RPA-LFD and qPCR assays was 1 (p<0.001). The application of this assay in experimentally infected ducklings reduced the mortality rate from 20 to 8%.

Data Summary:

The detection limit of the RPA-LFD assay was 1×10¹ copies/μL. In the evaluation of 65 clinical samples, both RPA-LFD and qPCR showed a positivity rate of 33.8% and a coincidence rate of 100%, with a kappa value of 1 (p<0.001). Additionally, the assay reduced the mortality rate in experimentally infected ducklings from 20 to 8%.

Conclusions:

The RPA-LFD assay established in this study demonstrated high specificity, sensitivity, rapidity, and efficacy, indicating its potential for rapid detection of DAdV-3 in clinical settings. The findings indicate that the RPA-LFD assay could be performed within 30 min at 42°C, with no cross-reactivity and a detection limit of 1×10¹ copies/μL, and its application reduced mortality in experimentally infected ducklings.

Practical Significance:

The RPA-LFD assay eliminates the need for special equipment and complex operational procedures, making it highly suitable for on-site rapid detection of DAdV-3 in clinical settings, thereby reducing the morbidity and mortality rates associated with DAdV-3 infection in veterinary practice.

📋 中文结构化总结 Chinese Structured Summary

中文

背景:

鸭腺病毒3型(DAdV-3)感染对鸭类健康有严重影响,快速检测方法对于降低该病原体在临床实践中的发病率和死亡率至关重要。DAdV-3血清型属于DAdV-B,是影响水禽最严重的腺病毒。目前检测DAdV-3的方法包括聚合酶链式反应(PCR)、定量PCR(qPCR)、间接酶联免疫吸附试验(ELISA)和环介导等温扩增(LAMP)。前三种方法需要专用仪器和专业操作人员,限制了其在养殖场的应用。虽然LAMP方法可在60–65°C下实现快速扩增,但对引物要求较高且操作不便。因此,亟需一种快速、特异且可现场检测的方法来克服这些局限性。

方法:

本研究建立、优化并验证了一种新型的重组酶聚合酶扩增(RPA)-侧流层析试纸条(LFD)检测方法用于DAdV-3的检测。随后,我们基于DAdV-3毒株的致病性建立了临床感染模型,并测试了RPA-LFD检测方法在控制DAdV-3感染暴发中的有效性。该检测方法可在42°C下30分钟内完成。上游和下游引物的5'端分别标记异硫氰酸荧光素(FITC)和生物素,扩增后形成的双标记产物使用含有高荧光铕(III)纳米颗粒(EuNPs)荧光微球的试纸条进行检测。

结果:

特异性试验表明与其他病毒无交叉反应。该检测方法的检测限为1×10¹ copies/μL。我们使用RPA-LFD和定量聚合酶链式反应(qPCR)对65份临床样本进行检测,两种方法的阳性率均为33.8%,符合率为100%。RPA-LFD与qPCR检测的kappa(κ)值为1(p<0.001)。该检测方法在实验感染雏鸭中的应用将死亡率从20%降低至8%。

数据总结:

RPA-LFD检测方法的检测限为1×10¹ copies/μL。在65份临床样本的评估中,RPA-LFD和qPCR的阳性率均为33.8%,符合率为100%,kappa值为1(p<0.001)。此外,该检测方法在实验感染雏鸭中将死亡率从20%降低至8%。

结论:

本研究建立的RPA-LFD检测方法具有高特异性、高灵敏度、快速性和有效性,表明其在临床环境中快速检测DAdV-3具有潜在应用价值。研究结果表明,RPA-LFD检测方法可在42°C下30分钟内完成,无交叉反应,检测限为1×10¹ copies/μL,其应用降低了实验感染雏鸭的死亡率。

实际意义:

RPA-LFD检测方法无需专用设备和复杂操作流程,非常适合在临床环境中对DAdV-3进行现场快速检测,从而降低兽医实践中DAdV-3感染相关的发病率和死亡率。

📖 英文全文 English Full Text

EN

TYPE Original Research PUBLISHED 13 August 2025 DOI 10.3389/fmicb.2025.1638182 OPEN ACCESS EDITED BY Peirong Jiao, South China Agricultural University, China REVIEWED BY

Mengmeng Zhao, Foshan University, China Yaoyao Zhang, The Pirbright Institute, United Kingdom *CORRESPONDENCE Fangfang Chen fang7828887@126.com These authors have contributed equally to this work † RECEIVED 30 May 2025 ACCEPTED 31 July 2025 PUBLISHED 13 August 2025

Development of a rapid recombinase polymerase amplification-lateral flow dipstick assay for sensitive detection of duck adenovirus type-3 Jiayu Sun 1†, Kewei Liu 1†, Chao Liu 1, Zhenyu Wang 1, Jiaxi Gao 1, Ruya Zhao 1, Long Yuan 1, Yan Shen 2, Jinchun Li 1 and Fangfang Chen 1* Zoonoses Laboratory and Key Laboratory of Veterinary Pathobiology and Disease Control, College of Veterinary Medicine, Anhui Agricultural University, Hefei, China, 2 Anhui Animal Disease Prevention and Control Center, Hefei, China 1

Sun J, Liu K, Liu C, Wang Z, Gao J, Zhao R, Yuan L, Shen Y, Li J and Chen F (2025) Development of a rapid recombinase polymerase amplification-lateral flow dipstick assay for sensitive detection of duck adenovirus type-3. Front. Microbiol. 16:1638182. doi: 10.3389/fmicb.2025.1638182 COPYRIGHT

© 2025 Sun, Liu, Liu, Wang, Gao, Zhao, Yuan, Shen, Li and Chen. This is an open-access article distributed under the terms of the Creative Commons Attribution License (CC BY). The use, distribution or reproduction in other forums is permitted, provided the original author(s) and the copyright owner(s) are credited and that the original publication in this journal is cited, in accordance with accepted academic practice. No use, distribution or reproduction is permitted which does not comply with these terms.

Duck adenovirus type-3 (DAdV-3) infections have severe effects on duck health, and rapid detection methods are crucial to reduce the morbidity and mortality associated with this pathogen in clinical practice. In this study, we established, optimized, and validated a novel recombinase polymerase amplification (RPA)lateral flow dipstick (LFD) assay for the detection of DAdV-3. Next, we established a clinical infection model based on the pathogenicity of the DAdV-3 strain and tested the effectiveness of the RPA-LFD assay in controlling an outbreak of DAdV3 infection. The findings indicated that the RPA-LFD assay could be performed within 30 min at 42°C. Specificity tests indicated no cross-reactivity with other viruses. The detection limit of the assay was 1 × 101 copies/μL. We evaluated 65 clinical samples using RPA-LFD and quantitative polymerase chain reaction (qPCR), and both methods showed a positivity rate of 33.8% and a coincidence rate of 100%. The kappa (κ) value of the RPA-LFD and qPCR assays was 1 (p < 0.001). The application of this assay in experimentally infected ducklings reduced the mortality rate from 20 to 8%. Thus, the RPA-LFD assay established in this study demonstrated high specificity, sensitivity, rapidity, and efficacy, indicating its potential for rapid detection of DAdV-3 in clinical settings. KEYWORDS

