Fangchinoline inhibits the PEDV replication in intestinal epithelial cells via autophagic flux suppression

✅ 全文

防己碱通过抑制自噬流抑制肠上皮细胞中PEDV的复制

作者 Weixiao Zhang; Haiyan Shen; Menglu Wang; Xuelei Fan; Songqi Wang; Nile Wuri; Bin Zhang; Haiyan He; Chunhong Zhang; Zhicheng Liu; Ming Liao; Jianfeng Zhang; Yugu Li; Jianmin Zhang 期刊 Frontiers in Microbiology 发表日期 2023 卷/期/页码 Vol. 14 ISSN 1664-302X DOI 10.3389/fmicb.2023.1164851 类型 原创研究 (Original Research)

📄 英文摘要 English Abstract

EN

Animal and human health are severely threatened by coronaviruses. The enteropathogenic coronavirus, porcine epidemic diarrhea virus (PEDV), is highly contagious, leading to porcine epidemic diarrhea (PED), which causes large economic losses in the world's swine industry. Piglets are not protected from emerging PEDV variants; therefore, new antiviral measures for PED control are urgently required. Herein, the anti-PEDV effects and potential mechanisms of fangchinoline (Fan) were investigated. Fan dose-dependently inhibited a PEDV infection at 24 h post-infection (EC50 value = 0.67 μM). We found that Fan mainly affected the PEDV replication phase but also inhibited PEDV at the attachment and internalization stages of the viral life cycle. Mechanistically, Fan blocked the autophagic flux in PEDV-infected cells by regulating the expression of autophagy-related proteins and changing PEDV virus particles. In summary, Fan inhibits PEDV infection by blocking the autophagic flux in cells. Our findings will help develop new strategies to prevent and treat PEDV infection.

📄 中文摘要 Chinese Abstract

中文
冠状病毒严重威胁动物和人类健康。肠道致病性冠状病毒——猪流行性腹泻病毒(PEDV)具有高度传染性,可导致猪流行性腹泻(PED),给全球养猪业造成巨大经济损失。仔猪对新兴PEDV变异株缺乏保护力,因此迫切需要新的抗病毒措施来控制PED。防己诺林碱(Fan)是一种传统中草药单体,是中药粉防己(Stephaniae Tetrandrine S. Moore)干燥根中的主要生物碱成分之一。Fan可调节自噬和凋亡、抑制炎症小体活化并抑制谷氨酸释放。近期研究表明,Fan可通过未知机制抑制HCoV-OC43感染。自噬参与多种病原体感染过程;研究发现PEDV可诱导活性氧(ROS)依赖性内质网(ER)应激介导的自噬以促进病毒复制,且PEDV诱导的自噬有利于其复制。因此,鉴于PEDV与自噬之间的关联,寻找通过破坏自噬来抑制PEDV的药物具有重要意义。

📋 英文结构化总结 English Structured Summary

全文整理

EN

Background:

Animal and human health are severely threatened by coronaviruses. The enteropathogenic coronavirus, porcine epidemic diarrhea virus (PEDV), is highly contagious, leading to porcine epidemic diarrhea (PED), which causes large economic losses in the world’s swine industry. Piglets are not protected from emerging PEDV variants; therefore, new antiviral measures for PED control are urgently required. Fangchinoline (Fan), a traditional Chinese herb monomer, is one of the major dried root alkaloidal components of radix Stephaniae Tetrandrine S. Moore. Fan can regulate autophagy and apoptosis, inactivate the inflammasome, and inhibit glutamate release. Recently, Fan was demonstrated to inhibit HCoV-OC43 infection via an unknown mechanism. Autophagy is involved in multiple pathogen infections; PEDV was observed to induce reactive oxygen species (ROS)-dependent endoplasmic reticulum (ER) stress-mediated autophagy to promote viral replication, and PEDV induced autophagy to benefit its replication. Therefore, considering the association between PEDV and autophagy, it would be useful to find drugs that inhibit PEDV via autophagic disruption.

Methods:

IPEC-J2 cells (porcine intestinal epithelial cells) were cultured in DMEM/F-12 containing 10% FBS and 1% penicillin–streptomycin at 37°C in a humidified atmosphere with 5% CO₂. The PEDV strain GD/HZ/2016 (GenBank Accession: OP191700.1) was propagated in Vero cells in DMEM containing trypsin. Fangchinoline (HY-N1372A), wortmannin, chloroquine, and bafilomycin A1 were purchased from MedChemExpress. For cytotoxicity testing, IPEC-J2 cells seeded in a 96-well plate were treated with 0, 2.5, 5, 10, 20, 40, and 80 µM Fan for 48 h. Cell viability was tested using a cell counting kit-8 (CCK-8), and the percentage of viable cells was calculated as (ODt/ODc) × 100%. The 50% cell cytotoxicity (CC50) was calculated from data generated.

Results:

Fan dose-dependently inhibited a PEDV infection at 24 h post-infection (EC50 value = 0.67 µM). Fan mainly affected the PEDV replication phase but also inhibited PEDV at the attachment and internalization stages of the viral life cycle. Mechanistically, Fan blocked the autophagic flux in PEDV-infected cells by regulating the expression of autophagy-related proteins and changing PEDV virus particles.

Data Summary:

Fan inhibited PEDV infection with an EC50 value of 0.67 µM at 24 h post-infection. The cytotoxicity of Fan toward IPEC-J2 cells was assessed using CCK-8, with CC50 calculated from the generated data.

Conclusions:

In summary, Fan inhibits PEDV infection by blocking the autophagic flux in cells. Our findings will help develop new strategies to prevent and treat PEDV infection. Fan could be used as the basis for anti-viral drugs to curb PED outbreaks.

Practical Significance:

Fan could be used as the basis for anti-viral drugs to curb PED outbreaks, highlighting its potential use to treat PEDV infection and develop new strategies to prevent and treat PEDV infection.

📋 中文结构化总结 Chinese Structured Summary

中文

背景:

冠状病毒严重威胁动物和人类健康。肠道致病性冠状病毒——猪流行性腹泻病毒(PEDV)具有高度传染性,可导致猪流行性腹泻(PED),给全球养猪业造成巨大经济损失。仔猪对新兴PEDV变异株缺乏保护力,因此迫切需要新的抗病毒措施来控制PED。防己诺林碱(Fan)是一种传统中草药单体,是中药粉防己(Stephaniae Tetrandrine S. Moore)干燥根中的主要生物碱成分之一。Fan可调节自噬和凋亡、抑制炎症小体活化并抑制谷氨酸释放。近期研究表明,Fan可通过未知机制抑制HCoV-OC43感染。自噬参与多种病原体感染过程;研究发现PEDV可诱导活性氧(ROS)依赖性内质网(ER)应激介导的自噬以促进病毒复制,且PEDV诱导的自噬有利于其复制。因此,鉴于PEDV与自噬之间的关联,寻找通过破坏自噬来抑制PEDV的药物具有重要意义。

方法:

IPEC-J2细胞(猪小肠上皮细胞)在含10%胎牛血清和1%青霉素-链霉素的DMEM/F-12培养基中,于37°C、5% CO₂的湿润环境中培养。PEDV毒株GD/HZ/2016(GenBank登录号:OP191700.1)在含胰蛋白酶的DMEM培养基中于Vero细胞中增殖。防己诺林碱(HY-N1372A)、渥曼青霉素、氯喹和巴佛洛霉素A1均购自MedChemExpress。细胞毒性检测中,将接种于96孔板的IPEC-J2细胞分别用0、2.5、5、10、20、40和80 µM Fan处理48小时。使用细胞计数试剂盒-8(CCK-8)检测细胞活力,活细胞百分比按(ODt/ODc)×1100%计算。50%细胞毒性浓度(CC50)由所生成的数据计算得出。

结果:

Fan在感染后24小时呈剂量依赖性抑制PEDV感染(EC50值=0.67 µM)。Fan主要影响PEDV复制阶段,同时也抑制PEDV病毒生命周期中的吸附和内化阶段。机制上,Fan通过调控自噬相关蛋白的表达并改变PEDV病毒颗粒,阻断PEDV感染细胞中的自噬流。

