Development and application of a high-sensitivity immunochromatographic test strip for detecting pseudorabies virus

✅ 全文

高灵敏度免疫层析试纸条检测伪狂犬病病毒的开发与应用

作者 Jiajia Yin; Huimin Liu; Yumei Chen; Jingming Zhou; Yankai Liu; Zhenglun Liang; Xifang Zhu; Hongliang Liu; Peiyang Ding; Enping Liu; Ying Zhang; Sixuan Wu; Aiping Wang 期刊 Frontiers in Microbiology 发表日期 2024 卷/期/页码 Vol. 15 ISSN 1664-302X DOI 10.3389/fmicb.2024.1399123 类型 原创研究 (Original Research)

📄 英文摘要 English Abstract

EN

IntroductionPseudorabies (PR) is a multi-animal comorbid disease caused by pseudorabies virus (PRV), which are naturally found in pigs. At the end of 2011, the emergence of PRV variant strains in many provinces in China had caused huge economic losses to pig farms. Rapid detection diagnosis of pigs infected with the PRV variant helps prevent outbreaks of PR. The immunochromatography test strip with colloidal gold nanoparticles is often used in clinical testing due to its low cost and high throughput.MethodsThis study was designed to produce monoclonal antibodies targeting PRV through immunization of mice using the eukaryotic system to express the gE glycoprotein. Subsequently, paired monoclonal antibodies were screened based on their sensitivity and specificity for use in the preparation of test strips.Results and discussionThe strip prepared in this study was highly specific, only PRV was detected, and there was no cross-reactivity with glycoprotein gB, glycoprotein gC, glycoprotein gD, and glycoprotein gE of herpes simplex virus and varicellazoster virus, porcine epidemic diarrhea virus, Senecavirus A, classical swine fever virus, porcine reproductive and respiratory syndrome virus, and porcine parvovirus. Moreover, it demonstrated high sensitivity with a detection limit of 1.336 × 103 copies/μL (the number of viral genome copies per microliter); the coincidence rate with the RT-PCR detection method was 96.4%. The strip developed by our laboratory provides an effective method for monitoring PRV infection and controlling of PR vaccine quality.

📄 中文摘要 Chinese Abstract

中文
伪狂犬病(PR)是由伪狂犬病病毒(PRV)引起的一种多动物共患疾病,猪是其天然宿主。2011年底,中国多个省份出现了PRV变异株,给养猪场造成了巨大的经济损失。对感染PRV变异株的猪进行快速检测诊断有助于预防PR的暴发。胶体金纳米颗粒免疫层析试纸条因其成本低、通量高,常被用于临床检测。 由US8基因编码的gE蛋白在病毒毒力中起关键作用,其缺失可降低病毒对宿主的感染性。因此,gE缺失毒株常用于疫苗研究。此外,gE常被用作检测方法中的标记靶标,以区分疫苗接种与野生型感染。利用gE蛋白作为标记物来区分野生型病毒感染产生的抗体与疫苗接种诱导的抗体的优势在于,gE在所有野生型病毒株中普遍表达。

📋 英文结构化总结 English Structured Summary

全文整理

EN

Background:

Pseudorabies (PR) is a multi-animal comorbid disease caused by pseudorabies virus (PRV), which are naturally found in pigs. At the end of 2011, the emergence of PRV variant strains in many provinces in China had caused huge economic losses to pig farms. Rapid detection diagnosis of pigs infected with the PRV variant helps prevent outbreaks of PR. The immunochromatography test strip with colloidal gold nanoparticles is often used in clinical testing due to its low cost and high throughput.

The gE protein encoded by US8 plays a crucial role in virulence, and its absence reduces the virus’s infectivity to the host. Therefore, gE-deleted strains are commonly used in vaccine research. Additionally, gE is frequently used as a marker target in detection methods for differentiating between vaccination and wild-type infection. The advantage of using the gE protein as a marker to distinguish between antibodies resulting from wild-type virus infection and those induced by vaccination lies in its ubiquitous expression across all wild-type virus strains.

Methods:

This study was designed to produce monoclonal antibodies targeting PRV through immunization of mice using the eukaryotic system to express the gE glycoprotein. Subsequently, paired monoclonal antibodies were screened based on their sensitivity and specificity for use in the preparation of test strips.

Results:

The strip prepared in this study was highly specific, only PRV was detected, and there was no cross-reactivity with glycoprotein gB, glycoprotein gC, glycoprotein gD, and glycoprotein gE of herpes simplex virus and varicella zoster virus, porcine epidemic diarrhea virus, Senecavirus A, classical swine fever virus, porcine reproductive and respiratory syndrome virus, and porcine parvovirus. Moreover, it demonstrated high sensitivity with a detection limit of 1.336 × 10³ copies/µL (the number of viral genome copies per microliter); the coincidence rate with the RT-PCR detection method was 96.4%.

Data Summary:

The strip demonstrated high sensitivity with a detection limit of 1.336 × 10³ copies/µL. The coincidence rate with the RT-PCR detection method was 96.4%. The test strip was highly specific, detecting only PRV with no cross-reactivity against a panel of other viruses and viral glycoproteins.

Conclusions:

The strip developed by our laboratory provides an effective method for monitoring PRV infection and controlling of PR vaccine quality.

Practical Significance:

Rapid detection diagnosis of pigs infected with the PRV variant helps prevent outbreaks of PR. Rapid antigen (RAD) testing plays a crucial role in the early diagnosis and containment of diseases, offering potential as an important diagnostic tool for PRV, particularly when molecular methods of detection are limited. Additionally, RAD can also be utilized to monitor whether there are residues of gE antigens in vaccines.

📋 中文结构化总结 Chinese Structured Summary

中文

背景:

伪狂犬病(PR)是由伪狂犬病病毒(PRV)引起的一种多动物共患疾病,猪是其天然宿主。2011年底,中国多个省份出现了PRV变异株,给养猪场造成了巨大的经济损失。对感染PRV变异株的猪进行快速检测诊断有助于预防PR的暴发。胶体金纳米颗粒免疫层析试纸条因其成本低、通量高,常被用于临床检测。

由US8基因编码的gE蛋白在病毒毒力中起关键作用,其缺失可降低病毒对宿主的感染性。因此,gE缺失毒株常用于疫苗研究。此外,gE常被用作检测方法中的标记靶标,以区分疫苗接种与野生型感染。利用gE蛋白作为标记物来区分野生型病毒感染产生的抗体与疫苗接种诱导的抗体的优势在于,gE在所有野生型病毒株中普遍表达。

方法:

本研究旨在通过用真核系统表达的gE糖蛋白免疫小鼠,制备针对PRV的单克隆抗体。随后,根据灵敏度和特异性筛选配对单克隆抗体,用于制备试纸条。

结果:

本研究制备的试纸条具有高度特异性,仅检测到PRV,与单纯疱疹病毒和水痘-带状疱疹病毒的糖蛋白gB、gC、gD和gE,以及猪流行性腹泻病毒、塞内卡病毒A、猪瘟病毒、猪繁殖与呼吸综合征病毒和猪细小病毒均无交叉反应。此外,该试纸条具有高灵敏度,检测限为1.336 × 10³拷贝/微升(每微升病毒基因组拷贝数);与RT-PCR检测方法的符合率为96.4%。

数据总结:

该试纸条具有高灵敏度,检测限为1.336 × 10³拷贝/微升。与RT-PCR检测方法的符合率为96.4%。该试纸条具有高度特异性,仅检测到PRV,与其他多种病毒和病毒糖蛋白无交叉反应。

结论:

本实验室开发的试纸条为监测PRV感染和控制PR疫苗质量提供了一种有效方法。

实际意义:

对感染PRV变异株的猪进行快速检测诊断有助于预防PR的暴发。快速抗原检测(RAD)在疾病的早期诊断和防控中发挥着重要作用,在分子检测方法受限的情况下,有望成为PRV的重要诊断工具。此外,RAD还可用于监测疫苗中是否存在gE抗原残留。

📖 英文全文 English Full Text

EN

TYPE Original Research PUBLISHED 03 May 2024 DOI 10.3389/fmicb.2024.1399123 OPEN ACCESS EDITED BY Zhixun Xie, Guangxi Veterinary Research Institute, China REVIEWED BY Mengmeng Zhao, Foshan University, China Bin Zhou, Nanjing Agricultural University, China

Development and application of a high-sensitivity immunochromatographic test strip for detecting pseudorabies virus *CORRESPONDENCE Aiping Wang pingaw@126.com †

These authors have contributed equally to this work RECEIVED 11 March 2024 ACCEPTED 16 April 2024 PUBLISHED 03 May 2024 CITATION

Yin J, Liu H, Chen Y, Zhou J, Liu Y, Liang Z, Zhu X, Liu H, Ding P, Liu E, Zhang Y, Wu S and Wang A (2024) Development and application of a high-sensitivity immunochromatographic test strip for detecting pseudorabies virus. Front. Microbiol. 15:1399123. doi: 10.3389/fmicb.2024.1399123 COPYRIGHT

© 2024 Yin, Liu, Chen, Zhou, Liu, Liang, Zhu, Liu, Ding, Liu, Zhang, Wu and Wang. 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.