DAdV-3, RPA-LFD, detection, clinical diagnosis, specificity

1 Introduction Aviadenovirus is a non-enveloped DNA virus with seven currently known species that can infect chickens or waterfowl, namely, fowl adenovirus (FAdV) A, B, C, D, and E and Duck adenovirus (DAdV) A and B (Hess et al., 1997; Niu et al., 2018; Schachner et al., 2018; Zhuang et al., 2023). Some serotypes, such as FAdV-1, 4, 8a, 8b, 11, DAdV-1 (egg-drop syndrome virus, EDSV), and DAdV-3, can exhibit cross-infection between chickens and waterfowl but produce different clinical signs and pathological changes (Kang et al., 2017; Ono et al., 2001; Wu et al., 2024; Zhang X. et al., 2024; Zhuang et al., 2023). However, DAdV-3 primarily affects Muscovy ducks, which exhibit liver bleeding, pericardial effusion, and renal swelling (Zhang et al., 2016). Recent studies have shown that the virus can also infect chickens, mainly causing hepatitis-hydropericardium syndrome (HHS), bursa necrosis, and disintegration of the gizzard endothelium (Zhang X. et al., 2024). However, some strains (HF-AN-2020) did not cause

obvious clinical symptoms in ducklings but induced interferon (IFN) production in animals (Tan et al., 2024). Significant differences have been observed in the virulence of different strains of DAdV-3, with the primary amino acid differences identified in ORF19B, ORF66, and ORF67 (Tan et al., 2024; Zhang X. et al., 2024). In veterinary clinical practice, timely detection can reduce the morbidity and mortality rates associated with DAdV-3 infection. The DAdV-3 serotype belongs to DAdV-B and is the most severe adenovirus that affects waterfowl. The virions of DAdV-3 are non-enveloped and spherical, with an icosahedral symmetry, and a diameter of 80 nm. The total genome length of the virus is 43,841 bp (Shi et al., 2022). All Aviadenovirus capsids include penton and hexon; the former contains a penton base and fibers, and DAdV-3 has two fiber proteins, fiber-1 and fiber-2, with amino acid homology of 58.42% (Benko et al., 2022; Marek et al., 2014). The distinct hexon amino acids of different Aviadenovirues form the basis of virus typing; in contrast, the fiber protein is relatively conserved and is the main domain for virus invasion of the host; therefore, it is a key target for virus detection and the development of subunit vaccines (Lin et al., 2023; Liu et al., 2024; Marek et al., 2010; Shao et al., 2022; Yin et al., 2019). Although both fiber-1 and fiber-2 are conserved among DAdV-3 strains with different virulence, fiber-2 has a longer coding sequence than fiber-1. Moreover, it exhibits lower homology with fiber proteins from other aviadenoviruses, making it more suitable as a target for DAdV-3 detection. The existing methods for the detection of DAdV-3 include polymerase chain reaction (PCR), quantitative PCR (qPCR), indirect enzyme-linked immunosorbent assay (ELISA), and loopmediated isothermal amplification (LAMP) (Chen et al., 2019; Kaján et al., 2011; Wan et al., 2018; Xie et al., 2011). The first three methods require special instruments and professional operators, which limits their application in aquaculture farms (Asiello and Baeumner, 2011). However, approaches based on these methods cannot simultaneously meet the requirements of high specificity and simple clinical operation. Although the LAMP method enables rapid amplification at 60–65°C,

it has high requirements for primers and is not easy to operate (Li et al., 2024). Thus, there is an urgent need for a rapid, specific, and on-site detection method to address these limitations. The recombinase polymerase amplification (RPA)-lateral flow dipstick (LFD) assay is a novel isothermal amplification technique that can achieve amplification of the target gene fragment within 20–40 min at 37–42°C and is often used for the detection of microorganisms and mutated genes (Chang et al., 2024; Hong et al., 2024; Xu et al., 2024). This method eliminates the need for special equipment and complex operational procedures, making it highly suitable for on-site rapid detection. The RPA-LFD assay operates based on isothermal amplification and lateral flow visualization, with detailed principles shown in Figure 1. The 5′ends of the upstream and downstream primers are labeled with fluorescein isothiocyanate (FITC) and biotin, respectively, and the double-labeled product formed after amplification is detected using a dipstick with fluorescent microspheres consisting of highly fluorescent europium (III) nanoparticles (EuNPs). The assay facilitates the visualization of clinical samples, and the long fluorescence decay lifetime of the EuNPs improves the specificity and sensitivity of detection (Du et al., 2022; Xu et al., 2020). Thus, to address the limitations of existing methods, in this study, based on a DAdV-3 strain (CH-AN-2022) isolated by our research group, DAdV-3-fiber-2 was used as the target gene to establish a visual fluorescent RPA-LFD rapid detection assay for clinical prevention and control of the virus.

2 Materials and methods 2.1 Animals Specific pathogen-free (SPF) duck embryos were purchased from the Chinese Academy of Agricultural Sciences (Harbin, Heilongjiang, China). SPF ducks aged 3 days were incubated and raised at the SPF

FIGURE 1

The basic principle underlying the detection of DAdV-3 through the RPA-LFD assay. (A) The recombinase polymerase amplification (RPA) reaction was applied to amplify double-stranded DNA fragments labeled with fluorescein isothiocyanate (FITC) and biotin. (B) 70 μL of the diluted RPA amplification product is dropped onto the lateral flow dipstick (LFD). Rabbit anti-FITC antibody was conjugated to fluorescent microspheres and subsequently applied onto the conjugate pad, while streptavidin and goat anti-rabbit antibody were fixed at the test line (T) and control line (C) positions, respectively. (C) A positive result was demonstrated by the simultaneous appearance of both the T and C. The appearance of only the C signified a negative. A result was deemed inconclusive or doubtful if only the T appeared. The fluorescence immunoassay analyzer can measure the fluorescence intensity of the T line and the C, and calculate the T/C value.

Animal Incubation Center of Anhui Agricultural University. Ninety 3-day-old Muscovy ducks were procured from a duck farm located in Anhui Province. The ducks were housed in a healthy and controlled setting, with the temperature maintained at 30–34°C in accordance with the age and behavior of the birds.

Primer 2.2 Establishment of the RPA-LFD assay 2.2.1 Coupling of biomolecules to microspheres Primer sequences (5′–3′) DAdV-3-Fiber2-F1 CAATCACTCTCCGTTAGAACTAATCCTCAAG DAdV-3-Fiber2-F2 CAAGGAGAGAAAGAGTTAGGCATCAACATC

DAdV-3-Fiber2-F3 CACATCGTGCATAACACTAGACAACGGAGGC DAdV-3-Fiber2-R1 CATACGATCTTGGCATAGTATGCGCACGGAAAC DAdV-3-Fiber2-R2 CGTAACAGACCCTGCTCCGCAGCACACTTG DAdV-3-Fiber2-R3 CACACTTGGGCTTGTGTCTTCTGAAGTGTGTC

First, the microspheres were washed and activated; 50 μL of highly fluorescent microspheres (100 mg/mL) (Bangs Laboratories, United States) were fully washed twice with 500 μL 4-morpholine ethanesulfonic acid (MES) buffer (10 mM, pH = 6.0); the supernatant was discarded after centrifugation at 4°C at 14,000 × g for 15 min; and the microspheres were resuspended in 200 μL of MES buffer and continuously stirred. Next, 250 μL of 1-ethyl-3-(3dimethylaminopropyl) carbodiimide hydrochloride (EDC; 10 mg/ mL) and N-hydroxysulfosuccinimide sodium salt (NHS) solution (10 mg/mL) were added successively, followed by ultrasound treatment in a water bath for 5 min and dispersed in a thermostatic oscillator at 30°C and 200 rpm for 30 min. Next, the microspheres were coupled to antibodies. The solution was washed twice with 500 μL of phosphate buffer (10 mM, pH 7.4) solution, and the microspheres were resuspended in 1 mL of phosphate buffer. Subsequently, 50 μL of rabbit anti-FITC antibody (Bioss, Beijing, China) was added for coupling. Next, dispersion and washing with phosphate buffer were performed using the methods described above. After washing, the microspheres were resuspended in 500 μL of sealing solution [30 mM ethanolamine and 1% w/v bovine serum albumin (BSA)], dispersed by the same method, and washed in a final wash buffer (sealing solution and 0.05% w/v Tween 20, pH = 8.0) before resuspension in 1 mL of phosphate buffer with 0.1% BSA. Finally, the labeled microspheres were sent to Biohan Biotechnology (Hefei, China) for the preparation and assembly of test dipsticks. Fluorescent microspheres were uniformly sprayed on the bonding pad at 5 μL/cm. The test line (T) was coated with rabbit antiFITC antibody (Bioss, Beijing, China), and the control line (C) was coated with goat anti-rabbit immunoglobulin G (Artron, Shandong, China) at 1 mg/mL. The dipsticks were stored in a desiccant aluminum foil bag away from light at room temperature.