数据总结:

Fan在感染后24小时抑制PEDV感染,EC50值为0.67 µM。使用CCK-8评估Fan对IPEC-J2细胞的细胞毒性,CC50由所生成的数据计算得出。

结论:

综上所述,Fan通过阻断细胞自噬流来抑制PEDV感染。我们的发现将有助于开发预防和治疗PEDV感染的新策略。Fan可作为抗病毒药物的基础,用于遏制PED暴发。

实际意义:

Fan可作为抗病毒药物的基础用于遏制PED暴发,凸显了其在治疗PEDV感染以及开发预防和治疗PEDV感染新策略方面的潜在应用价值。

📖 英文全文 English Full Text

EN

TYPE Original Research PUBLISHED 07 July 2023 DOI 10.3389/fmicb.2023.1164851 OPEN ACCESS EDITED BY

Fateh Singh, ICAR-National Institute of High Security Animal Diseases (ICAR-NIHSAD), India REVIEWED BY

Gaopeng Hou, Washington University in St. Louis, United States Jung-Eun Park, Chungnam National University, Republic of Korea Yun Chen, Hainan University, China Haifei Wang, Yangzhou University, China *CORRESPONDENCE

Jianmin Zhang junfeng-v@163.com Yugu Li liyugu@scau.edu.cn †

These authors have contributed equally to this work and share first authorship RECEIVED 13 February 2023 ACCEPTED 19 June 2023 PUBLISHED 07 July 2023 CITATION

Zhang W, Shen H, Wang M, Fan X, Wang S, Wuri N, Zhang B, He H, Zhang C, Liu Z, Liao M, Zhang J, Li Y and Zhang J (2023) Fangchinoline inhibits the PEDV replication in intestinal epithelial cells via autophagic flux suppression. Front. Microbiol. 14:1164851. doi: 10.3389/fmicb.2023.1164851 COPYRIGHT

© 2023 Zhang, Shen, Wang, Fan, Wang, Wuri, Zhang, He, Zhang, Liu, Liao, Zhang, Li and Zhang. 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.

Fangchinoline inhibits the PEDV replication in intestinal epithelial cells via autophagic flux suppression Weixiao Zhang1,2† , Haiyan Shen2,3† , Menglu Wang1,2 , Xuelei Fan1,2 , Songqi Wang1,2 , Nile Wuri2,4 , Bin Zhang2,4 , Haiyan He2,4 , Chunhong Zhang2,3 , Zhicheng Liu2,3 , Ming Liao2,3 , Jianfeng Zhang2,3 , Yugu Li1* and Jianmin Zhang1* 1 College of Veterinary Medicine, South China Agricultural University, Guangzhou, China, 2 Key Laboratory of Livestock Disease Prevention of Guangdong Province, Scientific Observation and Experiment Station of Veterinary Drugs and Diagnostic Techniques of Guangdong Province, Ministry of Agriculture and Rural Affairs, Institute of Animal Health, Guangdong Academy of Agricultural Sciences, Guangzhou, China, 3 Maoming Branch Center of Guangdong Laboratory for Lingnan Modern Agricultural Science and Technology, Guangzhou, China, 4 College of Veterinary Medicine, Inner Mongolia Agricultural University, Hohhot, China

Animal and human health are severely threatened by coronaviruses. The enteropathogenic coronavirus, porcine epidemic diarrhea virus (PEDV), is highly contagious, leading to porcine epidemic diarrhea (PED), which causes large economic losses in the world’s swine industry. Piglets are not protected from emerging PEDV variants; therefore, new antiviral measures for PED control are urgently required. Herein, the anti-PEDV effects and potential mechanisms of fangchinoline (Fan) were investigated. Fan dose-dependently inhibited a PEDV infection at 24 h post-infection (EC50 value = 0.67 µM). We found that Fan mainly affected the PEDV replication phase but also inhibited PEDV at the attachment and internalization stages of the viral life cycle. Mechanistically, Fan blocked the autophagic flux in PEDV-infected cells by regulating the expression of autophagy-related proteins and changing PEDV virus particles. In summary, Fan inhibits PEDV infection by blocking the autophagic flux in cells. Our findings will help develop new strategies to prevent and treat PEDV infection. KEYWORDS

porcine epidemic diarrhea virus, fangchinoline, antiviral agent, autophagy, replication

1. Introduction The enteropathogenic coronavirus, porcine epidemic diarrhea virus (PEDV), causes porcine epidemic diarrhea (PED) (Belouzard et al., 2012). PED damages the intestine via villus atrophy and shedding in pigs of any age. However, PEDV-infected neonatal piglets develop acute watery diarrhea and vomiting, with almost 100% mortality (Alvarez et al., 2015). PED was first reported in 1978; however, in China in 2010, a new PEDV variant strain emerged. Since then, PED has spread worldwide, causing huge losses to the pig industry (Stevenson et al., 2013; Lowe et al., 2014). Commercial PEDV vaccines are available; however, PEDV still persists, and the emergent variant strains make PEDV control more difficult (Pensaert and de Bouck, 1978; Sun et al., 2016; Yu et al., 2018).

Consequently, there is an urgent need to develop drugs to prevent porcine PEDV infection. For thousands of years, herbal medicines have been used to treat viral illnesses, thus representing potential sources of anticoronavirus treatment (Wen et al., 2011; Ling, 2020; Yang et al., 2020). Fangchinoline (Fan), a traditional Chinese herb monomera, is one of the major dried root alkaloidal components of radix Stephaniae Tetrandrine S. Moore (Zhu, W. et al., 2019). Fan can regulate autophagy and apoptosis, inactivate the inflammasome, and inhibit glutamate release (Lin et al., 2009; Fan et al., 2017; Tang et al., 2017; Liu et al., 2019). To date, most studies have focused on its anticancer activity. Recently, Fan was demonstrated to inhibit HCoV-OC43 infection via an unknown mechanism (Kim et al., 2019). Autophagy is involved in multiple pathogen infections. Studies have shown that some viruses can induce host cell autophagy, thereby promoting viral proliferation (Xu et al., 2018; Khabir et al., 2020). PEDV was observed to induce reactive oxygen species (ROS)-dependent endoplasmic reticulum (ER) stressmediated autophagy to promote viral replication (Sun et al., 2021). Moreover, PEDV induced autophagy to benefit its replication (Guo et al., 2017). PEDV replication was promoted by nsp6-induced autophagy, mainly occurring via the PI3K/Akt/mTOR signaling pathway (Lin et al., 2020). Therefore, considering the association between PEDV and autophagy, it would be useful to find drugs that inhibit PEDV via autophagic disruption. Herein, we aimed to assess Fan’s antiviral activity against PEDV in IPEC-J2 cells (porcine intestinal epithelial cells) and determine Fan’s antiviral mechanisms by inhibiting autophagic flux. Our study highlights the potential use of Fan to treat PEDV infection. Fan could be used as the basis for anti-viral drugs to curb PED outbreaks.

IPEC-J2 cells seeded in a 96-well plate were treated with 0, 2.5, 5, 10, 20, 40, and 80 µM Fan for 48 h. A cell counting kit-8 (CCK-8) (Abcam, China) was then used to test cell viability, following the supplier’s guidelines. For each concentration, the percentage of viable cells was determined as follows:   ODt × 100%, ODc where ODt and ODc are the absorbance of treated and control cells, respectively. We calculated 50% cell cytotoxicity (CC50 ) from data-generated dose–response curves subjected to non-linear regression analysis.

2.3. Time-of-addition assay PEDV strain GD/HZ/2016 was used to infect IPEC-J2 cells at a multiplicity of infection (MOI) of 0.1 and incubated for 1 h. Drugcontaining medium (20 µM of Fan) was added at different time points relative to the 1-h period of cell infection with PEDV (MOI = 0.1). Fan was added to the pre-treatment group (Pre) 1 h before the viral infection. It was added at the start of viral incubation in the co-treatment group (Co) and after virus incubation in the post-treatment group (Po). Fan was added throughout the infection period in the full-duration treatment group (Full). It was not added to the virus control group (VC). Following infection, the inoculum was replaced with fresh medium, and the cells were incubated for another 23 h. Thereafter, supernatants and cells were collected for all groups. Quantitative real-time reverse transcription PCR (qRTPCR) was used to assess viral RNA levels, and the Median Tissue Culture Infectious Dose (TCID50 ) was used to assess the virus titers (Wang et al., 2016; Lai et al., 2020).