Jiajia Yin1,2† , Huimin Liu1,3† , Yumei Chen1,2,4 , Jingming Zhou1,2,4 , Yankai Liu1,2,4 , Zhenglun Liang1,4 , Xifang Zhu1,2,4 , Hongliang Liu1,2,4 , Peiyang Ding1,2,4 , Enping Liu1,2,4 , Ying Zhang1,4 , Sixuan Wu1,4 and Aiping Wang1,2,4* 1

Longhu Laboratory, Zhengzhou, China, 2 School of Life Sciences, Zhengzhou University, Zhengzhou, China, 3 College of Basic Science, Zhengzhou University of Technology, Zhengzhou, Henan, China, 4 Henan Provincial Key Laboratory of Immunobiology, Zhengzhou, China

Introduction: Pseudorabies (PR) is a multi-animal comorbid disease caused by pseudorabies virus (PRV), which are naturally found in pigs. At the end of 2011, the emergence of PRV variant strains in many provinces in China had caused huge economic losses to pig farms. Rapid detection diagnosis of pigs infected with the PRV variant helps prevent outbreaks of PR. The immunochromatography test strip with colloidal gold nanoparticles is often used in clinical testing due to its low cost and high throughput. Methods: This study was designed to produce monoclonal antibodies targeting PRV through immunization of mice using the eukaryotic system to express the gE glycoprotein. Subsequently, paired monoclonal antibodies were screened based on their sensitivity and specificity for use in the preparation of test strips. Results and discussion: The strip prepared in this study was highly specific, only PRV was detected, and there was no cross-reactivity with glycoprotein gB, glycoprotein gC, glycoprotein gD, and glycoprotein gE of herpes simplex virus and varicellazoster virus, porcine epidemic diarrhea virus, Senecavirus A, classical swine fever virus, porcine reproductive and respiratory syndrome virus, and porcine parvovirus. Moreover, it demonstrated high sensitivity with a detection limit of 1.336 × 103 copies/µL (the number of viral genome copies per microliter); the coincidence rate with the RT-PCR detection method was 96.4%. The strip developed by our laboratory provides an effective method for monitoring PRV infection and controlling of PR vaccine quality. KEYWORDS

pseudorabies virus, monoclonal antibody, immunochromatographic strip, rapid antigen testing gold nanoparticles,

Introduction Pseudorabies (PR), also known as Aujeszky disease (AD), is a highly contagious viral disease caused by the pseudorabies virus (PRV), which can infect a variety of animals (Wong et al., 2019; Yu et al., 2021). PRV was first found in cats in China in 1957, and it spread to many regions in China in the 1980s, infecting a variety of animals. Pigs are natural hosts for PRV and can carry the virus latently (Yu et al., 2014). China, known as

Frontiers in Microbiology 01 frontiersin.org Yin et al. 10.3389/fmicb.2024.1399123 the largest producer and consumer of pork, has encountered two instances of pseudorabies outbreaks. The first outbreak occurred in the 1990s and then again in 2011 (Dong et al., 2018). Experiments such as virus isolation proved that the root cause of the 2011 outbreak was the mutation of the strain. The PRV variant strains when compared to classical strains exhibited a higher level of virulence in pigs. While the traditional Bartha-K61 vaccine strain can provide comprehensive protection against the classical strains, it proves inadequate in defending against variant strains (Meng et al., 2016; Cheng et al., 2020; Tan et al., 2021). PRV underwent mutation and regained its virulence, leading to a widespread outbreak in China. Henan, a major province for pig farming, has been particularly affected by this epidemic. The recirculation of pseudorabies wild-type poison in Chinese pig farms has posed great challenges to both the pig industry and efforts toward preventing and controlling epidemic diseases (Tan et al., 2021). Identification, rapid eradication, and vaccination of infected pigs are crucial measures implemented currently for controlling pseudorabies in the porcine population. Currently, the predominant clinical approaches for PRV diagnosis primarily involve serological detection and molecular biology techniques. Molecular biology detection methods encompass fluorescence quantitative PCR and reverse transcription PCR (RT-PCR) (Cheng et al., 2021). However, the use of PCR for diagnosing PRV infection in pigs is limited due to its requirement for specialized laboratory personnel (Porte et al., 2020). Serological detection methods for PRV mainly include microneutralization assay (MN), indirect enzyme-linked immunosorbent assay (i-ELISA), competitive ELISA (c-ELISA), and indirect immunofluorescence assay (IFA). Among these methods, blocking ELISA is commonly employed due to its high specificity and sensitivity, but is time-consuming (Maan et al., 2012). Rapid antigen (RAD) testing plays a crucial role in the early diagnosis and containment of diseases, offering potential as an important diagnostic tool for PRV, particularly when molecular methods of detection are limited (Mak et al., 2020; Scohy et al., 2020). Additionally, RAD can also be utilized to monitor whether there are residues of gE antigens in vaccines. In recent years, there has been an increase in the severity of co-infections between PR and other swine diseases, and there is an urgent need for rapid and accurate detection of PR antigens. The immunochromatography test strip rapid technology is an immunological rapid detection method developed based on the mAb technology, which has become a primary approach for rapid detection. The antigen test strip commonly adopts the “double antibody sandwich” detection mode to enable the identification of microbial antigens such as viruses, bacteria, and parasites, along with non-microbial antigens including self-antigens and tumor antigens (Wang et al., 2015). Therefore, this study aims to develop immunochromatographic strips for PR screening. At present, a total of 11 glycoproteins have been identified in porcine pseudorabies virus: gB (UL27), gC (UL44), gD (US6), gE (US8), gG (US4), gH (UL22), gI (US7), gK (UL53), gL (UL1), gM (UL10), and gN (UL49.5). The gE protein encoded by US8 plays a crucial role in virulence, and its absence reduces the virus’s infectivity to the host (Tirabassi and Enquist, 1999). Therefore, gE-deleted strains are commonly used in vaccine research. Additionally, gE is frequently used as a marker target

in detection methods for differentiating between vaccination and wild-type infection (Wang et al., 2018). The advantage of using the gE protein as a marker to distinguish between antibodies resulting from wild-type virus infection and those induced by vaccination lies in its ubiquitous expression across all wild-type virus strains (van Oirschot et al., 1990; Tirabassi et al., 1997), thereby enabling the establishment of PRV antigen detection methods based on this characteristic. In this study, mice were immunized with the gE protein used as an immunogen to generate monoclonal antibodies (mAbs) against PRV. Subsequently, a gold immunochromatographic strip specific for PRV was developed using two gE-specific mAbs, with the PRV gE protein having a detection limit of 31.25 ng/mL. The immunoassay strip described in this article enables rapid detection of PRV gE protein, making it suitable for early infection diagnosis of wild-type PRV strains and quality monitoring of PRV vaccines.

Materials and methods Ethics and biosafety statements The experimental research protocol for monoclonal antibody production in mice was approved by the Key Laboratory of Animal Immunology, Henan Academy of Agricultural Sciences, China, in line with its policies and procedures (LLSC100166).

Reagent, strains, and cells DH5α competent cells were purchased from Biomedical Technology (Beijing, China). FreeStyleTM 293-F cells were sourced from Sino Biological (Beijing, China). SP2/0 cells were provided by the Key Laboratory of Animal Immunology of Henan Academy of Agricultural Sciences (Zhengzhou, China). 293-F cells were cultured using SMM 293-TII serum-free medium (Sino Biological, China). SP2/0 cells were maintained with RPMI 1640 medium (Solarbio, China), supplemented with 10% (v/v) fetal bovine serum (TransGen, Beijing). Aminophenylboronate A6XL was purchased from Astrea Bioseparations Co., Ltd. (Cambridge, UK). Superdex200 10/300 GL was purchased from Cytiva (Montana, USA). The virus strain HeNL/2017 (GenBank no. MT775883) recombinant PRV-GFP strain was kindly provided by researcher Wang Hanzhong from Wuhan Institute of Virology, Chinese Academy of Sciences. The virus strain HeNL/2017 was propagated with DMEM supplemented with 2% (v/v) fetal bovine serum. Porcine epidemic diarrhea virus (PEDV), Senecavirus A (SVA), classical swine fever virus (CSFV), porcine reproductive and respiratory syndrome virus (PRRSV), and porcine parvovirus (PPV) were preserved and propagated by this experiment.

Expression and purification of PRV gE The genomic sequence of HeNLH/2017 (GenBank:QQL12221.1) was used as a sequence template to construct the gE protein, which was subsequently optimized based on a codon usage bias of mammalian expression systems and

02 frontiersin.org Yin et al. 10.3389/fmicb.2024.1399123 synthesized by General Biotech Co., Ltd. (Anhui, China). Following R the In-Fusion HD Cloning Kit manual for inserting gE into the pCAGGS plasmid (HonorGene, China), the recombinant plasmid was transfected into 293F cells mediated by polyethylenimine linear (PEI) MW40000 (Yisheng, China) with a cell density of 2∼3 × 106 cells/mL. After 72 h of transfection, the supernatant was harvested by centrifugation at 12,000 g × 10 min at 4◦ C and then identified by Western blot. The supernatant was filtered through a 0.22-µm Stericup filter and purified by aminophenylboronate A6XL affinity chromatography. Subsequently, the eluted protein solution was dialyzed against phosphate buffer (PBS, pH 7.4). The dialyzed protein solution was concentrated by using an ultrafiltration tube (MilliporeSigma, USA) with a retention capacity of 30 K and loaded onto the Superdex200 gel filtration chromatography column to separate the recombinant protein and identified by SDS-PAGE and Western blot. The concentration of the recombinant gE protein was determined using a NanoDrop2000 spectrophotometer (Thermo Fisher Scientific, USA).

