HDAC-Specific Inhibitors Induce the Release of Porcine Epidemic Diarrhea Virus via the COPII-Coated Vesicles

✅ 全文

HDAC特异性抑制剂通过COPII包被囊泡诱导猪流行性腹泻病毒的释放

作者 Ying Yang; Huan Chen; Caisheng Zhang; Hyun-Jin Shin; Yingjuan Qian; Yong-Sam Jung 期刊 Viruses 发表日期 2023 卷/期/页码 Vol. 15(9) ISSN 1999-4915 DOI 10.3390/v15091874 类型 原创研究 (Original Research)

📄 英文摘要 English Abstract

EN

Porcine epidemic diarrhea virus (PEDV) is an alpha-coronavirus causing acute diarrhea and high mortality in neonatal suckling piglets, resulting in huge economic losses for the global swine industry. The replication, assembly and cell egression of PEDV, an enveloped RNA virus, are mediated via altered intracellular trafficking. The underlying mechanisms of PEDV secretion are poorly understood. In this study, we found that the histone deacetylase (HDAC)-specific inhibitors, trichostatin A (TSA) and sodium butyrate (NaB), facilitate the secretion of infectious PEDV particles without interfering with its assembly. We found that PEDV N protein and its replicative intermediate dsRNA colocalize with coat protein complex II (COPII)-coated vesicles. We also showed that the colocalization of PEDV and COPII is enhanced by the HDAC-specific inhibitors. In addition, ultrastructural analysis revealed that the HDAC-specific inhibitors promote COPII-coated vesicles carrying PEDV virions and the secretion of COPII-coated vesicles. Consistently, HDAC-specific inhibitors-induced PEDV particle secretion was abolished by Sec24B knockdown, implying that the HDAC-specific inhibitors-mediated COPII-coated vesicles are required for PEDV secretion. Taken together, our findings provide initial evidence suggesting that PEDV virions can assemble in the endoplasmic reticulum (ER) and bud off from the ER in the COPII-coated vesicles. HDAC-specific inhibitors promote PEDV release by hijacking the COPII-coated vesicles.

📄 中文摘要 Chinese Abstract

中文
猪流行性腹泻病毒(PEDV)是一种α冠状病毒,可引起新生仔猪急性腹泻和高死亡率,给全球养猪业造成巨大经济损失。PEDV作为一种有包膜RNA病毒,其复制、组装和细胞释放通过改变细胞内运输介导。PEDV分泌的机制尚不清楚。冠状病毒利用和修饰分泌途径的细胞内区室以促进其复制、组装和释放,劫持宿主细胞的运输机器。在真核细胞中,常规分泌运输途径的特征是新合成的脂质和蛋白质通过ER、ERGIC和高尔基体通过运输囊泡从ER到质膜的顺序运输。COPII包被的囊泡介导货物从ER到高尔基体的运输。HDAC抑制剂已被美国食品药品监督管理局批准作为癌症治疗药物,并作为其他疾病的候选疗法。此外,已发现HDAC抑制剂具有抗病毒作用。

📋 英文结构化总结 English Structured Summary

全文整理

EN

Background:

Porcine epidemic diarrhea virus (PEDV) is an alpha-coronavirus causing acute diarrhea and high mortality in neonatal suckling piglets, resulting in huge economic losses for the global swine industry. The replication, assembly and cell egression of PEDV, an enveloped RNA virus, are mediated via altered intracellular trafficking. The underlying mechanisms of PEDV secretion are poorly understood. Coronaviruses use and modify intracellular compartments of the secretory pathway to facilitate their replication, assembly and egression by hijacking the host cell’s transport machinery. In eukaryotic cells, the conventional secretory transport pathway is characterized by the sequential transport of newly synthesized lipids and proteins from the ER to the plasma membrane by transport vesicles via the ERGIC and the Golgi apparatus. COPII-coated vesicles mediate the transport of cargo from the ER to the Golgi apparatus. HDAC inhibitors are approved by the United States Food and Drug Administration as cancer therapeutics and are candidate therapies for other diseases. In addition, HDAC inhibitors have been found to exert antiviral effects.

Methods:

The study used the histone deacetylase (HDAC)-specific inhibitors trichostatin A (TSA) and sodium butyrate (NaB) to facilitate the secretion of infectious PEDV particles. The researchers found that PEDV N protein and its replicative intermediate dsRNA colocalize with coat protein complex II (COPII)-coated vesicles. The colocalization of PEDV and COPII was shown to be enhanced by the HDAC-specific inhibitors. Ultrastructural analysis revealed that the HDAC-specific inhibitors promote COPII-coated vesicles carrying PEDV virions and the secretion of COPII-coated vesicles. Additionally, HDAC-specific inhibitors-induced PEDV particle secretion was abolished by Sec24B knockdown.

Results:

The HDAC-specific inhibitors TSA and NaB facilitated the secretion of infectious PEDV particles without interfering with its assembly. PEDV N protein and dsRNA were found to colocalize with COPII-coated vesicles, and this colocalization was enhanced by the HDAC-specific inhibitors. Ultrastructural analysis demonstrated that the HDAC-specific inhibitors promote COPII-coated vesicles carrying PEDV virions and the secretion of COPII-coated vesicles. Consistent with these findings, Sec24B knockdown abolished the HDAC-specific inhibitors-induced PEDV particle secretion, implying that the HDAC-specific inhibitors-mediated COPII-coated vesicles are required for PEDV secretion.