2. Materials and methods 2.4. Viral attachment, internalization, and replication assays

2.1. Virus, cells, and reagents Dulbecco’s Modified Eagle Medium (DMEM; Invitrogen, Carlsbad, CA, United States) containing 10% fetal bovine serum (FBS; Gibco, Grand Island, NY, United States) and 1% penicillin– streptomycin (NCM Biotech, Newport, RI, United States) was used to culture African green monkey kidney cells (Vero). IPEC-J2 cells (provided by Dr. Li Wang, Institute of Animal Science, Guangdong Academy of Agricultural Sciences China) were cultured in DMEM/F-12 (Gibco; Invitrogen, Carlsbad, CA, United States) containing 10% FBS and 1% penicillin–streptomycin. Both cell lines were cultured at 37◦ C in a humidified atmosphere with 5% CO2 . The PEDV strain GD/HZ/2016 (GenBank Accession: OP191700.1) was isolated, identified, and stored in our laboratory at the Institute of Animal Health, Guangdong Academy of Agricultural Sciences, Guangzhou, China. The GD/HZ/2016 strain was propagated in Vero cells in DMEM containing trypsin. Fangchinoline (HY-N1372A), wortmannin (SL-2052), chloroquine (HY-17589A), and bafilomycin A1 (HY-100558) were purchased from MedChemExpress (Monmouth Junction, NJ, United States).

2.4.1. Attachment assay Cells were cooled for 1 h at 4◦ C and treated with various concentrations of Fan (0, 2.5, 5, 10, and 20 µM) and then infected with PEDV GD/HZ/2016 (MOI = 0.5) at 4◦ C together with various concentrations of Fan and incubated for 1 h, during which time the viruses would adsorb onto the cell membrane but would not penetrate the cells. The cells were washed with ice-cold phosphatebuffered saline (PBS) (Zhu, Z. et al., 2019) and then cultured in the medium for 24 h at 37◦ C. To assess Fan’s effect on virus attachment, the supernatants were subjected to TCID50 analysis, and cell samples were collected for Western blotting and qRTPCR analyses.

2.4.2. Entry assay PEDV GD/HZ/2016 (0.5 MOI) was used to infect IPEC-J2 cells at 4◦ C for 1 h. The cells were then washed thrice with cold 02 frontiersin.org Zhang et al. 10.3389/fmicb.2023.1164851

PBS. Fan (0, 2.5, 5,10, and 20 µM) was added to each sample and incubated for 1 h at 37◦ C. The cells were washed thrice using PBS, a fresh medium was added, and then, the cells were incubated for 24 h. Next, the intracellular viral RNA, protein levels, and the supernatant virus titers were determined using qRT-PCR, Western blotting, and TCID50 , respectively.

(ThermoFisher Scientific, China) was used to lyse the cells. The resultant proteins were separated and then transferred to a polyvinylidene fluoride membrane. The membrane was, then, incubated for 1 h in 5% non-fat milk and incubated for 2 h with the following primary antibodies: anti-PEDV N-protein (Medgene Labs, United States), anti-glyceraldehyde-3-phosphate dehydrogenase (GAPDH; ABclonal, China), anti-microtubuleassociated protein 1 light chain 3 alpha isoform IIB (LC3II; NOVUS, United States), and anti-sequestosome 1 (SQSTM1/P62; ABclonal, China), followed by three washes with PBST. The membranes were then incubated with horseradish peroxidase (HRP)-conjugated goat anti-mouse and anti-rabbit IgG (H+L) secondary antibodies (Bioworld, China). Immunoreactive protein bands were visualized using an ECL Kit (Millipore, China).

2.4.3. Replication assay PEDV GD/HZ/2016 (0.1 MOI) was used to infect IPEC-J2 cells at 37◦ C for 1 h and then washed thrice using PBS to remove free virus particles. Then, fresh medium with 20 µM Fan was added to the cells. At 9 and 12 h post-infection, the RNA and protein levels of the PEDV N gene were detected using qRT-PCR and Western blotting, respectively.

2.8. Immunofluorescence assay 2.4.4. Release assay PEDV GD/HZ/2016 (0.1 MOI) was used to infect IPEC-J2 cells at 37◦ C for 1 h and then washed thrice using PBS to remove free virus particles. The cells were, then, incubated for 24 h at 37◦ C in the fresh medium containing different concentrations of Fan. Then, the collected cells or cell supernatants were subjected to qRT-PCR assays to determine the number of viral RNA copies.

Cells were fixed using 4% paraformaldehyde (Beyotime, China) and permeabilized with PBS containing 0.1% Triton X-100. Then, 1% bovine serum albumin (BBI Life Sciences, China) was used to block the cells for 1 h. Then, a mouse anti-PEDV N IgG antibody was incubated with the cells overnight at 4◦ C and then with Alexa FluorTM 594 goat anti-mouse IgG (Invitrogen, China) for ′ 1 h at 37◦ C. Thereafter, cells were incubated with 4 ,6-diamidino2-phenylindole (DAPI, Beyotime) for 5 min after washing with PBS three times. Then, the cells were examined using a differential fluorescence microscope.

2.5. Regulating cell autophagy using inhibitors IPEC-J2 cells were treated with wortmannin (0.1 µM), chloroquine (20 µM), or bafilomycin A1 (0.2 µM; all added directly to the medium) for 1 h and then infected with PEDV (MOI = 0.1) for 1 h at 37◦ C. Then, three washes with PBS removed the unbound viruses, followed by incubation in DMEM/F12 containing 2% FBS with varying concentrations of wortmannin, chloroquine, or bafilomycin A1. The control group was infected with PEDV only. Collected cells were subjected to qRT-PCR and Western blotting to determine the changes in PEDV N mRNA and protein levels. Virus titers were measured in cell supernatants using the TCID50 assay.

2.9. Viral titration Vero cells grown to 70%−80% confluence in a 96-well plate were infected with 10-fold serial dilutions of PEDV (n = 4 replicates) and incubated for 72 h at 37◦ C, followed by Immunofluorescence assay (IFA) assessment. The virus titers were determined using the Reed–Muench method (expressed as TCID50 per milliliter).

2.10. Calculation of the EC50 2.6. qRT-PCR

For the dose-dependent assay, PEDV strain GD/HZ/2016 was infected with IPEC-J2 cells in 12-well cell culture plates, which were then treated with increasing concentrations of Fan from 0 to 20 µM. qRT-PCR determined the PEDV N mRNA levels, and the inhibition value was calculated using the following formula: 1− mRNA (Fan) mRNA (mock) ×100%. A dose–response curve was established using the inhibitory value and the Fan concentration to calculate the EC50 (half maximal effective concentration).

The TaKaRa MiniBEST Universal RNA Extraction Kit (TaKaRa, China) was used to extract total RNA from differently treated IPEC-J2 cells. The qRT-PCR was then performed using a HiScript R II One Step qRT-PCR SYBR Green Kit (Vazyme, China) and the following primers: PEDV-N-F: GCAAAGACTGAACCCACTAAT, PEDV-N-R: GCCTCTGTTGTTACTTGGAG and βactin-F: GGACTTCGAGCAGGAGATGG, β-actinR: AGGAAGGAGGGCTGGAAGAG.