Preparation of monoclonal antibodies against PRV gE A standard protocol was followed to generate mAbs against PRV gE. Briefly, 6-week-old female Balb/c mice (n = 2) were immunized with PRV gE protein at a dose of 10 µg per mouse in Freund’s adjuvant medium. Blood samples were collected 14 days after the third immunization. The serum titer level was determined through indirect ELISA with the recombinant gE protein as a coated antigen. Mice with high serum titers were selected for the preparation of hybridoma cells. Positive hybridoma cell lines were screened, and the supernatant of positive hybridoma cell lines was identified by ELISA. Positive hybridoma cell lines were diluted through limiting dilution to obtain a monoclonal cell line that stably produced antibodies. IFA was used to further verify the reactivity of the mAbs against the gE protein. Ascitic fluids from positive hybridomas for colloidal gold labeling were produced in mice.

pCAGGS-gE recombinant vector digestion validation M: DL 2000, Lane 1: pCAGGS-gE digestion product. ′

Cells were simultaneously stained using DAPI (4 ,6-diamidino-2phenylindole) from Solarbio. After the final washing, fluorescence signals were visualized using fluorescence microscopy from ZEISS in Jena, Germany.

Preparation of gold-labeled mAbs Colloidal gold labeling of mAbs According to Liu et al. (2020), colloidal gold was prepared by the trisodium citrate method. Subsequently, gold-labeled antibodies were prepared as follows: 10 µL of ultrapure water was added to wells 1–6 in microplates, followed by the addition of 10 µL of ascites fluid (diluted at a ratio of 1: 10 with ddw) to well 1 and consecutively double-diluted to well 6. Then, 125 µL of colloidal gold solution at pH 9.0 was placed in each well, thoroughly mixed, and left standing for 5–15 min at room temperature. Next, 125 µL of 10% NaCl solution was added per well and allowed to react for 10 min at room temperature in order to observe any color changes in the solutions until the color of the solution does not change, and the concentration corresponding to the highest dilution of the well is the most suitable labeled concentration. We added the optimal labeled amount of ascites to 1 mL of colloidal gold solution, thoroughly mixed, and allowed to react at room temperature for 15 min. Then, 100 µL of a sodium borate solution containing 20 mmol/L concentration and 10% BSA was added, mixed well, and incubated at room temperature for 5 min.

Immunofluorescence assay The HEK293T cells were cultured in DMEM supplemented with 10% FBS and seeded into 48-well cell culture plates at a density of 2 × 104 cells/well. They were then incubated overnight at 37◦ C with 5% CO2 . Once the cells reached a confluency of 70–80%, the recombinant plasmid pCAGGS-gE was transfected into the cells R using the jetPRIME Versatile DNA/siRNA transfection reagent (Polyplus, France) and cultured at 37◦ C for 48 h. After culturing, the plates were fixed with methanol (precooled to −20◦ C) for 20 min at room temperature (RT). Next, the plates were washed with PBST and incubated with skim milk (5%) at 37◦ C for 1 h. Then, anti-PRV gE was used as a primary antibody for 30 min, while DMEM served as a negative control. Subsequently, the plates were washed three times with PBST and incubated with anti-mouse IgG H&L (FITC) (Solarbio, Beijing, China) for half an hour at 37◦ C.

Purification of glycoprotein gE. (A) SDS-PAGE of the purified PRV gE protein; M: protein molecular weight marker; Lane 1: gE protein purified by A6XL; Lane 2: gE protein purified by a molecular sieve; (B) Western blot of the purified gE recombinant protein reacted with the His tag Antibody; M: protein molecular weight marker; Lane 1: gE protein purified by A6XL; Lane 2: gE protein purified by a molecular sieve; (C) Western blot of the purified gE recombinant protein react with PRV-positive field serum. M: protein molecular weight marker; Lane 1: gE protein purified by A6XL; Lane 2: gE protein purified by a molecular sieve.

The mixture was then centrifuged at a speed of 15,000 r/min for 30 min at a temperature of 4◦ C, followed by careful removal of the supernatant. The pellet was resuspended in boric acid buffer containing 1% (w/v) BSA. Finally, the prepared gold-labeled antibody was stored at a temperature of 4◦ C.

for 30 min. Following Li et al. (2021), we assembled the NC membrane, conjugate pad, fiberglass sample pad, and absorption pad sequentially on the support board, with each overlapping by 1–2 millimeters before cutting them into pieces measuring 2.79 mm by using a CM4000 cutter from Bio-Dot to form an immunochromatographic strip, which we sealed in tin foil bags along with desiccants and then stored at 4◦ C.

Screening of the strip paired mAbs Among the positive clones, two mAbs with the highest binding affinity to the PRV gE protein were selected. The following steps were performed: each of the nine mAbs were used for detection and capturing of antibody (gold-Labeled) to each other, and a blank strip was used in a “sandwich method” mode to screen paired antibodies. A volume of 0.3 µl of the detection antibody was added dropwise onto the test strip’s detection membrane and dried, and then 1 µl of the gold-labeled antibody was added dropwise onto the conjugate pad. The test strip was placed in 100 µL of the positive sample solution. The color intensity on the nitrocellulose membrane was used to determine the pairing of two specific antibodies. Finally, the characteristics of the obtained mAbs were evaluated.

Evaluation of PRV rapid test strips Specificity evaluation of the strip The specific sample tray comprised PRV cell cultures, PRV gE protein, and other glycoproteins derived from the same virus strain, including PRV gB, gC, and gD glycoprotein, as well as HSV-derived gE glycoproteins. Additionally, it included virus strains such as VZV, PEDV, SVA, CSFV, PRRSV, and PPV. Negative controls were represented by media such as PBS and DMEM. The identification was performed using PRV antigen dipsticks.

Sensitivity evaluation of the strip The PRV standard plasmid was diluted sequentially into nine gradients, namely, 109 , 108 , 107 , 106 , 105 , 104 , 103 , 102 , and 101 copies/µL, which were used as templates for real-time fluorescence RT-PCR detection of porcine pseudorabies virus, and the standard curve of real-time fluorescent RT-PCR was plotted to obtain the standard equation for the PRV real-time fluorescence RT-PCR detection method. The copy number of PRV HeNL/2017 cell culture stock was calculated and diluted by 21 , 22 , 23 , 24 , 25 , 26 , and 27 . Meanwhile, the stock solution of the PRV HeNL/2017 cell culture was diluted by a series of gradients at 21 , 22 , 23 , 24 , 25 , 26 , and 27 to form a sensitivity sample tray. The samples

Preparation of the immunochromatographic strip A nitrocellulose (NC) membrane and three pads (sample pad, conjugation pad, and absorption pad) composed the test strip. The NC membrane was spotted with mAb-12E9E7 as the detection line and staphylococcal protein A (SPA) as the control line. Subsequently, it was dried at 42◦ C for 4 h. To prepare the sample pad, a glass wool strip was soaked in PBS (pH 8.0) containing 0.1 mol/L NaCl, 0.2% Tween-20 (v/v), and 0.1% (w/v) NaN3 for 30 min and dried in a drying oven at 50◦ C for 30 min. Next, goldstandard mAb was sprayed on glass wool at a concentration of 1 µg/µL to make a conjugate pad that was also dried at 50◦ C

Screening and identification of mAbs. A total of 10 positive hybridoma cell lines were screened by ELISA (A) (the color of the column represents different cell lines), and the titers of the mAb cell supernatant ranged from 1:3,200 to 1:25,600 (B). IFA demonstrated that all ten mAbs generated in this study had strong reactivity with the PRV gE protein. (C) IFA of the reactivity between mAbs and gE recombinant protein in 293T cells. The green color represents anti-gE mAbs, and the blue color represents nuclei (scale bars, 200 µm). These results demonstrated that mAbs react with the eukaryotic expression of the gE recombinant protein, which was consistent with the positive control.

of the sensitivity sample tray were detected with PRV rapid test strips and real-time fluorescence RT-PCR, and the detection results were compared. In addition, serial dilutions of the PRV gE protein produced in this study in the range of 2,000– 15.63 ng/mL were used to determine the sensitivity of the bands.

The coincidence rate of the test strip Stability evaluation of the strip Results

Twenty-eight samples of spleen or lymphoid tissue of pigs were detected by using the trial PRV rapid test strip and the real-time fluorescence RT-PCR detection method of porcine pseudorabies virus, and the results of the real-time fluorescence RT-PCR detection method were used to evaluate the consistency rate with the real-time fluorescence RT-PCR detection method for porcine pseudorabies virus.

In order to determine the stability of the test strip, we sealed the test strip and placed it in a 37-degree incubator for accelerated testing. These strips were stored at 37◦ C for 1 month and tested to verify the sensitivity of the PRV gE protein generated in this study, and its stability was determined based on the sensitivity assay results.

Frontiers in Microbiology

Expression and purification of PRV glycoprotein gE The linearized gE target gene sequence was ligated to the pCAGGS vector sequence using T4 05 frontiersin.org Yin et al. 10.3389/fmicb.2024.1399123 FIGURE 4

Screening of paired antibodies. Nine cell strains with high supernatant titers were selected to prepare ascites for colloidal gold labeling. When the NC film was dotted with 12E9E7, and the gold-standard 3D6B2 was used as a conjugate to bind the antigen, resulting in color development at the T line (A), and the ascites fluid of 12E9E7 was subjected to SDS-PAGE analysis before and after purification (B).