2.4 Screening of optimal reaction conditions for RPA-LFD assays

The full-length sequence of the fiber-2 gene of DAdV-3 was downloaded from the GenBank database (accession number: OP432083). We designed nine primer pairs (F1/R1, F1/R2, F1/R3, F2/R1, F2/R2, F2/R3, F3/R1, F3/R2, and F3/R3) for the fiber-2 gene using Oligo 6 software and validated and optimized them using PCR, qPCR, and RPA-LFD, respectively. The primers were synthesized by Sangon Biotech (Shanghai, China), and their sequences are listed in Table 1. First, the PCR reaction system (total volume 20 μL) consisted of the following components: PCR mixture, 10 μL; forward primer (10 μM), 0.5 μL; reverse primer (10 μM), 0.5 μL; DAdV-3 DNA, 1 μL; and double-distilled water (ddH2O), 8 μL. The primer pairs were initially validated by PCR to

The optimum conditions of the above assay were further optimized, and the optimum buffer type, temperature, and dilution ratio were screened. The 70 μL diluted amplified product was added to the dipsticks. After 5–10 min, the fluorescence signal intensity of the C and T lines was read by a fluorescence immunoassay analyzer (HIT-91A, Biouhan, Hefei, China), and the T/C value was calculated. Each group of experiments was repeated 3 times to calculate the mean (M) ± standard deviation (SD).

Frontiers in Microbiology confirm amplification feasibility. Subsequently, the primers were further screened using qPCR. DAdV-3 DNA was diluted 10-, 100-, and 1,000-fold as templates, and qPCR was performed with each sample analyzed in triplicate (mean values were calculated). The primers were deemed qualified if: (i) gel electrophoresis confirmed that the PCR amplification products of the target gene were free of primer dimers; (ii) melting curves analysis showed no non-specific peaks; and (iii) qPCR amplification curves exhibited specific single peaks with the lowest average Ct values. Ultimately, the primer pairs with the highest amplification efficiency were selected for subsequent experiments. This approach was based on the methods employed by other researchers who have performed primer selection for the RPA-LFD assay (Onchan et al., 2022). The RPA assay was performed according to the manufacturer’s instructions (LeSun Bio, Wuxi, China). The reaction mixtures contained 25 μL of reaction buffer, 16 μL of ddH2O, lyophilized enzyme powder, 2 μL of the FITC-labeled forward primer (10 μM), 2 μL of the biotin-labeled reverse primer (10 μM), 2 μL of pMD18T-fiber-2 recombinant vector template, and 3 μL of activator. After all the reaction components were added, we performed manual flicking and brief centrifugation. The amplification was performed at 37°C for 20 min. The amplified product was then diluted 10 times with 1% skim milk powder and tested with the dipstick. After 5–10 min, the results were observed (Figure 1). A positive result was demonstrated by the simultaneous appearance of both the T and C lines. Conversely, a negative result was evidenced by the appearance of only the C line, which indicated the absence of the target gene fragment. The results were deemed inconclusive or doubtful if only the T line appeared.

2.4.1 Optimization of the buffer type The amplified product was diluted 10-fold with phosphatebuffered saline with Tween 20 (PBST), 1% skim milk powder, or 03 frontiersin.org Sun et al. 10.3389/fmicb.2025.1638182

2.6 Clinical sample analysis

Blocker™ Casein in phosphate-buffered saline (PBS; Thermo Fisher, United States) and then added to the dipsticks.

To evaluate the concordance rate between the RPA-LFD assay and qPCR, 65 cloacal samples collected from three duck farms with clinical outbreaks were tested using both the established RPA-LFD assay and qPCR, and their results were compared. The qPCR assay was performed following a previously reported protocol (Zhang X. et al., 2024). The cycle threshold (Ct = 37), derived from amplification of the positive control plasmid pMD18-T-DAdV-3-fiber-2 at a concentration of 1 × 102 copies/μL, was defined as the cutoff value. Results were interpreted as follows: samples were classified as positive if the measured Ct value was less than 37, and negative if the measured Ct value exceeded 37. Each sample was analyzed in triplicate, and the mean Ct value was computed for final interpretation. The consistency between the two methods was evaluated by calculating the Kappa (κ) coefficient and p-value. κ is used to measure the degree of consistency in the data, and its value ranges between −1 and 1; additionally, the p-value represents the probability that the observed consistency occurred by chance. The closer the κ value is to 1, the higher the consistency between the indicators; on the other hand, the smaller the p-value, the more significant the consistency between the indicators. The formula for calculating the relevant detection indicators is presented below, in which a, b, c, and d are the numbers of samples counted, and n is the total number of samples: κ = (Po − Pe)/(1 − Pe), Po = (a + d)/(a + b + c + d), Pe = [(a + c)(b + d) + (a + b)(c + d)]/ (a + b + c + d)2, where Po is the actual coincidence rate, Pe is the theoretical coincidence rate, and n is the total number of samples (Table 3).

2.4.2 Optimization of temperature To identify the optimal reaction temperature, the RPA reaction was performed at six temperatures (30°C, 33°C, 36°C, 39°C, 42°C, and 45°C) controlled by the PCR instrument. At the end of the reactions, the RPA product was diluted 10-fold with 1% skim milk powder.

2.4.3 Optimization of the dilution ratio Highly viscous amplification products must be appropriately diluted to allow testing of the target gene amplification products. At the end of the reaction, the RPA amplification products were diluted 5-, 10-, 20-, 30-, 40-, 50-, 60-, 70-, and 80-fold in 1% skim milk powder (Table 2).

2.5 Analysis of the specificity, sensitivity, and limit of blank of the RPA-LFD assay The specificity, sensitivity, and limit of blank (LOB) of the RPA-LFD assay were also verified. The detection method for the amplified products was the same as described above in section 2.3.

2.5.1 Specificity analysis The DNA of DAdV-3, FAdV-4, DuCV-1 (Duck circovirus-1), DAdV-2, FAdV-8a, and the cDNA of MDPV (Muscovy duck parvovirus), DHV (Duck hepatitis virus), H7, and H9 subtypes of AIV (Avian Influenza virus) were used as templates for RPA specificity analysis to identify cross-reactions with other viruses in the assay. At the end of the reaction, the RPA amplification products were diluted 10-fold with 1% skim milk powder. The experiment was repeated 3 times to calculate the M ± SD.

2.7 Clinical detection To validate the efficacy of the timely detection with RPA-LFD for the effective prevention and control of DAdV-3 infections in a clinical setting, this study was also conducted in a farm. Thirty 3-day-old SPF ducks were inoculated with 0.2 mL of duck embryo allantoic fluid containing 2 × 105 TCID50/0.1 mL by subcutaneous injection on the neck and back. Two days later, the infected ducklings were marked and randomly assigned to two groups and placed among 45 3-day-old healthy Muscovy ducks, designated as Group 1 and Group 2. After 4 days of mixed culture, the SPF ducks were culled based on the markers and euthanized. During the mixed culture period, if the ducklings in Group 1 showed poor mental conditions or mild diarrhea symptoms, cloacal swabs were collected and promptly tested using RPA-LFD, and positive Muscovy ducks were culled. Group 2 was fed in accordance with normal procedures without any detection and culling, and the records of the ducklings were maintained for 30 days.

2.5.2 Sensitivity analysis Serial dilutions of pMD18-T-fiber-2 plasmid standards ranging from 106 to 100 copies/μL were used as templates. Optimized conditions for the RPA-LFD assay were used in the sensitivity test. The experiment was repeated 3 times to calculate the M ± SD.

2.5.3 LOB analysis The RPA assay system was tested with 20 samples of 1% skim milk powder buffer; the results were recorded on a fluorescence immunoassay analyzer; and the data were collated and analyzed. The formula used to calculate LOB was as follows: M + 2 × SD. TABLE 2 Dilution ratio of RPA products.

Reagent name RPA products (μL) 1% skim milk powder (μL) Dilution ratio 5 10 20 30 40 50 60 70 80 14.00 7.00 3.50 2.33 1.75 1.40 1.17 1.00 0.88 56.00 63.00 66.50 67.67 68.25 68.60 68.83 69.00 69.12 Frontiers in Microbiology

04 frontiersin.org Sun et al. 10.3389/fmicb.2025.1638182

The determination of virus TCID50 and the handling of the experimental animals were performed as previously reported (Zhang X. et al., 2024).

the results showed that the amplified products of F1/R1, F2/R1, F3/ R3, and F3/R1 showed the clearest bands on the dipsticks. In summary, the primer pair F1/R1 was chosen as the optimal pair for the RPA-LFD assay.