2.11. Statistical analysis 2.7. Western blotting assay The data are shown as the mean ± SD. Graph construction and statistical analyses were performed using GraphPad Prism 8.0, and Image J was used to quantify the immunoreactive

The procedure was carried out as described in a previous study (Wang et al., 2020). In brief, 150 µl of lysis buffer Frontiers in Microbiology 03 frontiersin.org Zhang et al. 10.3389/fmicb.2023.1164851

FIGURE 1

The cellular toxicity and anti-PEDV activity of Fan in IPEC-J2 cell cultures. (A) IPEC-J2 cells were treated with various concentrations of Fan at 37◦ C for 48 h. Cell viability was evaluated using CCK-8 assays. (B–D) Fan at various concentrations was used to treat cells for 1 h before PEDV GD/HZ/2016 infection (0.1 MOI), and the cells were then treated with various Fan concentrations for 24 h. At 24 hpi, supernatants and intact cells were collected. (B) Western blotting assessment of PEDV N protein levels. (C) QRT-PCR quantification of PEDV N mRNA levels. (D) TCID50 assay to determine the viral titers. (E) Assessment of the EC50 of Fan toward PEDV infection. (F) Effect of Fan on the inhibition of PEDV analyzed using IFA. * P < 0.05; ** P < 0.01; *** P < 0.001; and **** P < 0.0001 indicate significant differences vs. the control group.

protein bands. Statistical analysis was performed using a oneway analysis of variance (ANOVA). A P-value of <0.05 indicated statistical significance.

cytotoxic to IPEC-J2 cells at 20 µM (CC50 = 37.49 µM; Figure 1A). According to the non-cytotoxic range of Fan, we evaluated its inhibition of PEDV infection. The levels of the PEDV N protein declined markedly with increasing Fan concentration (Figure 1B). The qRT-PCR analysis showed that the PEDV N mRNA levels were downregulated by Fan treatment (Figure 1C), with an EC50 value of 0.67 µM (Figure 1E). Moreover, 20 µM

3. Results 3.1. Fan protects cells against PEDV infection

Fan treatment decreased the virus titers significantly from 107 to 100.75 TCID50 /ml (Figure 1D). IFA showed that Fan inhibited PEDV infection of IPEC-J2 cells in a concentration-dependent manner (Figure 1F).

We first evaluated Fan-related cytotoxicity toward IPEC-J2 cells using the CCK-8 assay, which revealed that Fan was not Frontiers in Microbiology 04 frontiersin.org Zhang et al. 10.3389/fmicb.2023.1164851

FIGURE 2

Time of addition assays of Fan. (A) IPEC-J2 cells were cultured in 12-well plates and then treated using 20 µM Fan for 1 h before infection with the virus (pre-treatment), for 1 h during infection with the virus (co-treatment), for 23 h after infection with the virus removal (post-treatment), or during the whole infection period (full-time treatment). (B) PEDV RNA levels were determined using qRT-PCR analysis. (C, D) Western blotting detection of the effects of Fan (20 µM) on PEDV infection in IPEC-J2 cells various times (12–36 h). (E) The effects of Fan (20 µM) on PEDV N mRNA in IPEC-J2 cells for various times (12–36 h). VC, virus control; Pre, pre-treatment; Co, co-treatment; Po, post-treatment; Full, full-duration treatment. *P < 0.05; **P < 0.01; ***P < 0.001; and ****P < 0.0001 indicate significant differences vs. the control group.

3.2. Fan-inhibited PEDV in both early and late stages of infection To determine which stage of PEDV infection was mainly affected by Fan, the time of addition analysis was used (Figure 2A). Fan reduced the PEDV N mRNA levels during the whole viral life cycle. It had the strongest inhibitory effect at the post-treatment stage (∼98.86% inhibition), indicating that Fan mainly inhibited PEDV infection at the later stage. Co-treatment suppressed PEDV N RNA levels, suggesting that Fan also affected PEDV infection at the early stage (Figure 2B). Furthermore, the addition of Fan resulted in a significant reduction in PEDV N protein and mRNA levels at 12, 24, and 36 h post-infection (hpi; Figures 2C–E).

a 1.91-log decrease in progeny virus levels (Figure 3C). These results showed that Fan inhibited PEDV attachment to IPECJ2 cells. In the internalization assay, Fan at 20 µM reduced the PEDV N mRNA levels by 97.63% (Figure 3D), and 20 µM Fan reduced PEDV N protein levels by 97.78% (Figure 3E). PEDV titers decreased by 99.00% in the presence of 20 µM Fan (Figure 3F). To clarify the inhibitory effect of Fan in the later stage of PEDV infection, replication and release were studied. In the viral replication tests, the relative levels of viral RNA and protein treated with 20 µM Fan decreased at 9 and 12 hpi (Figures 3G, H), which suggested that PEDV replication is prevented by Fan treatment. Further experiments showed that Fan treatment did not affect viral release from PEDV-infected cells (Figure 3I).

3.3. Fan inhibits PEDV by affecting viral attachment, internalization, and replication 3.4. Fan inhibits autophagic flux in IPEC-J2 cells

To further elucidate the inhibition process of Fan at the co-processing stage, binding and entry were performed. The viral attachment tests showed that Fan decreased the levels of PEDV N mRNA (Figure 3A) and protein significantly (Figure 3B), with inhibition rates of 33.77%−91.02%, according to the increasing Fan concentration. Meanwhile, Fan dose-dependently decreased the viral titers, and 20 µM Fan treatment produced

Previous research demonstrated that Fan increases LC3II expression (an autophagy marker) by autophagy inhibition (disrupting the fusion of autophagosome and lysosome and lysosome dysfunction) and induction (promoting the nuclear translocation of TFEB), providing insights into the complexity of agent-mediated autophagy (Tang et al., 2017). Autophagosome formation can be monitored by the conversion of LC3I to LC3II.

Frontiers in Microbiology 05 frontiersin.org Zhang et al. 10.3389/fmicb.2023.1164851 FIGURE 3

PEDV attachment, internalization, and replication are affected by Fan. (A–C) Fan inhibits PEDV by affecting viral attachment, as assessed using qRT-PCR, Western blotting, and TCID50 assays. (D–F) Fan inhibits PEDV by affecting viral internalization, as assessed using qRT-PCR analysis, Western blotting, and TCID50 analysis. (G, H) It inhibits PEDV by affecting viral replication as assessed using qRT-PCR analysis and Western blotting. (I) At 24 hpi, cellular supernatants and intact cells were obtained, and the PEDV N gene copy number was determined. *P < 0.05; **P < 0.01; ***P < 0.001; and ****P < 0.0001 indicate significant differences vs. the control group.

3.5. Inhibition of autophagy downregulates the replication of PEDV in IPEC-J2 cells

P62/SQSTM1 is a cargo protein receptor that is degraded upon the successful formation of autophagolysosomes (Pal et al., 2014). Therefore, P62 accumulation serves as a marker for autophagy flux inhibition. Our results showed that Fan increased the protein levels of LC3II and P62 in a concentration- and timedependent manner in IPEC-J2 cells (Figures 4A–F). Increased LC3II and P62 levels are regarded as indicative of defective autophagic flux. Then, we detected the effect of Fan on the early stage of autophagy by adding wortmannin (Figures 4G, H), which showed that wortmannin could not inhibit the Faninduced increase in LC3II. This indicated that the inhibition of autophagy flux was responsible for the Fan-induced accumulation of autophagosomes.

PEDV infection-induced autophagy positively affects viral replication (Sun et al., 2021; Park et al., 2022). Our results showed that LC3II levels were enhanced with increasing hours post-infection (Figure 5A). The LC3II to GAPDH ratio was significantly higher in PEDV-infected cells than in uninfected cells at 12 and 24 hpi (Figure 5B). To evaluate the effect of autophagy on PEDV infection, IPEC-J2 cells were treated with non-toxic autophagy inhibitors containing either 0.1 µM wortmannin (Supplementary Figure S1A), 20 µM chloroquine (Supplementary Figure S1B), or 0.2 µM bafilomycin

Fan inhibits autophagic flux. (A–C) Various concentrations of Fan were used to treat IPEC-J2 cells for 24 h. The cells were then harvested, and Western blotting was used to quantify the levels of autophagy markers LC3II and P62. (D–F) Fan at 10 µM was used to treat IPEC-J2 at different times, followed by Western blotting analysis of LC3II and P62. (G, H) IPEC-J2 cells were treated with 10 µM Fan, with or without 0.1 µM wortmannin for 24 h. The cells were then harvested, followed by Western blotting analysis of LC3II and P62. Wort, wortmannin. *P < 0.05; **P < 0.01; and ***P < 0.001 indicate significant differences vs. the control group.

decreased in the three groups (Figure 6). Thus, Fan inhibits PEDV infection by reducing autophagic flux and inhibiting the formation of autolysosomes.