DNA ligase, and the recombinant expression plasmid pCAGGS-gE was obtained. The results of 1% nucleic acid electrophoresis verified by double digestion were successfully obtained, the recombinant expression vector was successfully obtained, and the size was consistent with expectations (Figure 1). The PRV gE recombinant protein was successfully expressed and purified from the mammalian expression system. The cell supernatant was centrifuged and purified to harvest the recombinant protein. As demonstrated in Figure 2, the protein eluted in PBS had a purity above 95% (Figure 2A). Western blot analysis confirmed that the gE recombinant protein could react with Anti-His tag Antibody (HRP) (Figure 2B) as well as PRV-positive field serum at a dilution of 1: 500 in 5% skim milk (Figure 2C).

all ten mAbs generated in this study had a strong reactivity with the PRV gE protein (Figure 3C).

Screening of paired antibodies Nine cell strains with high supernatant titers were selected to prepare ascites for colloidal gold labeling. Antibody pairing experiments indicated that the mAb-3D6B2 as the capture antibody and mAb-12E9E7 as the detection antibody showed optimal performance according to the color development in this assay (Figure 4A). Subsequently, the capture antibody 12E9E7 was purified for the preparation of immunochromatography strips (Figure 4B).

The characteristics of mAbs In order to gain a more comprehensive understanding of the characteristics of mAbs, we used the mouse monoclonal antibody isotyping Elisa kit (Proteintech, Wuhan) following the manufacturer’s instructions to determine the subtypes of mAbs. The optical density reading at 450 nm indicated that both mAbs were classified as IgG2b and Kappa (Figure 5A). The affinity of the two mAbs was 9.994 × 107 L/moL (12E9E7) (Figure 5B) and 5.69 × 108 L/moL (3D6B2) (Figure 5C), respectively. Additionally, in

Preparation of mAbs and screening of paired antibodies Screening and identification of mAbs After cell fusion, a total of 10 positive hybridoma cell lines were screened (Figure 3A), and the titers of the mAbs cell supernatant ranged from 1:3,200 to 1:25,600 (Figure 3B). IFA demonstrated that

Frontiers in Microbiology 06 frontiersin.org Yin et al. 10.3389/fmicb.2024.1399123 FIGURE 5

Characteristics of mAbs. (A) Antibody isotype identification ( 3D6B2, 12E9E7). (B, C) Monoclonal antibody affinity assay. (B) Affinity curves of mAb-12E9E7 exhibited high correlation coefficients (the R2 value 0.9948). (C) mAb-3D6B2 affinity curves (the R2 values ranged from 0.96 to 0.98). (D) Specificity evaluation of mAb-3D6B22 and mAb-12E9E7 with (in that order) PRV cell cultures, PRV-gE proteins, PRV-gB proteins, PRV-gC proteins, PRV-gD proteins, VSV-gE protein, as well as PEDV, SVA, HSV, CSFV, PRRSV, PPV cell cultures, and PBS. The mAbs specifically reacted to PRV and gE recombinant proteins, whereas they had no response to the other proteins or diseases.

VSV PEDV, SVA, CSFV, PRRSV, PPV, and negative control showed T line no color and C line color development results, indicating that the PRV rapid test strip had good specificity.

order to determine the specificity of mAbs, PRV cell cultures, PRVgE proteins, PRV-gB proteins, PRV-gC proteins, PRV-gD proteins, VSV-gE protein, as well as PEDV, SVA, HSV, CSFV, PRRSV, PPV cell cultures, and PBS were simultaneously detected using DotELISA. The results demonstrated that the mAbs specifically reacted to PRV cell cultures and gE recombinant proteins, whereas they had no response to the other PRV proteins or diseases (Figure 5D).

Real-time fluorescent RT-PCR detection method for PRV The standard curve was plotted using PRV real-time fluorescence RT-PCR detection with the gradient-diluted PRV standard plasmid as a template. The equation of the standard curve was determined to be y = −4.2401x + 40.718 (R2 = 0.9898) (Figure 7). When the Ct value was >34.0, it indicated a negative test result, corresponding to a viral copy number below 38 copies/µL, thus establishing the limit of detection for the RT-PCR assay at 38 copies/µL.

Establishment of a rapid detective immunochromatographic strip The colloidal gold conjugation of 3D6B2 was dispensed on fiberglass pads as conjugated mAb. The mAb 12E9E7 (1 mg/mL) was sprayed on the NC film to form a detection line. Then, the SPA was diluted to 0.5 mg/mL in PBS as the control line. The two specific mAbs of PRV detected PRV by a double-antibody sandwich mode.

The specificity of the test strip Sensitivity evaluation of the strip

The specific sample tray was detected with PRV rapid test strips, and the results are shown in Figure 6; only when detecting PRV cell cultures, the T line and C line of the PRV rapid test strip were colored, and the cell culture medium for detecting PRV-gB, PRV-gC, PRV-gD, HSV, Frontiers in Microbiology

Limit of detection of the gE protein in test strips Serial dilutions of the PRV gE protein produced in this study ranging from 2,000 to 15.63 ng/mL were used to determine the 07 frontiersin.org Yin et al.

10.3389/fmicb.2024.1399123 FIGURE 6

Specificity evaluation of the strip. The specific sample tray was detected by PRV rapid test strips, and the results are depicted in this figure, and only when detecting PRV cell cultures, both the T line and C line of the PRV rapid test strip were colored. In contrast, other proteins or diseases as well as the negative control displayed no coloration in the T line but showed color development in the C line.

sensitivity of the strip. The G/D × area-ROD values reduced as the protein concentration in the samples reduced, so the results showed that the detection limit of RBD was 31.25 ng/mL (Figure 8; Table 1).

The stability of the test strip The limit of detection of PRV by the test strip The coincidence rate of the PRV rapid test strips

The PRV HeNL/2017 cell culture stock was diluted and then detected with PRV rapid test strips and real-time fluorescent RTPCR detection methods. The result is shown in Figure 9. The rapid test strip had a detection limit of 1: 64 and a corresponding viral load of 1.336 × 103 copies/µL (Table 2). Therefore, the number of detected copies of the PRV rapid test strip was 1.336 × 103 copies/µL.

Twenty-eight samples of spleen or lymphoid tissue from pigs were detected by PRV rapid test strip and real-time fluorescence RT-PCR. The results are shown in Table 3; 15 samples were found positive for porcine pseudorabies virus by the real-time fluorescence RT-PCR test method, and 14 samples were found positive for PRV rapid test strips. Based on the detection results of the real-time fluorescence RT-PCR detection method for porcine

Frontiers in Microbiology

The strips still had the same detection limit (31.25 ng/mL) for the PRV gE protein produced in this study after 1 month of storage at 37◦ C, indicating that the strip had good stability (Figure 10). 08

frontiersin.org Yin et al. 10.3389/fmicb.2024.1399123 FIGURE 7 The standard curve of qPCR. The slope of this linear fitting equation is 0.9898. FIGURE 8 Sensitivity assay for gE protein detection. pseudorabies virus, the coincidence rate of PRV rapid test strips was 96.4% (27/28).

diseases (An et al., 2013). To control these domestic circulating variants, researchers have developed a gene deletion vaccine with the PRV variant as its parent strain. This vaccine can provide complete immune protection efficacy in pigs and represents an ideal candidate for a PRV variant. In order to enhance the control and prevention of PRV in China, mandatory vaccination is accompanied by virological and serological surveillance as well as stringent biosecurity procedures. It is imperative to intensify nationwide testing and strengthen monitoring of infections in animals other than pigs. Although conventional methods for detecting PRV such as ELISA, RT-PCR, qPCR (Deblanc et al.,

Discussion As a potential zoonotic disease, PRV poses a threat to both the breeding industry and public health security (Ai et al., 2018; Wang et al., 2020). Since 2011, the circulation of wild-type PRV strains in China’s pig farms has brought significant challenges to the pig industry and the prevention and control of epidemic

Frontiers in Microbiology 09 frontiersin.org Yin et al. 10.3389/fmicb.2024.1399123 TABLE 1 Sensitivity evaluation of the strip. Region Target Dens—ROD G/dens—ROD G/DxA—ROD – pixel G/pos—pixel G/width—pixel

2 µg 1 0.4729 0.1878 477.4391 230 41 1 µg 1 0.4845 0.1269 322.4699 230 41 500 ng 1 0.4112 0.0478 121.472 230 41 250 ng 1 0.4091 0.0296 75.1328 230 41 125 ng 1 0.3979 0.0287 72.9479 230 41 62.5 ng 1 0.4174

0.0182 46.2436 230 41 31.25 ng 1 0.3895 0.0152 38.5618 230 41 15.625 ng 1 0.4206 0.0096 24.3839 230 41 – 1 0.4184 0.0026 4.5934 230 41 Mean 0.4248 0.0518 131.4716 230 41 SD 0.0577 0.0631 160.5984 0 0 FIGURE 9

Sensitivity assay for PRV detection. TABLE 2 Numbers of copies of gradient dilutions of PRV cell cultures. Dilution 1: 2 1: 4 1: 8 1: 16 1: 32 1: 64 1: 128 Ct value 20.781 21.401 22.277 23.697 25.312 27.464

28.91 5.035 × 104 3.597 × 104 2.234 × 104 1.033 × 104 4.602 × 103 1.336 × 103 0.603 × 103 Number of copies

colloidal selenium and up-converting phosphor nanoparticles were abundant (Li et al., 2011), we still chose the conventional colloidal gold in this study because colloidal gold is more stable, sensitive, and specific. The test results are visible to the naked eye and imply short time consumption, high sensitivity, good specificity, and suitability for grassroots promotion and application (Li et al., 2015, 2023).