3 Results 3.2 Optimization of RPA condition 3.1 Screening of the best primer pair for RPA

The optimal conditions for highly efficient RPA were determined by evaluating different buffer types, temperatures, and dilution ratios. The amplified products were diluted 10-fold with 1% skim milk powder, PBST, and Blocker™ casein in PBS. As shown in Figure 3A, the mean T/C values with the three diluents were 5.6183, 0.115667, and 0.0995, respectively. Therefore, 1% skim milk powder was identified as the optimal diluent for the RPA products. RPA products were diluted at gradients of 5- to 80-fold as shown in Table 2. The results are shown in Figure 3B. When the products were diluted 5-, 10-, 20-, 30-, 40-, 50-, 60-, 70-, and 80-fold, the mean T/C values were 2.6214, 4.4628, 0.9683, 0.5707, 0.3302, 0.2247, 0.2366, 0.1646, and 0.1415, respectively. The RPA products had relatively small T/C values at dilutions greater than 20-fold. A 10-fold dilution resulted in the highest T/C value. Therefore, 10-fold dilution was identified as the optimal dilution level for RPA products. The RPA reaction was also performed within a specific temperature range. The results are shown in Figure 3C. The amplification efficiency tended to increase from 33 to 42°C, while it decreased from 42 to 45°C. Thus, the optimal amplification temperature for the RPA-LFD assay was identified as 42°C.

PCR, qPCR, and RPA-LFD were used to select the optimal primer pairs. First, we performed PCR verification using the nine pairs of primers designed in this study. After electrophoresis on a 1.5% agarose gel, we observed the clearest bands when using 1 μL of the primers, as shown in Figure 2A. All nine primer pairs (F1/R1: 275 bp; F1/R2: 242 bp; F1/R3: 220 bp; F2/R1: 244 bp; F2/R2: 215 bp; F2/R3: 190 bp; F3/R1: 212 bp; F3/R2: 180 bp; F3/R3: 158 bp) could amplify the target fragment and yielded products with the expected size; however, the F1/R2, F1/R3, F2/R2, F2/R3, F3/R2, and F3/R3 amplification products had obvious primer dimers. In contrast, F1/R1, F2/R1, and F3/R1 produced clear bands without primer dimers. Furthermore, 10-, 100-, and 1,000-fold DNA dilutions were used as templates, and qPCR was used to evaluate the primers. The amplification efficiencies of the different primers are shown in Table 4. When F1/R1 was used as the primer pair, the amplification efficiency was the highest. Analysis of the melting curves revealed that F1/R2 and F3/R3 showed non-specific amplification (Figure 2B). Nine primer pairs were used to amplify the gene product using RPA, and

TABLE 3 Chi-square test was conducted on a four-grid table of data. Method RPA-LFD Sample 3.3 Sensitivity, specificity, and LOB determination of the RPA-LFD assay qPCR Positive Negative Total Positive

a b a+b Negative c d c+d Total a+c b+d a+b+c+d

The sensitivity of the RPA-LFD assays was evaluated using the pMD18-T-fiber-2 plasmid diluted to concentrations ranging from 106 to 100 copies/μL. The 1 × 101 copies/μL sample showed a significantly higher T/C value compared to the negative control (Figures 4A,B). The detection limit for the RPA-LFD assay was

(a) Both qPCR and RPA-LFD positive. (b) qPCR negative and RPA-LFD positive. (c) qPCR positive and RPA-LFD negative. (d) Both qPCR and RPA-LFD negative. FIGURE 2

Screening of optimal primer pairs. (A) Nine primer pairs (F1R1, F1R2, F1R3, F2R1, F2R2, F2R3, F3R1, F3R2, and F3R3) for PCR amplification, and the amplified fragments were visualized by 1.5% agarose gel electrophoresis. The target fragment sizes were 275, 242, 220, 244, 215, 190, 212, 180, and 158 bp, respectively. (B) qPCR reactions with nine primer pairs, obtaining the melt curves (DAdV-3 DNA 1:1,000 dilution). The data are presented as the mean values (n = 3).

Frontiers in Microbiology 05 frontiersin.org Sun et al. 10.3389/fmicb.2025.1638182

1 × 101 copies/μL. The specificity of the RPA-LFD assay was tested using nucleic acids of FAdV-4, DuCV-1, DAdV-2, FAdV-8a, MDPV, DHV, AIV-H7, and AIV-H9. Only DAdV-3 yielded positive signals (both T and C lines) in the RPA-LFD assay. Notably, FAdV-4, DuCV-1, DAdV-2, FAdV-8a, MDPV, DHV, AIV-H7, and AIV-H9 did not show cross-reactivity (Figures 4C,D), indicating that the established RPA-LFD assay had excellent specificity. LOB analysis was performed to determine the lowest signal intensity distinguishable from blank samples. Using 20 blank samples, the LOB of the RPA-LFD assay was calculated as 0.037285 based on the formula LOB = M + 2SD (Figures 4E,F).

(p < 0.001), indicating almost perfect agreement between the two methods.

3.5 Detection and analysis of the clinical efficacy of the RPA-LFD assay In Group 1, four DAdV-3-positive Muscovy ducks identified by RPA-LFD were culled within the first 10 days of the 30-day co-infection period [mortality rate, 8% (4/45)]. In contrast, in Group 2, after 30 days of observation, nine ducks died [mortality rate, 20% (9/45)], and the final positive Muscovy duck was identified on day 28. These results indicate that timely detection and culling substantially reduced the mortality rate, from 20 to 8%.

3.4 Validation of the RPA-LFD assay by using clinical samples 4 Discussion

The established RPA-LFD was used to evaluate 65 suspected DAdV-3 cloacal swab samples (Figure 5A), and the results for all samples were verified using qPCR (Figure 5B). As shown in Table 5, the positivity rate of the RPA-LFD assay was 33.8% (22/65), while the positivity rate in qPCR assessments was also 33.8% (22/65), with both methods showing a coincidence rate of 100% (65/65). The κ value of the RPA-LFD and qPCR assays was 1

The clinical experimental findings of this study highlighted the critical role of timely intervention in controlling DAdV-3 infections. Specifically, the mortality rate of DAdV-3-infected Muscovy ducks reached 20%, while their long-term sporadic death rate was significantly lower than that of SPF ducklings, likely due to the higher susceptibility of SPF ducklings to the virus. Importantly, prompt isolation of sick ducks reduced the mortality rate to 8%, underscoring that timely detection and isolation are pivotal for preventing and controlling DAdV-3. Against this backdrop, the development of a rapid and reliable detection method is imperative. Existing assays for the detection of DAdV-3 cannot simultaneously meet the requirements of high specificity and ease of operation (Ather et al., 2024; Wan et al., 2018; Xie et al., 2011). In contrast, the sensitivity of our newly developed RPA-LFD assay was as high as 1 × 101 copies/μL, and the detection results could be obtained within 30 min. This level of sensitivity is comparable to that of qPCR (Table 5), indicating the potential of the RPA-LFD assay as a new approach for clinical DAdV-3 detection. This method has also been applied by researchers to test the sensitivity and specificity for other avian viruses; for instance, the minimum detection limits for infectious bursal disease virus (IBDV), AIV (H5, H7, and H9 subtypes), and Newcastle disease virus (NDV) were 101, 102, and 102

TABLE 4 qPCR Ct values of DAdV-3 DNA at different dilutions. Primer qPCR 10-fold 100-fold 1,000-fold F1R1 18.28 23.73 27.58 F1R2 18.71 23.48 26.92 F1R3 19.50 23.22 27.17 F2R1 19.36 23.74 27.83 F2R2 18.71

23.38 27.21 F2R3 18.34 23.24 27.32 F3R1 19.35 23.69 27.75 F3R2 19.08 23.50 27.68 F3R3 17.96 23.34 27.76 FIGURE 3

Screening of optimal buffer types, dilution ratio, and temperature in RPA assay. (A) The RPA amplification product was diluted using 1% skimmed milk powder, PBST, and Blocker™ Casein in PBS. The fluorescence immunoassay analyzer can measure the fluorescence intensity of the T and C, and calculate the T/C value. (B) Dilute the RPA amplification product with 1% skim milk powder to 5-, 10-, 20-, 30-, 40-, 50-, 60-, 70-, and 80-fold, respectively, and the resulting T/C values are 2.6214, 4.4628, 0.9683, 0.5707, 0.3302, 0.2247, 0.2366, 0.1646, and 0.1415, respectively. (C) The T/C values were measured at different RPA amplification temperatures (30, 33, 36, 39, 42, and 45°C). The fluorescence immunoassay analyzer can measure the fluorescence intensity of the T and C, and calculate the T/C value. All data in A–C are presented as M ± SDs (n = 3).