A1 (Supplementary Figure S1C). Wortmannin, chloroquine, and bafilomycin A1 treatment decreased the protein and mRNA levels of the N gene in PEDV-infected but not mock-infected cells (Figures 5C, D). At 24 hpi, the PEDV titers in the autophagy inhibitor-treated cells were significantly lower (P < 0.05) compared with those in the mock-infected cells (Figure 5E). Thus, the autophagy inhibitors effectively inhibited PEDV infection.

4. Discussion The recent outbreak of COVID-19 has focused on the research of antiviral medications (Frediansyah et al., 2021; Ohashi et al., 2021; Wu et al., 2022). The enteropathogenic coronavirus PEDV causes a highly contagious enteric infection that results in significant lethality in neonatal piglets (Huang et al., 2013; Shi et al., 2017; Zhang et al., 2019). Therefore, therapeutic strategies to prevent and control PEDV infection are critical. Fan, a natural bisbenzylisoquinoline alkaloid extracted from Stephania tetrandra roots, has numerous pharmacological properties, e.g., anti-inflammatory effects (Choi et al., 2000; Hristova et al., 2003) and inhibition of cancer growth and proliferation (Li et al., 2017; Wang et al., 2017; Zhang et al., 2021;

3.6. Fan inhibits PEDV replication by inhibiting autophagic degradation Taken together, the results suggested that Fan’s inhibition of PEDV infection results from the inhibition of autophagy. Consequently, we treated PEDV-infected IPEC-J2 cells with Fan, chloroquine, and bafilomycin A1 and then detected LC3II, P62, and PEDV N protein levels. The results showed increased LC3II and p62 levels in the three drug-treatment groups compared with that in the untreated group. Meanwhile, PEDV N protein levels

Inhibition of autophagy downregulates the PEDV replication in IPEC-J2 Cells. (A, B) At various time points, IPEC-J2 cells were mock infected or infected with PEDV GD/HZ/2016 (MOI = 0.5), followed by Western blotting analysis of autophagy markers. (C–E) IPEC-J2 cells were treated with wortmannin (0.1 µM), chloroquine (20 µM), and bafilomycin A1 (0.2 µM) for 1 h and then infected with PEDV (MOI = 0.1). At 24 h hpi, PEDV N mRNA (C), protein (D), and the virus titers (E) were assessed using qRT-PCR analysis, Western blotting, and TCID50 analysis. Wort, wortmannin; CQ, chloroquine; Baf A1, bafilomycin A1; **P < 0.01, ****, P < 0.0001 indicate significant differences vs. the control group.

Chen et al., 2022). Although most studies have focused on its anticancer activity, its antiviral effect has begun to receive attention. Herein, we found that Fan is a potent natural inhibitor of PEDV infection. Fan dose-dependently restricted PEDV replication in IPEC-J2 cells, with an EC50 value of 0.67 µM (Figure 1E). Previous studies have reported the EC50 values of Fan against HIV-1 and HCoVs of 0.8–1.7 and 1.01 ± 0.07 µM, respectively (Wan et al., 2012; Kim et al., 2019), which suggests that the effective dose of Fan to inhibit different viruses varies. Fan pre-treatment, co-treatment, and post-infection treatment all exerted an anti-PEDV effect, with post-infection treatment showing the best inhibitory effect. The coronavirus life cycle comprises attachment, internalization, replication, and release, and our results showed that Fan could disrupt multiple steps of PEDV’s life cycle, thus inhibiting infection. Fan’s inhibitory effect was strongest in the replication stage. A previous study reported that Fan can interfere with the proteolytic processing of gp160 to target Env at the late stage of HIV-1 replication, thereby inhibiting viral propagation (Wan et al., 2012). In addition, it has been reported that some herbal medicines have an antiviral effect on PEDV infection. Li et al. (2020) reported that quercetin could significantly suppress PEDV infection in CCL-81 cells. The possible approach of quercetin for anti-PEDV seemed to inhibit the activity of PEDV 3C-like protease (Li et al., 2020). The other research demonstrated that the aqueous leaf extract of Moringa oleifera (MOE) inhibited PEDV replication rather than attachment and internalization. MOE can alleviate oxidative stress and suppress the expression of inflammatory cytokines, which

resulted in fewer apoptotic cells during PEDV infection (Cao et al., 2022). Fan could induce autophagy by activating the AMPK/mTOR/ULK1 signaling pathway in colorectal cancer cell lines (Xiang et al., 2021). Although Fan could increase LC3II levels and the GFP-LC3 puncta formation in non-small cell lung cancer, the use of the autophagy inhibitor bafilomycin A1 did not further increase the Fan-mediated LC3II levels (Tang et al., 2017). This suggested that Fan inhibits autophagic flux. Herein, Fan increased the levels of the autophagy factors LC3II and P62 in IPEC-J2 cells, while the early autophagy inhibitor wortmannin failed to inhibit the increase in Fan-induced LC3II. There has been limited research on the role of autophagy in PEDV replication (Guo et al., 2017; Lin et al., 2020). Given the association between PEDV replication and autophagy and the Fan-mediated regulation of autophagy, we speculate that Fan inhibits PEDV by affecting autophagy. Herein, we demonstrated that PEDV-infected IPEC-J2 cells showed increased conversion of LC3I to LC3II (Figures 5A, B). Accordingly, the replication of PEDV was inhibited by the treatment of IPEC-J2 cells with autophagy inhibitors (wortmannin, chloroquine, or bafilomycin A1). Furthermore, Fan inhibited the late stages of autophagy, resulting in the accumulation of autophagosomes, which has an important function in PEDV infection of IPEC-J2 cells. Similar to chloroquine, Fan inhibits PEDV infection by reducing autophagic degradation in IPEC-J2 cells. Moreover, Fan suppresses PEDV better than chloroquine. Previous research showed that Fan is a potential natural antiviral

Fan inhibits PEDV replication by inhibiting autophagic degradation. (A) IPEC-J2cells were treated with 10 µM fangchinoline, 20 µM chloroquine, and 0.2 µM bafilomycin A1 for 1 h. At 24 h after PEDV (MOI = 0.1) infection, cell lysates were collected for Western blotting as indicated. (B) LC3, (C) P62, and (D) N protein of PEDV were quantitated. CQ, chloroquine; Baf A1, bafilomycin A1. *P < 0.05, ***P < 0.001, and ****P < 0.0001 indicate significant differences vs. the control group.

agent to prevent and treat HCoV-OC43 infection (Kim et al., 2019), which is β-CoV. Therefore, Fan can inhibit α-CoV and β-CoV. Consequently, Fan might have utility as a broad-spectrum anti-coronavirus drug to treat human and animal coronaviruses. The present study demonstrated that Fan has antiviral activity against PEDV in IPEC-J2 cells via a mechanism involving autophagy regulation. Therefore, Fan might be a promising agent to prevent and treat infection by PEDV or other porcine enteric coronaviruses.

conceptualized this study. CZ, ZL, ML, JianfZ, and YL prepared the materials for the experiments. All authors contributed to the article and approved the submitted version.