2019; Cheng et al., 2021), and rabbit inoculation test are accurate, they do have certain limitations. For instance, the PCR technology requires advanced skills and may not be suitable for routine farm testing; rabbit inoculation tests require professional personnel and are not suitable for large-scale animal husbandry; ELISA based on antibodies in the sample may miss the optimal period for prevention and control. Although the new labeled materials such as

Frontiers in Microbiology 10 frontiersin.org Yin et al. 10.3389/fmicb.2024.1399123

In this study, we selected the PRV gE protein as our research target for the following reasons: first, the gE protein is a glycoprotein located in the viral envelope, which is commonly used to detect wild-type virus infection, and its antibody detection can also distinguish between wild-type virus infection and vaccine immunization animals (Nauwynck, 1997; Ao et al., 2003). Additionally, establishing methods to detect the gE protein allows for strict quality control of inactivated vaccines and live vaccines lacking gE. It has been reported that the PRV gE protein has successfully been expressed in E. coli, yeast, and insect cells. The established ELISA, immunofluorescence, and other methods can effectively distinguish wild-type virus infection from vaccine-induced immune antibodies, thus demonstrating promising application prospects. However, some conventional challenges persist: most of the gE recombinant proteins expressed by the prokaryotic expression system exist as inclusion bodies with low antigen activity, which often fails to meet clinical detection requirements (Wu et al., 2023). There is low expression in yeast expression systems (Ren, 2004) and long expression cycles in the insect system (Zhu et al., 2019). All of these factors significantly impact the practical application of the PRV gE protein. The HEK 293F expression system modifies the expressed protein to ensure correct folding, high levels of protein expression, and preservation of a more complete natural conformation with enhanced biological activity (Nettleship et al., 2015; Qiao-Li et al., 2019). In this study, we used 293F cells for expressing the PRV gE protein. The size of the obtained gE recombinant protein was consistent with Lang et al.’s findings, while achieving higher purity than found in previous studies. These results provide valuable insights for developing detection methods. In this study, a total of 10 cell lines producing mAbs against PRV gE were generated. Nine strains were selected for ascites production, while one strain exhibited low supernatant titers, possibly due to a non-dominant region of antigenic determinants recognized by the cell lines. Two mAbs, namely, 12E9E7 and 3D6B2, were selected as detection and capture antibodies in the sandwich detection mode for the immunochromatographic test strip. The affinity of the two mAbs was determined to be 9.994 × 107 L/moL (12E9E7) and 5.69 × 108 L/moL, respectively. Notably, the high-affinity mAb-3D6B2 was used as capture antibodies in accordance with established principles. Furthermore, it is worth mentioning that two mAbs exhibited no cross-reactivity toward other PRV proteins and viruses, thereby demonstrating their exceptional specificity. The remaining eight mAbs can be used for fundamental research in the field of immunology, pathogen detection, antigen purification, disease diagnosis, and prevention (Liu et al., 2015). In this study, a rapid immunochromatographic test strip was developed for detection of the PR antigen using the high-affinity mAb-3D6B2 along with the highly sensitive mAb12E9E7. Gradient-diluted PRV HeNL/2017 cell cultures were tested with a positive limit dilution of 1:64 and a viral load of 1.336 × 103 copies/µL. The test strip had good specificity and showed no cross-reactivity with other viral antigens. Upon comparing the results of the test strips, it was observed that 15 samples tested positive for porcine pseudorabies virus by use of the real-time fluorescence RT-PCR detection method, while 14 samples were detected by the test strips. By analyzing these findings, it can be

speculated that this discrepancy may be attributed to the sensitivity of the porcine pseudorabies virus real-time fluorescence RT-PCR assay, which has a limit of detection lower than 1.336 × 103 copies/µL and may yield false-negative results for samples with low viral loads. It is possible that the sensitivity of the test strip is slightly lower when compared to RT-PCR; however, its higher coincidence rate (27/28) with RT-PCR results indicates that the PRV rapid test strip possesses characteristics such as convenience, speediness, high sensitivity, and high specificity. Therefore, it

TABLE 3 Detection twenty-eight samples of spleen or lymphoid tissue from pigs.

The original contributions presented in the study are included in the article, further inquiries can be directed to the corresponding author. Porcine pseudorabies virus real-time fluorescence RT-PCR detection

PRV rapid test strips Positive Negative Total Positive 14 0 14 Negative 1 13 14 Total 15 13 28

Ethics statement The animal study was approved by the Key Laboratory of Animal Immunology, Henan Academy of Agricultural Sciences, China, in line with its policies and procedures (LLSC100166). The study was conducted in accordance with the local legislation and institutional requirements.

can be effectively utilized for rapid diagnosis of clinical cases involving PR. Studies have demonstrated that since 2016, the prevalence of PRV epidemics in our country has continued to be predominantly driven by variants. The comparison of gE amino acid sequences revealed individual site mutations compared to the classical strain, while no specific mutations were observed when compared to variant strains (Ujvári et al., 2019). The monoclonal antibody used in this study is a variant-specific monoclonal antibody capable of distinguishing between the wild-type and vaccine antigens. Despite variations in the amino acid sequences of PRV variants and classical strain gE antigens, their sequence homology remains remarkably high. However, it should be noted that the monoclonal antibody employed in this study cannot differentiate between PR classical strain and variant strain antigens, which highlights an area for future research. PRV primarily manifests as a latent infection, wherein the vaccinated herd may resume normal production but still experience reactivation of hidden infections and subsequent clinical symptoms under stress. This makes them a secondary source of long-term poison and dispersion, perpetuating the circulation of the disease within the pig population for an extended period. Consequently, it significantly impedes the development of China’s pig industry. Therefore, conducting research on preventive and control measures for swine pseudorabies is crucial. The immunochromatography test strip developed in this study offers a valuable diagnostic tool for treating PR disease.

Author contributions JY: Data curation, Visualization, Writing – original draft, Writing – review & editing. HuL: Conceptualization, Methodology, Validation, Writing – review & editing. YC: Investigation, Validation, Visualization, Writing – review & editing. JZ: Investigation, Visualization, Writing – review & editing. YL: Formal analysis, Software, Writing – review & editing. ZL: Conceptualization, Investigation, Methodology, Visualization, Writing – review & editing. XZ: Supervision, Writing – review & editing. HoL: Validation, Writing – review & editing. PD: Validation, Writing – review & editing. EL: Validation, Writing – review & editing. YZ: Writing – review & editing. SW: Writing – review & editing. AW: Project administration, Visualization, Writing – review & editing.

📖 中文全文 Chinese Full Text

中文

# 用于检测伪狂犬病病毒的高灵敏度免疫层析试纸条的开发与应用

**类型** 原创研究 **发表日期** 2024年5月3日 **DOI** 10.3389/fmicb.2024.1399123 **开放获取** **编辑** 谢志训,广西兽医研究所,中国 **审稿人** 赵萌萌,佛山大学,中国 **周斌**,南京农业大学,中国

## 用于检测伪狂犬病病毒的高灵敏度免疫层析试纸条的开发与应用

**通讯作者** 王爱萍 pingaw@126.com † 这些作者对本工作做出了同等贡献

**收稿日期** 2024年3月11日 **接受日期** 2024年4月16日 **发表日期** 2024年5月3日

**引用格式**

Yin J, Liu H, Chen Y, Zhou J, Liu Y, Liang Z, Zhu X, Liu H, Ding P, Liu E, Zhang Y, Wu S and Wang A (2024) Development and application of a high-sensitivity immunochromatographic test strip for detecting pseudorabies virus. Front. Microbiol. 15:1399123. doi: 10.3389/fmicb.2024.1399123

**版权声明**

© 2024 Yin, Liu, Chen, Zhou, Liu, Liang, Zhu, Liu, Ding, Liu, Zhang, Wu and Wang. 这是一篇根据知识共享署名许可协议(CC BY)条款分发的开放获取文章。在适当引用原作者和版权持有人,并注明本期刊原始发表出处的前提下,允许在其他论坛使用、分发或复制,符合公认的学术实践规范。任何不符合上述条款的使用、分发或复制行为均不被允许。

贾佳佳 Yin¹'²†,刘慧敏 Liu¹'³†,陈玉梅 Chen¹'²'⁴,周敬明 Zhou¹'²'⁴,刘彦凯 Liu¹'²'⁴,梁正伦 Liang¹'⁴,朱希芳 Zhu¹'²'⁴,刘洪亮 Liu¹'²'⁴,丁培阳 Ding¹'²'⁴,刘恩平 Liu¹'²'⁴,张颖 Zhang¹'⁴,吴思远 Wu¹'⁴,王爱萍 Wang¹'²'⁴*