Performance analysis of the RPA-LFD assay. (A) The RPA-LFD assay is employed to detect the values of T/C under different concentrations of pMD18T-fiber-2 plasmid (100–106 copies/μL) The data are presented as M ± SDs (n = 3). ***p < 0.0001, **p < 0.001, *p < 0.01, and nsp > 0.05. (B) Representative dipsticks for plasmid concentrations in A. The fluorescence signal intensity of T and C lines are calculated by a fluorescence immunoassay analyzer. The position of the C value is between 60 and 160, and the position of the T value is between 320 and 420. (C) The specificity of the RPA-LFD assay was assessed using FAdV-4, DuCV-1, DAdV-2, FAdV-8a, MDPV, DHV, AIV-H7, and AIV-H9 viral nucleic acids. The T/C value is calculated by a fluorescence immunoassay analyzer. The data are presented as M ± SDs (n = 3). (D) Specificity strip readouts: corresponding to the LFD results for the viruses in C. The position of the C value is between 60 and 160, and the position of the T value is between 320 and 420. (E) To determine the LOB for the RPA-LFD assay, a set of 20 1% skim milk powder buffer samples were employed as amplification templates for assay, and read the T/C values. Based on the calculation LOB = M + 2SD, the result obtained is 0.037285. (F) Detect the fluorescence signal intensity of T and C for the amplification products of 20 1% skim milk powder buffer samples. The position of the C value is between 60 and 160, and the position of the T value is between 320 and 420.

The RPA-LFD and qPCR assays were employed to analyze a total of 65 clinical samples. (A) The T/C values were obtained by detecting 65 samples using the RPA-LFD assay. (B) Ct values were obtained through qPCR analysis of 65 samples. The “+” sample is a positive plasmid. A sample was considered positive when the difference between 37 and the cycle threshold (Ct value; 37-Ct) was greater than 0, and negative when the difference was less than 0. The data are presented as the means ±SDs (n = 3).

TABLE 5 Detection results of 65 clinical samples by RPA-LFD and qPCR assays. Sample Positive RPA-LFD qPCR Positive Negative Total 22 0 22 Negative 0 43 43 Total 22 43 65

copies/μL, respectively, with no cross-reactivity observed (Wang et al., 2023; Wang et al., 2020; Zhang Z. et al., 2024). In the current study, 65 cloacal samples tested in this study were collected from Frontiers in Microbiology

Kappa (κ) p-value of kappa 1 <0.001 three duck farms experiencing clinical outbreaks as suspected positive specimens, which may explain the relatively high positivity rate (33.8%). 07 frontiersin.org Sun et al.

10.3389/fmicb.2025.1638182

Beyond method validation, our analysis of detection targets and viral tropism provided additional insights. The fiber-2 gene was selected as the target due to its high conservation across all DAdV-3 strains, ensuring the assay’s applicability to diverse DAdV-3 isolates. Consistent with reports that the intestine is the primary excretory organ of fowl adenoviruses (including DAdV-3) (Shi et al., 2022; Zhang X. et al., 2024), cloacal swabs effectively indicated viral presence in our study. Notably, positive results in this study suggest that DAdV-3 is not only detected in Muscovy ducks but also in different breeds of elderly ducks, including 180-day-old Peking ducks, 240-dayold white ducks, and 200-day-old Shaoxing ducks, indicating that DAdV-3 can spread not only within Muscovy ducks but also across breeds. These results suggest that DAdV-3 can infect not only ducklings but also older ducks; however, the specific transmission mechanism requires further study. This study has certain limitations. First, the efficacy of the assay was validated under controlled experimental conditions, which may fail to fully recapitulate the intricate nature of natural clinical settingsencompassing variations in pathogen load, fluctuations in host immune competence, and co-infections prevalent in poultry production systems. Second, the number and diversity of duck breeds employed for validation were relatively restricted, potentially compromising the statistical power and generalizability of the findings. Furthermore, the current cost of the method remains relatively high, which may impede its widespread adoption in resource-limited field settings. Consequently, the clinical applicability and robustness of the assay including its performance under field conditions and consistent detection across diverse duck populationswarrant further validation, while cost optimization is also imperative. Notably, the optimized RPA-LFD system holds promise for extension to the detection and clinical elimination of other avian pathogens (including viruses and bacteria), with particular potential utility in the screening and culling of oncogenic pathogens.

The original contributions presented in the study are included in the article/supplementary material, further inquiries can be directed to the corresponding author. The authors declare that no Gen AI was used in the creation of this manuscript.

JS: Methodology, Data curation, Software, Writing – original draft. KL: Data curation, Methodology, Software, Writing – original draft. CL: Writing – review & editing, Formal analysis, Validation. ZW: Writing – review & editing, Formal analysis, Validation. JG: Data curation, Writing – review & editing. RZ: Validation, Writing – review & editing. LY: Writing – review & editing, Software. YS: Resources, Writing – review & editing. JL: Writing – review & editing. FC: Writing – review & editing, Conceptualization, Supervision, Funding acquisition, Project administration.

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# 用于鸭腺病毒3型灵敏检测的快速重组酶聚合酶扩增-侧向层析试纸条检测法的建立

**类型** 原创研究 **发表日期** 2025年8月13日 **DOI** 10.3389/fmicb.2025.1638182 **开放获取** **编辑** 焦培荣,华南农业大学,中国 **审稿人**

赵萌萌,佛山大学,中国 张耀耀,英国皮布赖特研究所 *通讯作者* 陈芳芳 fang7828887@126.com † 这些作者对本研究做出了同等贡献 † 收稿日期 2025年5月30日 录用日期 2025年7月31日 发表日期 2025年8月13日

**用于鸭腺病毒3型灵敏检测的快速重组酶聚合酶扩增-侧向层析试纸条检测法的建立**

孙佳宇1†,刘可为1†,刘超1,王振宇1,高嘉希1,赵茹雅1,袁龙1,申燕2,李金春1,陈芳芳1*

1 安徽农业大学兽医学院,人畜共患病实验室与兽医病理生物学及疾病控制重点实验室,合肥,中国 2 安徽省动物疫病预防与控制中心,合肥,中国

孙佳宇,刘可为,刘超,王振宇,高嘉希,赵茹雅,袁龙,申燕,李金春,陈芳芳(2025)用于鸭腺病毒3型灵敏检测的快速重组酶聚合酶扩增-侧向层析试纸条检测法。 《微生物学前沿》16:1638182. doi: 10.3389/fmicb.2025.1638182

**版权**

© 2025 孙佳宇,刘可为,刘超,王振宇,高嘉希,赵茹雅,袁龙,申燕,李金春,陈芳芳。本文为开放获取文章,依据知识共享署名许可协议(CC BY)条款分发。在其他论坛使用、分发或复制本文时,须注明原作者和版权所有者,并引用本期刊的原始发表信息,符合公认的学术规范。不符合上述条件的使用、分发或复制行为均不被允许。

鸭腺病毒3型(DAdV-3)感染对鸭的健康影响严重,快速检测方法对于降低该病原在临床实践中的发病率和死亡率至关重要。本研究建立、优化并验证了一种用于检测DAdV-3的新型重组酶聚合酶扩增(RPA)-侧向层析试纸条(LFD)检测法。随后,我们基于DAdV-3毒株的致病性建立了临床感染模型,并测试了RPA-LFD检测法在控制DAdV-3感染暴发中的有效性。结果表明,RPA-LFD检测法可在42°C条件下30分钟内完成检测。特异性测试显示与其他病毒无交叉反应。该检测法的检测限为1×10¹拷贝/μL。我们使用RPA-LFD和定量聚合酶链式反应(qPCR)对65份临床样本进行了检测,两种方法的阳性率均为33.8%,符合率为100%。RPA-LFD与qPCR检测法的Kappa(κ)值为1(p<0.001)。该检测法在实验感染雏鸭中的应用使死亡率从20%降至8%。因此,本研究建立的RPA-LFD检测法具有高特异性、高灵敏度、快速性和高效性,表明其在临床环境中快速检测DAdV-3方面具有应用潜力。