📖 中文全文 Chinese Full Text

中文

# 翻译

**类型** 原创研究 **发表日期** 2023年7月7日 **DOI** 10.3389/fmicb.2023.1164851 **开放获取** **编辑**

Fateh Singh, 印度ICAR-高安全动物疾病国家研究所(ICAR-NIHSAD) **审稿人**

Gaopeng Hou, 美国圣路易斯华盛顿大学 Jung-Eun Park, 韩国忠南国立大学 Yun Chen, 中国海南大学 Haifei Wang, 中国扬州大学 **通讯作者**

Jianmin Zhang junfeng-v@163.com Yugu Li liyugu@scau.edu.cn †

这些作者对本研究做出了同等贡献,共享第一作者身份 **收稿日期** 2023年2月13日 **录用日期** 2023年6月19日 **发表日期** 2023年7月7日 **引用格式**

Zhang W, Shen H, Wang M, Fan X, Wang S, Wuri N, Zhang B, He H, Zhang C, Liu Z, Liao M, Zhang J, Li Y and Zhang J (2023) 粉防己碱通过抑制自噬流抑制猪流行性腹泻病毒在肠上皮细胞中的复制. Front. Microbiol. 14:1164851. doi: 10.3389/fmicb.2023.1164851 **版权声明**

© 2023 Zhang, Shen, Wang, Fan, Wang, Wuri, Zhang, He, Zhang, Liu, Liao, Zhang, Li and Zhang. 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、分发或复制时,须注明原作者和版权所有者,并按照本期刊引用的原始出版物进行引用,方被允许。任何不符合上述条款的使用、分发或复制均不被允许。

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# 粉防己碱通过抑制自噬流抑制猪流行性腹泻病毒在肠上皮细胞中的复制

Weixiao Zhang1,2†, Haiyan Shen2,3†, Menglu Wang1,2, Xuelei Fan1,2, Songqi Wang1,2, Nile Wuri2,4, Bin Zhang2,4, Haiyan He2,4, Chunhong Zhang2,3, Zhicheng Liu2,3, Ming Liao2,3, Jianfeng Zhang2,3, Yugu Li1* and Jianmin Zhang1*

1 华南农业大学兽医学院,中国广州;2 广东省畜禽疫病防控重点实验室,农业农村部兽药与诊断技术科学观测实验站,广东省农业科学院动物卫生研究所,中国广州;3 广东省实验室茂名分中心(岭南现代农业科学与技术),中国广州;4 内蒙古农业大学兽医学院,中国呼和浩特

**摘要**

冠状病毒严重威胁动物和人类健康。肠道致病性冠状病毒——猪流行性腹泻病毒(PEDV)具有高度传染性,可引起猪流行性腹泻(PED),给全球养猪业造成巨大经济损失。目前仔猪对PEDV新型变异株缺乏有效保护,因此迫切需要开发新的抗病毒措施来控制PED。本研究探讨了粉防己碱(Fan)的抗PEDV效应及其潜在机制。Fan在感染后24小时呈剂量依赖性抑制PEDV感染(EC50值=0.67 µM)。研究发现,Fan主要影响PEDV的复制阶段,同时也能抑制病毒生命周期的吸附和内化阶段。机制上,Fan通过调控自噬相关蛋白的表达并改变PEDV病毒颗粒,阻断PEDV感染细胞中的自噬流。综上所述,Fan通过阻断细胞自噬流来抑制PEDV感染。本研究结果将为开发预防和治疗PEDV感染的新策略提供参考。

**关键词**

猪流行性腹泻病毒,粉防己碱,抗病毒剂,自噬,复制

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## 1. 引言

肠道致病性冠状病毒——猪流行性腹泻病毒(PEDV)可引起猪流行性腹泻(PED)(Belouzard et al., 2012)。PED通过绒毛萎缩和脱落损伤各日龄猪的肠道。然而,感染PEDV的新生仔猪会出现急性水样腹泻和呕吐,死亡率接近100%(Alvarez et al., 2015)。PED于1978年首次被报道,但2010年中国出现了新的PEDV变异株。此后,PED在全球范围内传播,给养猪业造成了巨大损失(Stevenson et al., 2013; Lowe et al., 2014)。尽管已有商品化PEDV疫苗,但PEDV仍持续存在,新出现的变异株使PEDV防控更加困难(Pensaert and de Bouck, 1978; Sun et al., 2016; Yu et al., 2018)。

因此,迫切需要开发预防猪PEDV感染的药物。数千年来,草药一直被用于治疗病毒性疾病,是潜在的抗冠状病毒治疗药物来源(Wen et al., 2011; Ling, 2020; Yang et al., 2020)。粉防己碱(Fan)是一种传统中药单体,是中药粉防己(Stephaniae Tetrandrine S. Moore)干燥根中的主要生物碱成分之一(Zhu, W. et al., 2019)。Fan可调节自噬和凋亡、抑制炎症小体活化并抑制谷氨酸释放(Lin et al., 2009; Fan et al., 2017; Tang et al., 2017; Liu et al., 2019)。迄今为止,大多数研究集中在其抗肿瘤活性方面。最近研究表明,Fan可通过未知机制抑制HCoV-OC43感染(Kim et al., 2019)。

自噬参与多种病原体感染过程。研究表明,某些病毒可诱导宿主细胞自噬,从而促进病毒增殖(Xu et al., 2018; Khabir et al., 2020)。研究发现PEDV可诱导活性氧(ROS)依赖性内质网(ER)应激介导的自噬,从而促进病毒复制(Sun et al., 2021)。此外,PEDV诱导的自噬有利于其复制(Guo et al., 2017)。PEDV非结构蛋白6(nsp6)诱导的自噬主要通过PI3K/Akt/mTOR信号通路促进PEDV复制(Lin et al., 2020)。因此,鉴于PEDV与自噬之间的关联,寻找通过破坏自噬来抑制PEDV的药物具有重要意义。

本研究旨在评估Fan在IPEC-J2细胞(猪肠上皮细胞)中对PEDV的抗病毒活性,并通过抑制自噬流阐明Fan的抗病毒机制。本研究揭示了Fan在治疗PEDV感染中的潜在应用价值。Fan可作为抗病毒药物的基础,用于遏制PED暴发。

将接种于96孔板中的IPEC-J2细胞分别用0、2.5、5、10、20、40和80 µM的Fan处理48 h。随后使用细胞计数试剂盒-8(CCK-8)(Abcam,中国)按照供应商提供的操作指南检测细胞活力。各浓度的细胞活力百分比按以下公式计算:

$$\frac{OD_t}{OD_c} \times 100\%$$

其中,$OD_t$和$OD_c$分别为处理组和对照组细胞的吸光度值。通过非线性回归分析对数据生成的剂量-反应曲线计算50%细胞毒性浓度(CC50)。

## 2.3 加药时间点实验

以感染复数(MOI)= 0.1的PEDV毒株GD/HZ/2016感染IPEC-J2细胞,孵育1 h。在细胞感染PEDV(MOI = 0.1)的1 h期间的不同时间点加入含药培养基(20 µM Fan)。预处理组(Pre)在病毒感染前1 h加入Fan;共处理组(Co)在病毒孵育开始时加入Fan;后处理组(Po)在病毒孵育结束后加入Fan;全程处理组(Full)在整个感染期间均加入Fan;病毒对照组(VC)不加入Fan。感染后,将接种物更换为新鲜培养基,细胞继续孵育23 h。随后收集各组上清液和细胞。采用实时荧光定量逆转录PCR(qRT-PCR)检测病毒RNA水平,采用50%组织培养感染剂量(TCID50)法检测病毒滴度(Wang et al., 2016; Lai et al., 2020)。

## 2. 材料与方法

### 2.1 病毒、细胞和试剂

非洲绿猴肾细胞(Vero)在含有10%胎牛血清(FBS;Gibco,美国大岛)和1%青霉素-链霉素(NCM Biotech,美国纽波特)的Dulbecco改良Eagle培养基(DMEM;Invitrogen,美国卡尔斯巴德)中培养。IPEC-J2细胞(由广东省农业科学院动物科学研究所Li Wang博士提供)在含有10% FBS和1%青霉素-链霉素的DMEM/F-12培养基(Gibco;Invitrogen,美国卡尔斯巴德)中培养。两种细胞系均在37°C、含5% CO2的湿润气氛中培养。PEDV毒株GD/HZ/2016(GenBank登录号:OP191700.1)在本实验室(广东省农业科学院动物卫生研究所,中国广州)分离、鉴定和保存。GD/HZ/2016毒株在含胰蛋白酶的DMEM中于Vero细胞中增殖。粉防己碱(HY-N1372A)、渥曼青霉素(SL-2052)、氯喹(HY-17589A)和巴弗洛霉素A1(HY-100558)均购自MedChemExpress(美国蒙茅斯章克申)。