¹ 龙湖实验室,郑州,中国;² 郑州大学生命科学学院,郑州,中国;³ 郑州工程技术学院基础科学学院,郑州,河南,中国;⁴ 河南省免疫生物学重点实验室,郑州,中国

## 摘要

**引言:** 伪狂犬病(PR)是由伪狂犬病病毒(PRV)引起的一种多动物共患疾病,PRV的自然宿主为猪。2011年底,中国多个省份出现了PRV变异株,给养猪场造成了巨大的经济损失。快速检测诊断感染PRV变异株的猪只有助于预防PR的暴发。基于胶体金纳米颗粒的免疫层析试纸条因其低成本和高通量特点,常被用于临床检测。

**方法:** 本研究通过用真核系统表达的gE糖蛋白免疫小鼠,制备针对PRV的单克隆抗体。随后,基于其灵敏度和特异性筛选配对单克隆抗体,用于制备试纸条。

**结果与讨论:** 本研究制备的试纸条具有高度特异性,仅能检测到PRV,与水痘-带状疱疹病毒的糖蛋白gB、gC、gD和gE,以及猪流行性腹泻病毒、塞内卡病毒A型、猪瘟病毒、猪繁殖与呼吸综合征病毒和猪细小病毒无交叉反应。此外,该试纸条具有高灵敏度,检测限为1.336 × 10³ copies/µL(每微升病毒基因组拷贝数);与RT-PCR检测方法的一致率为96.4%。本实验室开发的试纸条为监测PRV感染和控制PR疫苗质量提供了一种有效方法。

**关键词:** 伪狂犬病病毒,单克隆抗体,免疫层析试纸条,快速抗原检测,胶体金纳米颗粒

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## 引言

伪狂犬病(PR),又称奥耶斯基病(AD),是由伪狂犬病病毒(PRV)引起的一种高度传染性病毒性疾病,可感染多种动物(Wong et al., 2019; Yu et al., 2021)。PRV于1957年首次在中国猫中发现,并在20世纪80年代传播到中国多个地区,感染多种动物。猪是PRV的自然宿主,可潜伏携带该病毒(Yu et al., 2014)。中国作为全球最大的猪肉生产国和消费国,曾经历过两次伪狂犬病暴发。第一次暴发发生在20世纪90年代,第二次发生在2011年(Dong et al., 2018)。病毒分离等实验证明,2011年暴发的根本原因是毒株发生了变异。与经典毒株相比,PRV变异株对猪表现出更高的毒力。传统的Bartha-K61疫苗株虽然能对经典毒株提供全面保护,但在防御变异株方面却显得不足(Meng et al., 2016; Cheng et al., 2020; Tan et al., 2021)。PRV发生变异并重新获得毒力,导致了中国的大规模暴发。河南作为养猪大省,受到这一疫情的严重影响。伪狂犬病野毒株在中国猪场的再次流行给养猪业和疫病防控工作带来了巨大挑战(Tan et al., 2021)。

识别、快速扑杀和疫苗接种是目前控制猪群伪狂犬病的重要措施。目前,PRV诊断的主要临床方法包括血清学检测和分子生物学技术。分子生物学检测方法包括荧光定量PCR和逆转录PCR(RT-PCR)(Cheng et al., 2021)。然而,由于PCR技术需要专业的实验室人员操作,其在猪PRV感染诊断中的应用受到限制(Porte et al., 2020)。PRV的血清学检测方法主要包括微量中和试验(MN)、间接酶联免疫吸附试验(i-ELISA)、竞争ELISA(c-ELISA)和间接免疫荧光试验(IFA)。在这些方法中,阻断ELISA因其高特异性和敏感性而被广泛应用,但耗时较长(Maan et al., 2012)。

快速抗原检测(RAD)在疾病的早期诊断和遏制中发挥着重要作用,在分子检测方法受限的情况下,有望成为PRV的重要诊断工具(Mak et al., 2020; Scohy et al., 2020)。此外,RAD还可用于监测疫苗中是否存在gE抗原残留。近年来,PR与其他猪疾病共感染的严重程度不断增加,迫切需要快速、准确地检测PR抗原。基于单克隆抗体(mAb)技术的免疫层析试纸条快速技术是一种免疫学快速检测方法,已成为快速检测的主要手段。抗原试纸条通常采用"双抗体夹心"检测模式,用于识别病毒、细菌和寄生虫等微生物抗原,以及自身抗原和肿瘤抗原等非微生物抗原(Wang et al., 2015)。因此,本研究旨在开发用于PR筛查的免疫层析试纸条。

目前,已在猪伪狂犬病病毒中鉴定出11种糖蛋白:gB(UL27)、gC(UL44)、gD(US6)、gE(US8)、gG(US4)、gH(UL22)、gI(US7)、gK(UL53)、gL(UL1)、gM(UL10)和gN(UL49.5)。由US8编码的gE蛋白在毒力中起关键作用,其缺失可降低病毒对宿主的感染能力(Tirabassi and Enquist, 1999)。因此,gE缺失毒株常用于疫苗研究。此外,gE常被用作区分疫苗接种与野毒株感染检测方法中的标志靶标(Wang et al., 2018)。利用gE蛋白作为标志物区分野毒株感染产生的抗体与疫苗接种诱导的抗体的优势在于,gE在所有野毒株中普遍表达(van Oirschot et al., 1990; Tirabassi et al., 1997),从而能够基于这一特性建立PRV抗原检测方法。

在本研究中,以gE蛋白作为免疫原免疫小鼠,制备针对PRV的单克隆抗体(mAbs)。随后,利用两种gE特异性mAb开发了PRV特异性胶体金免疫层析试纸条,PRV gE蛋白的检测限为31.25 ng/mL。本文所述的免疫分析试纸条可实现PRV gE蛋白的快速检测,适用于野毒株PRV感染的早期诊断和PRV疫苗的质量监测。

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## 材料与方法

### 伦理与生物安全声明

小鼠单克隆抗体生产的实验方案经河南省农业科学院动物免疫学重点实验室批准,符合其政策和程序(LLSC100166)。

### 试剂、毒株和细胞

DH5α感受态细胞购自北京生物医学技术有限公司。FreeStyle™ 293-F细胞购自北京义翘神州生物技术有限公司。SP2/0细胞由河南省农业科学院动物免疫学重点实验室提供(郑州,中国)。293-F细胞使用SMM 293-TII无血清培养基培养(义翘神州,中国)。SP2/0细胞使用RPMI 1640培养基(Solarbio,中国)培养,补充10%(v/v)胎牛血清(TransGen,北京)。氨基苯硼酸A6XL购自Astrea Bioseparations有限公司(剑桥,英国)。Superdex200 10/300 GL购自Cytiva(蒙大拿州,美国)。病毒株HeNL/2017(GenBank编号:MT775883)重组PRV-GFP毒株由中国科学院武汉病毒研究所王汉忠研究员惠赠。HeNL/2017毒株在补充2%(v/v)胎牛血清的DMEM中增殖。猪流行性腹泻病毒(PEDV)、塞内卡病毒A型(SVA)、猪瘟病毒(CSFV)、猪繁殖与呼吸综合征病毒(PRRSV)和猪细小病毒(PPV)由本实验保存和增殖。

### PRV gE蛋白的表达与纯化

以HeNLH/2017的基因组序列(GenBank: QQL12221.1)为序列模板构建gE蛋白,随后根据哺乳动物表达系统的密码子使用偏好进行优化,并由通用生物技术有限公司合成(安徽,中国)。按照In-Fusion HD克隆试剂盒说明书将gE插入pCAGGS质粒(HonorGene,中国),重组质粒通过线性聚乙烯亚胺(PEI)MW40000(Yisheng,中国)介导转染至293F细胞,细胞密度为2~3 × 10⁶ cells/mL。转染72小时后,通过4°C、12,000 g离心10分钟收集上清,并通过Western blot进行鉴定。

上清液经0.22 µm Stericup滤膜过滤后,通过氨基苯硼酸A6XL亲和层析进行纯化。随后,将洗脱的蛋白溶液对磷酸盐缓冲液(PBS,pH 7.4)进行透析。透析后的蛋白溶液使用截留分子量为30 K的超滤管(MilliporeSigma,美国)进行浓缩,上样至Superdex200凝胶过滤层析柱以分离重组蛋白,并通过SDS-PAGE和Western blot进行鉴定。重组gE蛋白的浓度使用NanoDrop2000分光光度计(Thermo Fisher Scientific,美国)测定。

### 抗PRV gE单克隆抗体的制备

按照标准方案制备抗PRV gE的mAbs。简言之,6周龄雌性Balb/c小鼠(n = 2)以每只小鼠10 µg的剂量在弗氏佐剂中用PRV gE蛋白进行免疫。第三次免疫后14天采集血样。以重组gE蛋白作为包被抗原,通过间接ELISA测定血清效价水平。选择血清效价高的小鼠用于制备杂交瘤细胞。筛选阳性杂交瘤细胞系,并通过ELISA鉴定阳性杂交瘤细胞系的上清液。通过有限稀释法稀释阳性杂交瘤细胞系,获得稳定产生抗体的单克隆细胞系。使用IFA进一步验证mAbs对gE蛋白的反应性。在小鼠体内制备用于胶体金标记的阳性杂交瘤腹水。