**关键词**

DAdV-3,RPA-LFD,检测,临床诊断,特异性

## 1 引言

禽腺病毒(Aviadenovirus)是一种无囊膜DNA病毒,目前已知的七个种可感染鸡或水禽,即禽腺病毒(FAdV)A、B、C、D和E以及鸭腺病毒(DAdV)A和B(Hess等,1997;Niu等,2018;Schachner等,2018;Zhuang等,2023)。某些血清型,如FAdV-1、4、8a、8b、11,DAdV-1(产蛋下降综合征病毒,EDSV)和DAdV-3,可在鸡和水禽之间表现出交叉感染,但产生不同的临床症状和病理变化(Kang等,2017;Ono等,2001;Wu等,2024;Zhang X.等,2024;Zhuang等,2023)。然而,DAdV-3主要影响番鸭,表现为肝脏出血、心包积液和肾脏肿胀(Zhang等,2016)。近期研究表明,该病毒也可感染鸡,主要引起肝炎-心包积液综合征(HHS)、法氏囊坏死和胃内皮崩解(Zhang X.等,2024)。但部分毒株(HF-AN-2020)在雏鸭中未引起明显临床症状,而是诱导动物产生干扰素(IFN)(Tan等,2024)。DAdV-3不同毒株的毒力存在显著差异,主要氨基酸差异位于ORF19B、ORF66和ORF67(Tan等,2024;Zhang X.等,2024)。在兽医临床实践中,及时检测可降低DAdV-3感染相关的发病率和死亡率。

DAdV-3血清型属于DAdV-B,是影响水禽最严重的腺病毒。DAdV-3病毒粒子无囊膜,呈球形,具有二十面体对称结构,直径为80 nm。病毒基因组总长度为43,841 bp(Shi等,2022)。所有禽腺病毒衣壳均包含五邻体和六邻体;前者包含五邻体基底和纤突,DAdV-3具有两种纤突蛋白,纤突-1和纤突-2,氨基酸同源性为58.42%(Benko等,2022;Marek等,2014)。不同禽腺病毒的特异性六邻体氨基酸构成病毒分型的基础;相比之下,纤突蛋白相对保守,是病毒入侵宿主的主要结构域,因此是病毒检测和亚单位疫苗开发的关键靶标(Lin等,2023;Liu等,2024;Marek等,2010;Shao等,2022;Yin等,2019)。尽管纤突-1和纤突-2在不同毒力的DAdV-3毒株中均保守,但纤突-2的编码序列长于纤突-1。此外,纤突-2与其他禽腺病毒纤突蛋白的同源性较低,使其更适合作为DAdV-3检测的靶标。现有的DAdV-3检测方法包括聚合酶链式反应(PCR)、定量PCR(qPCR)、间接酶联免疫吸附试验(ELISA)和环介导等温扩增(LAMP)(Chen等,2019;Kaján等,2011;Wan等,2018;Xie等,2011)。前三种方法需要专用仪器和专业操作人员,限制了其在养殖场中的应用(Asiello和Baeumner,2011)。然而,基于这些方法的技术无法同时满足高特异性和临床操作简便性的要求。尽管LAMP方法可在60–65°C下实现快速扩增,但其对引物要求较高,操作不便(Li等,2024)。因此,迫切需要一种快速、特异且可现场检测的方法来克服这些局限性。

重组酶聚合酶扩增(RPA)-侧向层析试纸条(LFD)检测法是一种新型等温扩增技术,可在37–42°C条件下20–40分钟内实现靶基因片段的扩增,常用于微生物和突变基因的检测(Chang等,2024;Hong等,2024;Xu等,2024)。该方法无需专用设备和复杂操作步骤,非常适合现场快速检测。RPA-LFD检测法基于等温扩增和侧向层析可视化原理运行,详细原理见图1。上游引物和下游引物的5'端分别标记异硫氰酸荧光素(FITC)和生物素,扩增后形成的双标记产物使用含有高荧光铕(III)纳米颗粒(EuNPs)荧光微球的试纸条进行检测。该检测法便于临床样本的可视化检测,且EuNPs的长荧光衰变寿命提高了检测的特异性和灵敏度(Du等,2022;Xu等,2020)。

因此,为克服现有方法的局限性,本研究基于本课题组分离的DAdV-3毒株(CH-AN-2022),以DAdV-3-fiber-2为靶基因,建立了一种可视化荧光RPA-LFD快速检测法,用于该病毒的临床防控。

## 2 材料与方法

### 2.1 动物

无特定病原体(SPF)鸭胚购自中国农业科学院(黑龙江哈尔滨)。3日龄SPF鸭在安徽农业大学SPF动物孵化中心孵育和饲养。90只3日龄番鸭购自安徽省某鸭场。鸭群饲养于健康可控环境中,温度根据日龄和行为维持在30–34°C。

### 2.2 RPA-LFD检测法的建立

#### 2.2.1 生物分子与微球的偶联

首先对微球进行洗涤和活化:取50 μL高荧光微球(100 mg/mL)(Bangs Laboratories,美国),用500 μL 4-吗啉乙磺酸(MES)缓冲液(10 mM,pH=6.0)充分洗涤两次;4°C、14,000×g离心15分钟后弃上清;将微球重悬于200 μL MES缓冲液中并持续搅拌。随后依次加入250 μL 1-乙基-3-(3-二甲基氨基丙基)碳二亚胺盐酸盐(EDC;10 mg/mL)和N-羟基磺基琥珀酰亚胺钠盐(NHS)溶液(10 mg/mL),水浴超声处理5分钟后,在30°C、200 rpm的恒温振荡器中分散30分钟。接下来将微球与抗体偶联。用500 μL磷酸盐缓冲液(10 mM,pH 7.4)洗涤溶液两次,将微球重悬于1 mL磷酸盐缓冲液中。随后加入50 μL兔抗FITC抗体(Bioss,北京,中国)进行偶联。之后采用上述方法进行磷酸盐缓冲液分散和洗涤。洗涤后,将微球重悬于500 μL封闭液[30 mM乙醇胺和1% w/v牛血清白蛋白(BSA)]中,以相同方法分散,在最终洗涤缓冲液(封闭液和0.05% w/v Tween 20,pH=8.0)中洗涤后,重悬于含0.1% BSA的1 mL磷酸盐缓冲液中。最后将标记的微球送至Biohan生物科技有限公司(合肥,中国)制备和组装检测试纸条。荧光微球以5 μL/cm均匀喷涂在结合垫上。检测线(T)包被兔抗FITC抗体(Bioss,北京,中国),质控线(C)包被山羊抗兔免疫球蛋白G(Artron,山东,中国),浓度均为1 mg/mL。试纸条避光保存于含干燥剂的铝箔袋中,室温储存。

**表1 引物序列(5′–3′)**

| 引物名称 | 序列(5′–3′) | |---|---| | DAdV-3-Fiber2-F1 | CAATCACTCTCCGTTAGAACTAATCCTCAAG | | DAdV-3-Fiber2-F2 | CAAGGAGAGAAAGAGTTAGGCATCAACATC | | DAdV-3-Fiber2-F3 | CACATCGTGCATAACACTAGACAACGGAGGC | | DAdV-3-Fiber2-R1 | CATACGATCTTGGCATAGTATGCGCACGGAAAC | | DAdV-3-Fiber2-R2 | CGTAACAGACCCTGCTCCGCAGCACACTTG | | DAdV-3-Fiber2-R3 | CACACTTGGGCTTGTGTCTTCTGAAGTGTGTC |

### 2.4 RPA-LFD检测法最佳反应条件的筛选

从GenBank数据库下载DAdV-3 fiber-2基因全长序列(登录号:OP432083)。我们使用Oligo 6软件为fiber-2基因设计了九对引物(F1/R1、F1/R2、F1/R3、F2/R1、F2/R2、F2/R3、F3/R1、F3/R2和F3/R3),并分别通过PCR、qPCR和RPA-LFD进行验证和优化。引物由Sangon Biotech(上海,中国)合成,序列见表1。首先,PCR反应体系(总体积20 μL)包含以下组分:PCR混合物10 μL;正向引物(10 μM)0.5 μL;反向引物(10 μM)0.5 μL;DAdV-3 DNA 1 μL;双蒸水(ddH₂O)8 μL。引物对首先通过PCR验证扩增可行性。随后通过qPCR进一步筛选引物。将DAdV-3 DNA进行10倍、100倍和1,000倍稀释作为模板,每个样本进行三次重复检测(计算平均值)。引物合格的判定标准为:(i)凝胶电泳确认靶基因PCR扩增产物无引物二聚体;(ii)熔解曲线分析无非特异性峰;(iii)qPCR扩增曲线呈现特异性单峰且平均Ct值最低。最终选择扩增效率最高的引物对用于后续实验。该方法是基于其他研究者在RPA-LFD检测法引物筛选中所采用的策略(Onchan等,2022)。