### 2.4 病毒吸附、内化和复制实验

#### 2.4.1 吸附实验

将细胞在4°C冷却1 h,用不同浓度的Fan(0、2.5、5、10和20 µM)处理,然后在4°C下与不同浓度的Fan共同感染PEDV GD/HZ/2016(MOI = 0.5)1 h。在此期间,病毒将吸附于细胞膜上但不会穿透细胞。用冰冷的磷酸盐缓冲液(PBS)洗涤细胞(Zhu, Z. et al., 2019),然后在37°C培养基中培养24 h。为评估Fan对病毒吸附的影响,对上清液进行TCID50分析,收集细胞样品进行Western blotting和qRT-PCR分析。

#### 2.4.2 内化实验

以0.5 MOI的PEDV GD/HZ/2016在4°C下感染IPEC-J2细胞1 h。然后用冰冷的PBS洗涤细胞三次。向各样品中加入Fan(0、2.5、5、10和20 µM),在37°C下孵育1 h。用PBS洗涤细胞三次,加入新鲜培养基,然后孵育细胞24 h。随后分别使用qRT-PCR、Western blotting和TCID50法测定细胞内病毒RNA、蛋白水平和上清液病毒滴度。

#### 2.4.3 复制实验

以0.1 MOI的PEDV GD/HZ/2016在37°C下感染IPEC-J2细胞1 h,然后用PBS洗涤三次以去除游离病毒颗粒。随后向细胞中加入含20 µM Fan的新鲜培养基。在感染后9 h和12 h,分别使用qRT-PCR和Western blotting检测PEDV N基因的RNA和蛋白水平。

#### 2.4.4 释放实验

以0.1 MOI的PEDV GD/HZ/2016在37°C下感染IPEC-J2细胞1 h,然后用PBS洗涤三次以去除游离病毒颗粒。随后将细胞在含不同浓度Fan的新鲜培养基中于37°C孵育24 h。然后对收集的细胞或细胞上清液进行qRT-PCR检测,以确定病毒RNA拷贝数。

### 2.5 使用抑制剂调控细胞自噬

将IPEC-J2细胞分别用渥曼青霉素(0.1 µM)、氯喹(20 µM)或巴弗洛霉素A1(0.2 µM,均直接加入培养基)处理1 h,然后在37°C下感染PEDV(MOI = 0.1)1 h。然后用PBS洗涤三次以去除未结合的病毒,随后在含2% FBS的DMEM/F12培养基中孵育,培养基中含有不同浓度的渥曼青霉素、氯喹或巴弗洛霉素A1。对照组仅感染PEDV。收集细胞进行qRT-PCR和Western blotting检测,以确定PEDV N mRNA和蛋白水平的变化。使用TCID50法测定细胞上清液中的病毒滴度。

### 2.6 qRT-PCR

使用TaKaRa MiniBEST通用RNA提取试剂盒(TaKaRa,中国)从不同处理的IPEC-J2细胞中提取总RNA。随后使用HiScript II One Step qRT-PCR SYBR Green试剂盒(Vazyme,中国)进行qRT-PCR,引物序列如下:PEDV-N-F: GCAAAGACTGAACCCACTAAT,PEDV-N-R: GCCTCTGTTGTTACTTGGAG,以及β-actin-F: GGACTTCGAGCAGGAGATGG,β-actin-R: AGGAAGGAGGGCTGGAAGAG。

### 2.7 Western blotting实验

实验步骤参照先前研究(Wang et al., 2020)。简言之,使用150 µl裂解液(ThermoFisher Scientific,中国)裂解细胞。将所得蛋白分离后转移至聚偏二氟乙烯(PVDF)膜上。将膜在5%脱脂牛奶中封闭1 h,然后与以下一抗在室温下孵育2 h:抗PEDV N蛋白抗体(Medgene Labs,美国)、抗3-磷酸甘油醛脱氢酶(GAPDH)抗体(ABclonal,中国)、抗微管相关蛋白1轻链3α亚型II(LC3II)抗体(NOVUS,美国)和抗sequestosome 1(SQSTM1/P62)抗体(ABclonal,中国),随后用PBST洗涤三次。然后将膜与辣根过氧化物酶(HRP)标记的山羊抗小鼠和抗兔IgG(H+L)二抗(Bioworld,中国)孵育。使用ECL试剂盒(Millipore,中国)显色观察免疫反应蛋白条带。

### 2.8 免疫荧光实验

使用4%多聚甲醛(Beyotime,中国)固定细胞,用含0.1% Triton X-100的PBS透化。然后用1%牛血清白蛋白(BBI Life Sciences,中国)封闭细胞1 h。将小鼠抗PEDV N IgG抗体与细胞在4°C下孵育过夜,然后在37°C下与Alexa FluorTM 594山羊抗小鼠IgG(Invitrogen,中国)孵育1 h。随后用PBS洗涤细胞三次,再用4',6-二脒基-2-苯基吲哚(DAPI,Beyotime)孵育5 min。然后使用微分荧光显微镜观察细胞。

### 2.9 病毒滴定

将生长至70%-80%汇合度的Vero细胞接种于96孔板中,用10倍系列稀释的PEDV感染(n = 4个重复),在37°C下孵育72 h,随后进行免疫荧光实验(IFA)评估。使用Reed-Muench法测定病毒滴度(以每毫升TCID50表示)。

### 2.10 EC50的计算

在剂量依赖性实验中,将PEDV毒株GD/HZ/2016接种于12孔细胞培养板中的IPEC-J2细胞,然后用0至20 µM递增浓度的Fan处理。通过qRT-PCR测定PEDV N mRNA水平,抑制率按以下公式计算:

$$1 - \frac{mRNA(Fan)}{mRNA(mock)} \times 100\%$$

利用抑制率和Fan浓度建立剂量-反应曲线,计算EC50(半数最大效应浓度)。

### 2.11 统计学分析

数据以平均值±标准差(SD)表示。使用GraphPad Prism 8.0进行图形构建和统计分析,使用Image J对免疫反应蛋白条带进行定量。采用单因素方差分析(ANOVA)进行统计学分析。P值<0.05表示差异具有统计学意义。

## 3. 结果

### 3.1 Fan保护细胞抵抗PEDV感染

首先使用CCK-8法评估Fan对IPEC-J2细胞的细胞毒性,结果显示Fan在20 µM浓度下对IPEC-J2细胞无细胞毒性(CC50 = 37.49 µM;图1A)。根据Fan的无细胞毒性浓度范围,我们评估了其对PEDV感染的抑制作用。结果显示,随着Fan浓度增加,PEDV N蛋白水平显著下降(图1B)。qRT-PCR分析显示,Fan处理后PEDV N mRNA水平下调(图1C),EC50值为0.67 µM(图1E)。此外,20 µM Fan处理使病毒滴度从10^7显著降低至10^0.75 TCID50/ml(图1D)。IFA结果显示,Fan以浓度依赖性方式抑制PEDV对IPEC-J2细胞的感染(图1F)。

### 3.2 Fan在感染早期和晚期均抑制PEDV

为确定Fan主要影响PEDV感染的哪个阶段,进行了加药时间点分析(图2A)。Fan在整个病毒生命周期中均降低了PEDV N mRNA水平。其在后处理阶段的抑制效果最强(约98.86%抑制率),表明Fan主要在感染晚期抑制PEDV感染。共处理也抑制了PEDV N RNA水平,表明Fan在感染早期也影响PEDV感染(图2B)。此外,在感染后12 h、24 h和36 h(hpi),加入Fan均导致PEDV N蛋白和mRNA水平显著降低(图2C-E)。