### pCAGGS-gE重组载体酶切验证

M:DL 2000;泳道1:pCAGGS-gE酶切产物。

### 免疫荧光试验

将HEK293T细胞在补充10% FBS的DMEM中培养,以2 × 10⁴ cells/well的密度接种于48孔细胞培养板中。然后在37°C、5% CO₂条件下过夜培养。当细胞达到70-80%汇合度时,使用jetPRIME多功能DNA/siRNA转染试剂(Polyplus,法国)将重组质粒pCAGGS-gE转染至细胞中,37°C培养48小时。培养结束后,用甲醇(预冷至-20°C)在室温(RT)下固定20分钟。随后,用PBST洗涤,在37°C下用脱脂奶粉(5%)封闭1小时。然后,以抗PRV gE作为一抗孵育30分钟,DMEM作为阴性对照。随后,用PBST洗涤三次,在37°C下用抗小鼠IgG H&L(FITC)(Solarbio,北京,中国)孵育半小时。

同时使用DAPI(4',6-二脒基-2-苯基吲哚,Solarbio)对细胞进行染色。最后一次洗涤后,使用德国耶蔡司荧光显微镜观察荧光信号。

### gE糖蛋白的纯化

(A)纯化PRV gE蛋白的SDS-PAGE;M:蛋白质分子量标记;泳道1:经A6XL纯化的gE蛋白;泳道2:经分子筛纯化的gE蛋白。(B)纯化gE重组蛋白与His标签抗体反应的Western blot;M:蛋白质分子量标记;泳道1:经A6XL纯化的gE蛋白;泳道2:经分子筛纯化的gE蛋白。(C)纯化gE重组蛋白与PRV阳性田间血清反应的Western blot。M:蛋白质分子量标记;泳道1:经A6XL纯化的gE蛋白;泳道2:经分子筛纯化的gE蛋白。

### 金标单克隆抗体的制备

**单克隆抗体的胶体金标记**

根据Liu等(2020)的方法,通过柠檬酸三钠法制备胶体金。随后,按以下步骤制备金标抗体:在微孔板的1-6孔中各加入10 µL超纯水,然后在1号孔中加入10 µL腹水(用ddw按1:10稀释),连续倍比稀释至6号孔。随后,每孔加入125 µL pH 9.0的胶体金溶液,充分混匀,室温静置5-15分钟。接着,每孔加入125 µL 10% NaCl溶液,室温反应10分钟,观察溶液颜色变化直至溶液颜色不再变化,此时颜色不发生变化孔对应的最高稀释度即为最适标记浓度。

将最适标记量的腹水加入1 mL胶体金溶液中,充分混匀,室温反应15分钟。然后加入100 µL含20 mmol/L浓度和10% BSA的硼酸钠溶液,充分混匀,室温孵育5分钟。

随后,将混合物在4°C、15,000 r/min条件下离心30分钟,小心去除沉淀。将沉淀重悬于含1%(w/v)BSA的硼酸缓冲液中。最后,将制备好的金标抗体保存于4°C。

### 试纸条配对单克隆抗体的筛选

在阳性克隆中,选择对PRV gE蛋白结合亲和力最高的两种mAb。按以下步骤进行:将9种mAb分别用于检测抗体和捕获抗体(金标),以"夹心法"模式使用空白试纸条筛选配对抗体。将0.3 µL检测抗体滴加于试纸条的检测膜上并干燥,然后将1 µL金标抗体滴加于结合垫上。将试纸条置于100 µL阳性样品溶液中。根据硝酸纤维素膜上的显色强度确定两种特异性抗体的配对。最后,评估所获mAb的特性。

### PRV快速检测试纸条的评估

**试纸条的特异性评估**

特异性样品盘包括PRV细胞培养物、PRV gE蛋白以及来自同一毒株的其他糖蛋白,包括PRV gB、gC和gD糖蛋白,以及HSV来源的gE糖蛋白。此外,还包括VZV、PEDV、SVA、CSFV、PRRSV和PPV等病毒株。阴性对照为PBS和培养基如DMEM。使用PRV抗原检测试纸条进行鉴定。

**试纸条的敏感性评估**

将PRV标准质粒依次稀释为9个梯度,即10⁹、10⁸、10⁷、10⁶、10⁵、10⁴、10³、10²和10¹ copies/µL,作为猪伪狂犬病病毒实时荧光RT-PCR检测的模板,绘制实时荧光RT-PCR标准曲线,获得PRV实时荧光RT-PCR检测方法的标准方程。计算PRV HeNL/2017细胞培养原液的拷贝数,并按2¹、2²、2³、2⁴、2⁵、2⁶和2⁷进行稀释。

同时,将PRV HeNL/2017细胞培养原液按2¹、2²、2³、2⁴、2⁵、2⁶和2⁷系列梯度稀释,形成敏感性样品盘。使用PRV快速检测试纸条和实时荧光RT-PCR检测敏感性样品盘的样品,并比较检测结果。

此外,将本研究制备的PRV gE蛋白进行系列稀释,范围为2,000-15.63 ng/mL,以确定试纸条的敏感性。

### 免疫层析试纸条的制备

试纸条由硝酸纤维素(NC)膜和三块垫(样品垫、结合垫和吸收垫)组成。NC膜上点样mAb-12E9E7作为检测线,葡萄球菌蛋白A(SPA)作为质控线。随后,在42°C下干燥4小时。为制备样品垫,将玻璃棉条浸泡在含0.1 mol/L NaCl、0.2% Tween-20(v/v)和0.1%(w/v)NaN₃的PBS(pH 8.0)中30分钟,在50°C干燥箱中干燥30分钟。接下来,将金标mAb以1 µg/µL的浓度喷涂在玻璃棉上,制成结合垫,同样在50°C下干燥30分钟。按照Li等(2021)的方法,将NC膜、结合垫、玻璃纤维样品垫和吸收垫依次组装在支撑板上,每层重叠1-2毫米,然后使用Bio-Dot CM4000切割机切割成2.79 mm宽的试纸条,与干燥剂一起密封在锡箔袋中,4°C保存。

### 单克隆抗体的筛选与鉴定

通过ELISA筛选出10株阳性杂交瘤细胞系(A)(柱状图颜色代表不同细胞系),mAb细胞上清效价范围为1:3,200至1:25,600(B)。IFA证实,本研究制备的所有10种mAb均与PRV gE蛋白具有强反应性。(C)mAbs与293T细胞中gE重组蛋白反应性的IFA。绿色代表抗gE mAbs,蓝色代表细胞核(标尺,200 µm)。这些结果表明,mAbs与真核表达的gE重组蛋白发生反应,与阳性对照一致。

### 试纸条的稳定性评估

为确定试纸条的稳定性,我们将试纸条密封后置于37°C培养箱中进行加速试验。将试纸条在37°C下保存1个月,检测本研究制备的PRV gE蛋白的敏感性,并根据敏感性试验结果确定其稳定性。

### 试纸条的一致率

使用PRV快速检测试纸条和猪伪狂犬病病毒实时荧光RT-PCR检测方法检测28份猪脾脏或淋巴组织样品,以猪伪狂犬病病毒实时荧光RT-PCR检测方法的结果评估与猪伪狂犬病病毒实时荧光RT-PCR检测方法的一致率。

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## 结果

### PRV gE糖蛋白的表达与纯化

使用T4 DNA连接酶将线性化的gE靶基因序列与pCAGGS载体序列连接,获得重组表达质粒pCAGGS-gE。双酶切验证的1%核酸电泳结果证实成功获得重组表达载体,大小与预期一致(图1)。

PRV gE重组蛋白在哺乳动物表达系统中成功表达和纯化。离心细胞上清液并纯化以获得重组蛋白。如图2所示,在PBS中洗脱的蛋白纯度在95%以上(图2A)。Western blot分析证实,gE重组蛋白可与抗His标签抗体(HRP)反应(图2B),也可与1:500稀释于5%脱脂奶粉中的PRV阳性田间血清反应(图2C)。

### 单克隆抗体的制备与配对抗体的筛选

**单克隆抗体的筛选与鉴定**

细胞融合后,共筛选出10株阳性杂交瘤细胞系(图3A),mAb细胞上清效价范围为1:3,200至1:25,600(图3B)。IFA证实,本研究制备的所有10种mAb均与PRV gE蛋白具有强反应性(图3C)。

### 配对抗体的筛选

选择上清效价高的9株细胞系制备腹水用于胶体金标记。抗体配对实验表明,以mAb-3D6B2作为捕获抗体、mAb-12E9E7作为检测抗体时,根据该试验中的显色效果表现最佳(图4A)。随后,纯化捕获抗体12E9E7用于制备免疫层析试纸条(图4B)。

### 单克隆抗体的特性

为更全面地了解mAb的特性,我们使用小鼠单克隆抗体同种型ELISA试剂盒(Proteintech,武汉)按照制造商说明书测定mAb的亚型。450 nm处的光密度读数表明,两种mAb均属于IgG2b和Kappa型(图5A)。两种mAb的亲和力分别为9.994 × 10⁷ L/moL(12E9E7)(图5B)和5.69 × 10⁸ L/moL(3D6B2)(图5C)。此外,为确定mAb的特异性,使用Dot-ELISA同时检测PRV细胞培养物、PRV-gE蛋白、PRV-gB蛋白、PRV-gC蛋白、PRV-gD蛋白、VSV-gE蛋白以及PEDV、SVA、HSV、CSFV、PRRSV、PPV细胞培养物和PBS。结果表明,mAb与PRV细胞培养物和gE重组蛋白特异性反应,而对其他PRV蛋白或疾病无反应(图5D)。