RPA检测按照制造商说明书(LeSun Bio,江苏无锡,中国)进行。反应混合物包含25 μL反应缓冲液、16 μL ddH₂O、冻干粉酶、2 μL FITC标记的正向引物(10 μM)、2 μL生物素标记的反向引物(10 μM)、2 μL pMD18T-fiber-2重组载体模板和3 μL激活剂。所有反应组分加入后,手动轻弹混匀并短暂离心。扩增在37°C下进行20分钟。扩增产物用1%脱脂奶粉稀释10倍后用试纸条检测。5–10分钟后观察结果(图1)。T线和C线同时出现为阳性结果。相反,仅C线出现为阴性结果,表明靶基因片段不存在。仅T线出现则结果不确定或可疑。

进一步优化上述检测法的最佳条件,筛选最佳缓冲液类型、温度和稀释比。将70 μL稀释后的扩增产物加至试纸条上。5–10分钟后,用荧光免疫分析仪(HIT-91A,Biouhan,安徽合肥,中国)读取C线和T线的荧光信号强度,计算T/C值。每组实验重复3次,计算平均值(M)±标准差(SD)。

#### 2.4.1 缓冲液类型的优化

将扩增产物用含Tween 20的磷酸盐缓冲液(PBST)、1%脱脂奶粉或PBS中的Blocker™ Casein(Thermo Fisher,美国)进行10倍稀释,然后加至试纸条上。

#### 2.4.2 温度的优化

为确定最佳反应温度,在PCR仪控制下于六个温度(30°C、33°C、36°C、39°C、42°C和45°C)进行RPA反应。反应结束后,RPA产物用1%脱脂奶粉稀释10倍。

#### 2.4.3 稀释比的优化

高粘度扩增产物需适当稀释以利于靶基因扩增产物的检测。反应结束后,RPA扩增产物用1%脱脂奶粉进行5倍、10倍、20倍、30倍、40倍、50倍、60倍、70倍和80倍梯度稀释(表2)。

### 2.5 RPA-LFD检测法的特异性、灵敏度和空白限分析

还对RPA-LFD检测法的特异性、灵敏度和空白限(LOB)进行了验证。扩增产物的检测方法同上述2.3节所述。

#### 2.5.1 特异性分析

以DAdV-3、FAdV-4、DuCV-1(鸭圆病毒1型)、DAdV-2、FAdV-8a的DNA以及MDPV(番鸭细小病毒)、DHV(鸭肝炎病毒)、AIV(禽流感病毒)H7和H9亚型的cDNA作为模板进行RPA特异性分析,以鉴定该检测法与其他病毒的交叉反应。反应结束后,RPA扩增产物用1%脱脂奶粉稀释10倍。实验重复3次,计算M±SD。

#### 2.5.2 灵敏度分析

将pMD18-T-fiber-2质粒标准品进行系列稀释,浓度范围为10⁶至10⁰拷贝/μL,作为模板。灵敏度测试采用RPA-LFD检测法的优化条件。实验重复3次,计算M±SD。

#### 2.5.3 LOB分析

用20份1%脱脂奶粉缓冲液样品检测RPA反应体系;在荧光免疫分析仪上记录结果;整理和分析数据。LOB计算公式为:M + 2×SD。

**表2 RPA产物稀释比**

| 试剂名称 | RPA产物(μL) | 1%脱脂奶粉(μL) | 稀释比 | |---|---|---|---| | 5倍 | 14.00 | 56.00 | 5 | | 10倍 | 7.00 | 63.00 | 10 | | 20倍 | 3.50 | 66.50 | 20 | | 30倍 | 2.33 | 67.67 | 30 | | 40倍 | 1.75 | 68.25 | 40 | | 50倍 | 1.40 | 68.60 | 50 | | 60倍 | 1.17 | 68.83 | 60 | | 70倍 | 1.00 | 69.00 | 70 | | 80倍 | 0.88 | 69.12 | 80 |

### 2.6 临床样本分析

为评估RPA-LFD检测法与qPCR的一致率,对从三个临床发病鸭场采集的65份肛拭子样本分别采用建立的RPA-LFD检测法和qPCR进行检测,并比较结果。qPCR检测按照先前报道的方案进行(Zhang X.等,2024)。将浓度为1×10²拷贝/μL的阳性对照质粒pMD18-T-DAdV-3-fiber-2扩增得到的循环阈值(Ct=37)定义为临界值。结果判读如下:Ct值小于37的样本判定为阳性,Ct值大于37的样本判定为阴性。每个样本进行三次重复检测,计算平均Ct值用于最终判读。通过计算Kappa(κ)系数和p值评估两种方法的一致性。κ用于衡量数据的一致性程度,其值介于−1和1之间;p值表示观察到的一致性由偶然因素导致的概率。κ值越接近1,指标间的一致性越高;p值越小,指标间的一致性越显著。相关检测指标的计算公式如下,其中a、b、c、d为计数的样本数,n为样本总数:κ = (Po − Pe)/(1 − Pe),Po = (a + d)/(a + b + c + d),Pe = [(a + c)(b + d) + (a + b)(c + d)]/(a + b + c + d)²,其中Po为实际符合率,Pe为理论符合率,n为样本总数(表3)。

**表3 数据四格表的卡方检验**

| 方法 | RPA-LFD | | | |---|---|---|---| | qPCR | 阳性 | 阴性 | 总计 | | 阳性 | a | b | a+b | | 阴性 | c | d | c+d | | 总计 | a+c | b+d | a+b+c+d |

注:(a) qPCR和RPA-LFD均为阳性。(b) qPCR阴性而RPA-LFD阳性。(c) qPCR阳性而RPA-LFD阴性。(d) qPCR和RPA-LFD均为阴性。

### 2.7 临床检测

为验证RPA-LFD及时检测在临床环境中有效防控DAdV-3感染的效果,本研究还在一个养殖场进行了实验。将30只3日龄SPF鸭经颈背部皮下注射0.2 mL含2×10⁵ TCID₅₀/0.1 mL的鸭胚尿囊液进行接种。两天后,对感染雏鸭进行标记,随机分为两组,放入45只3日龄健康番鸭中,分别命名为第1组和第2组。混养4天后,根据标记对SPF鸭实施安乐死。混养期间,若第1组雏鸭出现精神沉郁或轻度腹泻症状,立即采集肛拭子使用RPA-LFD进行快速检测,阳性番鸭予以扑杀。第2组按常规程序饲养,不进行检测和扑杀,记录雏鸭情况持续30天。

病毒TCID₅₀的测定和实验动物的处理按照先前报道的方法进行(Zhang X.等,2024)。

## 3 结果

### 3.1 RPA最佳引物对的筛选

采用PCR、qPCR和RPA-LFD筛选最佳引物对。首先,使用本研究设计的九对引物进行PCR验证。1.5%琼脂糖凝胶电泳后,使用1 μL引物时观察到最清晰的条带,如图2A所示。所有九对引物(F1/R1:275 bp;F1/R2:242 bp;F1/R3:220 bp;F2/R1:244 bp;F2/R2:215 bp;F2/R3:190 bp;F3/R1:212 bp;F3/R2:180 bp;F3/R3:158 bp)均可扩增靶片段,产物大小符合预期;但F1/R2、F1/R3、F2/R2、F2/R3、F3/R2和F3/R3扩增产物存在明显的引物二聚体。相比之下,F1/R1、F2/R1和F3/R1产生清晰条带且无引物二聚体。

此外,以10倍、100倍和1,000倍稀释的DNA为模板,使用qPCR评估引物。不同引物的扩增效率见表4。当使用F1/R1作为引物对时,扩增效率最高。熔解曲线分析显示F1/R2和F3/R3存在非特异性扩增(图2B)。使用九对引物通过RPA扩增基因产物,结果表明F1/R1、F2/R1、F3/R3和F3/R1的扩增产物在试纸条上显示最清晰的条带。