### 3.3 Fan通过影响病毒吸附、内化和复制来抑制PEDV

为进一步阐明Fan在共处理阶段的抑制过程,进行了吸附和内化实验。病毒吸附实验显示,Fan显著降低了PEDV N mRNA(图3A)和蛋白水平(图3B),抑制率随Fan浓度增加而达到33.77%-91.02%。同时,Fan呈剂量依赖性降低病毒滴度,20 µM Fan处理使子代病毒水平降低1.91个对数级(图3C)。这些结果表明Fan抑制了PEDV对IPEC-J2细胞的吸附。在内化实验中,20 µM Fan使PEDV N mRNA水平降低97.63%(图3D),20 µM Fan使PEDV N蛋白水平降低97.78%(图3E)。在20 µM Fan存在下,PEDV滴度降低99.00%(图3F)。为明确Fan在PEDV感染晚期的抑制作用,研究了病毒复制和释放。在病毒复制实验中,经20 µM Fan处理后,病毒RNA和蛋白的相对水平在9 hpi和12 hpi均降低(图3G、H),表明Fan处理可阻止PEDV复制。进一步实验显示,Fan处理不影响PEDV感染细胞的病毒释放(图3I)。

### 3.4 Fan抑制IPEC-J2细胞中的自噬流

先前研究表明,Fan通过自噬抑制(破坏自噬体与溶酶体的融合及溶酶体功能障碍)和自噬诱导(促进TFEB的核转位)增加LC3II(一种自噬标志物)的表达,这为药物介导的自噬复杂性提供了深入见解(Tang et al., 2017)。可通过LC3I向LC3II的转化来监测自噬体形成。P62/SQSTM1是一种货物蛋白受体,在自噬溶酶体成功形成后被降解(Pal et al., 2014)。因此,P62的积累是自噬流抑制的标志。我们的结果显示,Fan以浓度和时间依赖性方式增加了IPEC-J2细胞中LC3II和P62的蛋白水平(图4A-F)。LC3II和P62水平升高被认为是自噬流缺陷的指示。随后,我们通过添加渥曼青霉素检测Fan对自噬早期阶段的影响(图4G、H),结果显示渥曼青霉素不能抑制Fan诱导的LC3II增加。这表明自噬流抑制是Fan诱导自噬体积累的原因。

### 3.5 抑制自噬下调PEDV在IPEC-J2细胞中的复制

PEDV感染诱导的自噬对病毒复制有正向影响(Sun et al., 2021; Park et al., 2022)。我们的结果显示,LC3II水平随感染时间延长而增强(图5A)。在12 hpi和24 hpi,PEDV感染细胞中LC3II与GAPDH的比值显著高于未感染细胞(图5B)。为评估自噬对PEDV感染的影响,用无毒浓度的自噬抑制剂处理IPEC-J2细胞,包括0.1 µM渥曼青霉素(补充图S1A)、20 µM氯喹(补充图S1B)或0.2 µM巴弗洛霉素A1(补充图S1C)。渥曼青霉素、氯喹和巴弗洛霉素A1处理降低了PEDV感染细胞(而非模拟感染细胞)中N基因的蛋白和mRNA水平(图5C、D)。在24 hpi时,经自噬抑制剂处理的细胞中PEDV滴度显著低于模拟感染细胞(P < 0.05)(图5E)。因此,自噬抑制剂有效抑制了PEDV感染。

### 3.6 Fan通过抑制自噬降解来抑制PEDV复制

综合上述结果,Fan对PEDV感染的抑制作用源于对自噬的抑制。因此,我们用Fan、氯喹和巴弗洛霉素A1处理PEDV感染的IPEC-J2细胞,然后检测LC3II、P62和PEDV N蛋白水平。结果显示,与未处理组相比,三种药物处理组的LC3II和P62水平均升高。同时,PEDV N蛋白水平在三组中均降低(图6)。因此,Fan通过降低自噬流和抑制自噬溶酶体形成来抑制PEDV感染。

## 4. 讨论

近期COVID-19的暴发推动了抗病毒药物的研究(Frediansyah et al., 2021; Ohashi et al., 2021; Wu et al., 2022)。肠道致病性冠状病毒PEDV可引起高度传染性肠道感染,导致新生仔猪严重致死(Huang et al., 2013; Shi et al., 2017; Zhang et al., 2019)。因此,预防和控制PEDV感染的治疗策略至关重要。

Fan是一种从粉防己根中提取的天然双苄基异喹啉类生物碱,具有多种药理特性,如抗炎作用(Choi et al., 2000; Hristova et al., 2003)以及抑制肿瘤生长和增殖(Li et al., 2017; Wang et al., 2017; Zhang et al., 2021; Chen et al., 2022)。尽管大多数研究集中在其抗肿瘤活性方面,但其抗病毒作用已开始受到关注。本研究发现Fan是PEDV感染的强效天然抑制剂。Fan以剂量依赖性方式抑制PEDV在IPEC-J2细胞中的复制,EC50值为0.67 µM(图1E)。先前研究报道Fan对HIV-1和HCoVs的EC50值分别为0.8-1.7 µM和1.01 ± 0.07 µM(Wan et al., 2012; Kim et al., 2019),这表明Fan抑制不同病毒的有效剂量存在差异。Fan的预处理、共处理和感染后处理均表现出抗PEDV效应,其中感染后处理的抑制效果最佳。

冠状病毒的生命周期包括吸附、内化、复制和释放,我们的结果表明Fan可破坏PEDV生命周期的多个环节,从而抑制感染。Fan的抑制作用在复制阶段最强。先前研究报道Fan可通过干扰gp160的蛋白水解加工靶向HIV-1复制晚期的Env,从而抑制病毒传播(Wan et al., 2012)。此外,有报道显示某些草药对PEDV感染具有抗病毒作用。Li et al.(2020)报道槲皮素可在CCL-81细胞中显著抑制PEDV感染。槲皮素抗PEDV的可能途径是抑制PEDV 3C样蛋白酶的活性(Li et al., 2020)。另一项研究证明辣木(Moringa oleifera)叶水提物(MOE)可抑制PEDV复制,但不影响吸附和内化。MOE可减轻氧化应激并抑制炎症细胞因子的表达,从而减少PEDV感染期间的凋亡细胞(Cao et al., 2022)。

Fan可通过激活AMPK/mTOR/ULK1信号通路在结直肠癌细胞系中诱导自噬(Xiang et al., 2021)。尽管Fan可增加非小细胞肺癌中LC3II水平和GFP-LC3斑点形成,但使用自噬抑制剂巴弗洛霉素A1并未进一步增加Fan介导的LC3II水平(Tang et al., 2017)。这表明Fan抑制自噬流。本研究中,Fan增加了IPEC-J2细胞中自噬因子LC3II和P62的水平,而早期自噬抑制剂渥曼青霉素未能抑制Fan诱导的LC3II增加。关于自噬在PEDV复制中作用的研究有限(Guo et al., 2017; Lin et al., 2020)。鉴于PEDV复制与自噬之间的关联以及Fan介导的自噬调控,我们推测Fan通过影响自噬来抑制PEDV。本研究表明,PEDV感染的IPEC-J2细胞中LC3I向LC3II的转化增加(图5A、B)。相应地,用自噬抑制剂(渥曼青霉素、氯喹或巴弗洛霉素A1)处理IPEDV感染的IPEC-J2细胞可抑制PEDV复制。此外,Fan抑制自噬晚期阶段,导致自噬体积累,这在PEDV感染IPEC-J2细胞中起重要作用。与氯喹类似,Fan通过减少IPEC-J2细胞中的自噬降解来抑制PEDV感染。此外,Fan对PEDV的抑制效果优于氯喹。

先前研究表明Fan是一种潜在的天然抗病毒剂,可用于预防和治疗HCoV-OC43感染(Kim et al., 2019),HCoV-OC43属于β属冠状病毒。因此,Fan可抑制α属冠状病毒和β属冠状病毒。因此,Fan可能作为一种广谱抗冠状病毒药物,用于治疗人类和动物冠状病毒感染。

本研究证明Fan通过涉及自噬调控的机制在IPEC-J2细胞中对PEDV具有抗病毒活性。因此,Fan可能是一种有前景的预防和治疗PEDV或其他猪肠道冠状病毒感染的药物。

CZ、ZL、ML、JianfZ和YL为本研究准备了实验材料。所有作者均对本研究做出了贡献并批准了投稿版本。