### 快速检测免疫层析试纸条的建立

将3D6B2的胶体金偶联物喷涂在玻璃纤维垫上作为偶联mAb。将mAb 12E9E7(1 mg/mL)喷涂在NC膜上形成检测线。然后,将SPA在PBS中稀释至0.5 mg/mL作为质控线。两种PRV特异性mAb通过双抗体夹心模式检测PRV。

### 试纸条的特异性

使用PRV快速检测试纸条检测特异性样品盘,结果如图6所示;仅在检测PRV细胞培养物时,PRV快速检测试纸条的T线和C线均显色,而检测PRV-gB、PRV-gC、PRV-gD、HSV、VZV、PEDV、SVA、CSFV、PRRSV、PPV的培养基和阴性对照显示T线不显色而C线显色,表明PRV快速检测试纸条具有良好的特异性。

### PRV实时荧光RT-PCR检测方法

以梯度稀释的PRV标准质粒为模板,使用PRV实时荧光RT-PCR检测绘制标准曲线。标准曲线方程确定为y = -4.2401x + 40.718(R² = 0.9898)(图7)。当Ct值>34.0时,表明检测结果为阴性,对应的病毒拷贝数低于38 copies/µL,从而确定RT-PCR检测的检测限为38 copies/µL。

### 试纸条中gE蛋白的检测限

将本研究制备的PRV gE蛋白进行系列稀释,范围为2,000至15.63 ng/mL,以确定试纸条的敏感性。随着样品中蛋白浓度的降低,G/D × area-ROD值降低,结果表明RBD的检测限为31.25 ng/mL(图8;表1)。

### 试纸条的稳定性

试纸条在37°C下保存1个月后,对本研究制备的PRV gE蛋白的检测限仍为31.25 ng/mL,表明试纸条具有良好的稳定性(图10)。

### 试纸条对PRV的检测限

将PRV HeNL/2017细胞培养原液稀释后,使用PRV快速检测试纸条和实时荧光RT-PCR检测方法进行检测。结果如图9所示。快速检测试纸条的检测限为1:64,对应的病毒载量为1.336 × 10³ copies/µL(表2)。因此,PRV快速检测试纸条的检测拷贝数为1.336 × 10³ copies/µL。

### PRV快速检测试纸条的一致率

使用PRV快速检测试纸条和实时荧光RT-PCR检测28份猪脾脏或淋巴组织样品。结果如表3所示;实时荧光RT-PCR检测方法检出15份猪伪狂犬病病毒阳性样品,PRV快速检测试纸条检出14份阳性样品。根据猪伪狂犬病病毒实时荧光RT-PCR检测方法的检测结果,PRV快速检测试纸条的一致率为96.4%(27/28)。

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## 讨论

作为一种潜在的人畜共患病,PRV对养殖业和公共卫生安全构成威胁(Ai et al., 2018; Wang et al., 2020)。自2011年以来,中国猪场野毒株PRV的流行给养猪业和疫病防控带来了重大挑战。为控制这些国内流行变异株,研究人员以PRV变异株为亲本株开发了基因缺失疫苗。该疫苗可为猪提供完全的免疫保护效力,是PRV变异株的理想候选疫苗。为加强中国PRV的防控,强制接种辅以病毒学和血清学监测以及严格的生物安全措施。必须加强全国范围内的检测,并强化对猪以外动物感染的监测。尽管PRV的传统检测方法如ELISA、RT-PCR、qPCR(Deblanc et al., 2019; Cheng et al., 2021)和兔接种试验是准确的,但它们确实存在一定的局限性。例如,PCR技术需要高级技能,可能不适合常规农场检测;兔接种试验需要专业人员,不适合大规模畜牧业;基于样品中抗体的ELISA可能错过防控的最佳时期。尽管胶体硒和上转换荧光纳米颗粒等新型标记材料丰富(Li et al., 2011),本研究仍选择常规胶体金,因为胶体金更稳定、更灵敏、更特异。检测结果肉眼可见,具有耗时短、灵敏度高、特异性好、适合基层推广应用等特点(Li et al., 2015, 2023)。

在本研究中,我们选择PRV gE蛋白作为研究靶标,原因如下:首先,gE蛋白是位于病毒包膜上的糖蛋白,常用于检测野毒株感染,其抗体检测也可区分野毒株感染和疫苗免疫动物(Nauwynck, 1997; Ao et al., 2003)。此外,建立检测gE蛋白的方法可对灭活疫苗和gE缺失活疫苗进行严格的质量控制。据报道,PRV gE蛋白已在大肠杆菌、酵母和昆虫细胞中成功表达。建立的ELISA、免疫荧光等方法可有效区分野毒株感染与疫苗诱导的免疫抗体,显示出良好的应用前景。然而,一些常规挑战仍然存在:原核表达系统表达的大多数gE重组蛋白以包涵体形式存在,抗原活性低,往往无法满足临床检测要求(Wu et al., 2023)。酵母表达系统表达量低(Ren, 2004),昆虫系统表达周期长(Zhu et al., 2019)。所有这些因素都显著影响了PRV gE蛋白的实际应用。HEK 293F表达系统对表达的蛋白进行修饰,确保正确折叠、高水平蛋白表达,并保持更完整的天然构象和增强的生物活性(Nettleship et al., 2015; Qiao-Li et al., 2019)。在本研究中,我们使用293F细胞表达PRV gE蛋白。所获gE重组蛋白的大小与Lang等的发现一致,同时实现了比以往研究更高的纯度。这些结果为开发检测方法提供了有价值的见解。

在本研究中,共产生了10株产生抗PRV gE mAb的细胞系。选择9株制备腹水,一株上清效价较低,可能是由于细胞系识别的抗原决定簇非优势区域。选择两种mAb,即12E9E7和3D6B2,作为免疫层析试纸条夹心检测模式中的检测抗体和捕获抗体。两种mAb的亲和力分别确定为9.994 × 10⁷ L/moL(12E9E7)和5.69 × 10⁸ L/moL。值得注意的是,按照既定原则,高亲和力mAb-3D6B2用作捕获抗体。此外,两种mAb对其他PRV蛋白和病毒无交叉反应,从而证明了其优异的特异性。其余8种mAb可用于免疫学、病原检测、抗原纯化、疾病诊断和预防领域的基础研究(Liu et al., 2015)。在本研究中,利用高亲和力mAb-3D6B2和高灵敏度mAb-12E9E7开发了用于检测PR抗原的快速免疫层析试纸条。梯度稀释的PRV HeNL/2017细胞培养物经检测,阳性极限稀释度为1:64,病毒载量为1.336 × 10³ copies/µL。试纸条具有良好的特异性,与其他病毒抗原无交叉反应。比较试纸条的结果发现,使用实时荧光RT-PCR检测方法检出15份猪伪狂犬病病毒阳性样品,而试纸条检出14份。通过分析这些结果,可以推测这种差异可能归因于猪伪狂犬病病毒实时荧光RT-PCR检测的敏感性,其检测限低于1.336 × 10³ copies/µL,可能对低病毒载量样品产生假阴性结果。与RT-PCR相比,试纸条的敏感性可能略低;然而,其与RT-PCR结果的高一致率(27/28)表明,PRV快速检测试纸条具有便捷、快速、高灵敏度和高特异性等特点。因此,它可有效用于PR临床病例的快速诊断。

研究表明,自2016年以来,我国PRV疫情的流行仍以变异株为主。gE氨基酸序列比较显示,与经典毒株相比存在个别位点突变,而与变异株相比未观察到特异性突变(Ujvári et al., 2019)。本研究中使用的单克隆抗体是一种变异株特异性单克隆抗体,能够区分野毒株和疫苗抗原。尽管PRV变异株和经典毒株gE抗原的氨基酸序列存在差异,但其序列同源性仍然非常高。然而,需要注意的是,本研究中使用的单克隆抗体无法区分PR经典毒株和变异株抗原,这是未来研究的一个方向。

PRV主要表现为潜伏感染,接种疫苗的猪群可能恢复正常生产,但在应激条件下仍可重新激活隐藏的感染并出现临床症状。这使它们成为长期排毒和传播的继发来源,使疾病在猪群中持续流行较长时间。因此,它严重阻碍了中国养猪业的发展。因此,开展猪伪狂犬病防控措施的研究至关重要。本研究开发的免疫层析试纸条为PR疾病的治疗提供了有价值的诊断工具。

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## 数据可用性声明

本研究中提出的原始贡献包含在文章中,进一步的询问可联系通讯作者。

## 伦理声明

动物研究经河南省农业科学院动物免疫学重点实验室批准,符合其政策和程序(LLSC100166)。本研究按照当地立法和机构要求进行。

## 作者贡献

JY:数据整理、可视化、撰写——初稿、撰写——审阅编辑。HuL:概念化、方法学、验证、撰写——审阅编辑。YC:调查、验证、可视化、撰写——审阅编辑。JZ:调查、可视化、撰写——审阅编辑。YL:形式分析、软件、撰写——审阅编辑。ZL:概念化、调查、方法学、可视化、撰写——审阅编辑。XZ:监督、撰写——审阅编辑。HoL:验证、撰写——审阅编辑。PD:验证、撰写——审阅编辑。EL:验证、撰写——审阅编辑。YZ:撰写——审阅编辑。SW:撰写——审阅编辑。AW:项目管理、可视化、撰写——审阅编辑。