综上所述,选择引物对F1/R1作为RPA-LFD检测法的最佳引物对。

**表4 不同稀释度DAdV-3 DNA的qPCR Ct值**

| 引物 | 10倍稀释 | 100倍稀释 | 1,000倍稀释 | |---|---|---|---| | F1R1 | 18.28 | 23.73 | 27.58 | | F1R2 | 18.71 | 23.48 | 26.92 | | F1R3 | 19.50 | 23.22 | 27.17 | | F2R1 | 19.36 | 23.74 | 27.83 | | F2R2 | 18.71 | 23.38 | 27.21 | | F2R3 | 18.34 | 23.24 | 27.32 | | F3R1 | 19.35 | 23.69 | 27.75 | | F3R2 | 19.08 | 23.50 | 27.68 | | F3R3 | 17.96 | 23.34 | 27.76 |

### 3.2 RPA条件的优化

通过评估不同缓冲液类型、温度和稀释比确定高效RPA的最佳条件。扩增产物分别用1%脱脂奶粉、PBST和PBS中的Blocker™ Casein稀释10倍。如图3A所示,三种稀释液的T/C均值分别为5.6183、0.115667和0.0995。因此,确定1%脱脂奶粉为RPA产物的最佳稀释液。

将RPA产物按5倍至80倍梯度稀释,如表2所示。结果如图3B所示。当产物稀释5倍、10倍、20倍、30倍、40倍、50倍、60倍、70倍和80倍时,T/C均值分别为2.6214、4.4628、0.9683、0.5707、0.3302、0.2247、0.2366、0.1646和0.1415。稀释20倍以上时RPA产物的T/C值相对较小。10倍稀释时T/C值最高。因此,确定10倍稀释为RPA产物的最佳稀释水平。

RPA反应还在特定温度范围内进行。结果如图3C所示。扩增效率从33°C到42°C呈上升趋势,而从42°C到45°C呈下降趋势。因此,确定RPA-LFD检测法的最佳扩增温度为42°C。

### 3.3 RPA-LFD检测法的灵敏度、特异性和LOB测定

使用浓度范围为10⁶至10⁰拷贝/μL的pMD18-T-fiber-2质粒稀释液评估RPA-LFD检测法的灵敏度。1×10¹拷贝/μL样品的T/C值显著高于阴性对照(图4A、B)。RPA-LFD检测法的检测限为1×10¹拷贝/μL。使用FAdV-4、DuCV-1、DAdV-2、FAdV-8a、MDPV、DHV、AIV-H7和AIV-H9的核酸检测RPA-LFD检测法的特异性。在RPA-LFD检测法中,仅DAdV-3产生阳性信号(T线和C线均出现)。值得注意的是,FAdV-4、DuCV-1、DAdV-2、FAdV-8a、MDPV、DHV、AIV-H7和AIV-H9未显示交叉反应(图4C、D),表明建立的RPA-LFD检测法具有优异的特异性。进行LOB分析以确定可与空白样本区分开的最低信号强度。使用20份空白样本,根据公式LOB = M + 2SD计算RPA-LFD检测法的LOB为0.037285(图4E、F)。

### 3.4 RPA-LFD检测法的临床样本验证

使用建立的RPA-LFD检测法对65份疑似DAdV-3肛拭子样本进行评估(图5A),所有样本的结果均经qPCR验证(图5B)。如表5所示,RPA-LFD检测法的阳性率为33.8%(22/65),qPCR评估的阳性率同样为33.8%(22/65),两种方法的符合率为100%(65/65)。RPA-LFD与qPCR检测法的κ值为1(p<0.001),表明两种方法几乎完全一致。

**表5 RPA-LFD和qPCR检测法对65份临床样本的检测结果**

| | RPA-LFD阳性 | RPA-LFD阴性 | 总计 | |---|---|---|---| | qPCR阳性 | 22 | 0 | 22 | | qPCR阴性 | 0 | 43 | 43 | | 总计 | 22 | 43 | 65 |

Kappa(κ)= 1,p值 < 0.001

### 3.5 RPA-LFD检测法临床效能的检测与分析

在第1组中,在30天混养期的前10天内,通过RPA-LFD鉴定出的4只DAdV-3阳性番鸭被扑杀[死亡率,8%(4/45)]。相比之下,在第2组中,经过30天观察,9只鸭死亡[死亡率,20%(9/45)],最终阳性番鸭在第28天被鉴定出来。这些结果表明,及时检测和扑杀使死亡率从20%大幅降至8%。

## 4 讨论

本研究的临床实验结果强调了及时干预在控制DAdV-3感染中的关键作用。具体而言,DAdV-3感染番鸭的死亡率达到20%,而其长期零星的死亡率显著低于SPF雏鸭,这可能是由于SPF雏鸭对病毒的易感性更高。重要的是,及时隔离病鸭使死亡率降至8%,凸显了及时检测和隔离对于防控DAdV-3的重要性。在此背景下,开发一种快速可靠的检测方法势在必行。现有的DAdV-3检测方法无法同时满足高特异性和操作简便性的要求(Ather等,2024;Wan等,2018;Xie等,2011)。相比之下,我们新开发的RPA-LFD检测法的灵敏度高达1×10¹拷贝/μL,可在30分钟内获得检测结果。该灵敏度水平与qPCR相当(表5),表明RPA-LFD检测法有望成为临床DAdV-3检测的新途径。该方法也已被研究者应用于其他禽类病毒的灵敏度和特异性检测;例如,传染性法氏囊病病毒(IBDV)、AIV(H5、H7和H9亚型)和新城疫病毒(NDV)的最低检测限分别为10¹、10²和10²拷贝/μL,且未观察到交叉反应(Wang等,2023;Wang等,2020;Zhang Z.等,2024)。在本研究中,检测的65份肛拭子样本采集自三个临床发病鸭场的疑似阳性标本,这可能解释了相对较高的阳性率(33.8%)。

除方法验证外,我们对检测靶标和病毒嗜性的分析提供了额外见解。选择fiber-2基因作为靶标是因为其在所有DAdV-3毒株中高度保守,确保了该检测法对不同DAdV-3分离株的适用性。与报道一致,肠道是禽腺病毒(包括DAdV-3)的主要排泄器官(Shi等,2022;Zhang X.等,2024),肛拭子在本研究中有效指示了病毒的存在。值得注意的是,本研究中的阳性结果表明,DAdV-3不仅在番鸭中检出,还在不同品种的老龄鸭中检出,包括180日龄北京鸭、240日龄白鸭和200日龄绍兴鸭,表明DAdV-3不仅可在番鸭间传播,还可跨品种传播。这些结果表明DAdV-3不仅可感染雏鸭,还可感染老龄鸭;但其具体传播机制有待进一步研究。

本研究存在一定的局限性。首先,该检测法的效能是在受控实验条件下验证的,可能无法完全再现自然临床环境的复杂性——包括病原载量的变化、宿主免疫能力的波动以及家禽生产系统中常见的混合感染。其次,用于验证的鸭品种数量和多样性相对有限,可能影响结果的统计效力和推广性。此外,该方法的成本仍然相对较高,可能阻碍其在资源有限现场环境中的广泛应用。因此,该检测法的临床适用性和稳健性——包括其在现场条件下的表现以及对不同鸭群的一致性检测——有待进一步验证,同时成本优化也势在必行。值得注意的是,优化的RPA-LFD系统有望扩展应用于其他禽类病原(包括病毒和细菌)的检测和临床清除,在致癌性病原的筛查和扑杀方面具有特殊的应用潜力。

本研究提出的原创性贡献包含在文章/补充材料中,进一步的咨询可联系通讯作者。作者声明本手稿的创作未使用生成式人工智能。

**作者贡献**

孙佳宇:方法论、数据整理、软件、撰写初稿。刘可为:数据整理、方法论、软件、撰写初稿。刘超:撰写审阅与编辑、形式分析、验证。王振宇:撰写审阅与编辑、形式分析、验证。高嘉希:数据整理、撰写审阅与编辑。赵茹雅:验证、撰写审阅与编辑。袁龙:撰写审阅与编辑、软件。申燕:资源、撰写审阅与编辑。李金春:撰写审阅与编辑。陈芳芳:撰写审阅与编辑、概念化、监督、经费获取、项目管理。