Data Summary:

The study provided qualitative observations rather than quantitative statistics. Key observations include: HDAC-specific inhibitors TSA and NaB facilitate secretion of infectious PEDV particles; colocalization of PEDV N protein and dsRNA with COPII-coated vesicles is enhanced by these inhibitors; ultrastructural analysis shows COPII-coated vesicles carrying PEDV virions; and Sec24B knockdown abolishes induced PEDV particle secretion.

Conclusions:

The findings provide initial evidence suggesting that PEDV virions can assemble in the endoplasmic reticulum (ER) and bud off from the ER in the COPII-coated vesicles. HDAC-specific inhibitors promote PEDV release by hijacking the COPII-coated vesicles.

Practical Significance:

PEDV causes huge economic losses in the global swine industry. The study’s identification of HDAC-specific inhibitors as modulators of PEDV release via COPII-coated vesicles may inform future strategies to control PEDV outbreaks, leveraging the fact that HDAC inhibitors are already FDA-approved for other therapeutic applications.

📋 中文结构化总结 Chinese Structured Summary

中文

背景:

猪流行性腹泻病毒(PEDV)是一种α冠状病毒,可引起新生仔猪急性腹泻和高死亡率,给全球养猪业造成巨大经济损失。PEDV作为一种有包膜RNA病毒,其复制、组装和细胞释放通过改变细胞内运输介导。PEDV分泌的机制尚不清楚。冠状病毒利用和修饰分泌途径的细胞内区室以促进其复制、组装和释放,劫持宿主细胞的运输机器。在真核细胞中,常规分泌运输途径的特征是新合成的脂质和蛋白质通过ER、ERGIC和高尔基体通过运输囊泡从ER到质膜的顺序运输。COPII包被的囊泡介导货物从ER到高尔基体的运输。HDAC抑制剂已被美国食品药品监督管理局批准作为癌症治疗药物,并作为其他疾病的候选疗法。此外,已发现HDAC抑制剂具有抗病毒作用。

方法:

该研究使用组蛋白去乙酰化酶(HDAC)特异性抑制剂曲古抑菌素A(TSA)和丁酸钠(NaB)促进感染性PEDV颗粒的分泌。研究人员发现PEDV N蛋白及其复制中间体dsRNA与包被蛋白复合体II(COPII)包被的囊泡共定位。HDAC特异性抑制剂增强了PEDV与COPII的共定位。超微结构分析显示,HDAC特异性抑制剂促进携带PEDV病毒粒子的COPII包被囊泡和COPII包被囊泡的分泌。此外,Sec24B敲低消除了HDAC特异性抑制剂诱导的PEDV颗粒分泌。

结果:

HDAC特异性抑制剂TSA和NaB在不干扰其组装的情况下促进感染性PEDV颗粒的分泌。PEDV N蛋白和dsRNA与COPII包被囊泡共定位,并且这种共定位被HDAC特异性抑制剂增强。超微结构分析表明,HDAC特异性抑制剂促进携带PEDV病毒粒子的COPII包被囊泡和COPII包被囊泡的分泌。与这些发现一致,Sec24B敲低消除了HDAC特异性抑制剂诱导的PEDV颗粒分泌,这意味着HDAC特异性抑制剂介导的COPII包被囊泡是PEDV分泌所必需的。

数据总结:

该研究提供了定性观察而非定量统计数据。关键观察包括:HDAC特异性抑制剂TSA和NaB促进感染性PEDV颗粒的分泌;PEDV N蛋白和dsRNA与COPII包被囊泡的共定位被这些抑制剂增强;超微结构分析显示COPII包被囊泡携带PEDV病毒粒子;Sec24B敲低消除了诱导的PEDV颗粒分泌。

结论:

这些发现提供了初步证据,表明PEDV病毒粒子可以在内质网(ER)中组装,并从ER出芽进入COPII包被囊泡。HDAC特异性抑制剂通过劫持COPII包被囊泡促进PEDV释放。

实际意义:

PEDV给全球养猪业造成巨大经济损失。该研究确定HDAC特异性抑制剂作为通过COPII包被囊泡调节PEDV释放的调节因子,可能为未来控制PEDV爆发的策略提供信息,利用HDAC抑制剂已被FDA批准用于其他治疗应用的事实。

📖 英文全文 English Full Text

EN

viruses Article

HDAC-Specific Inhibitors Induce the Release of Porcine Epidemic Diarrhea Virus via the COPII-Coated Vesicles Ying Yang 1,2 , Huan Chen 1,2 , Caisheng Zhang 1,2 , Hyun-Jin Shin 3 , Yingjuan Qian 1,2,4, * and Yong-Sam Jung 1,2, * 1

2 3 4 *

Citation: Yang, Y.; Chen, H.; Zhang, C.; Shin, H.-J.; Qian, Y.; Jung, Y.-S. HDAC-Specific Inhibitors Induce the Release of Porcine Epidemic Diarrhea

One Health Laboratory, Jiangsu Foreign Expert Workstation, College of Veterinary Medicine, Nanjing Agricultural University, Nanjing 210095, China; 2018207012@njau.edu.cn (Y.Y.); chenhuan2019@njau.edu.cn (H.C.); 2020107034@stu.njau.edu.cn (C.Z.) MOE Joint International Research Laboratory of Animal Health and Food Safety, College of Veterinary Medicine, Nanjing Agricultural University, Nanjing 210095, China College of Veterinary Medicine, Chungnam National University, Daejeon 34134, Republic of Korea; shin0089@cnu.ac.kr Jiangsu Key Laboratory for High-Tech Research and Development of Veterinary Biopharmaceuticals, Jiangsu Agri-Animal Husbandry Vocational College, Veterinary Bio-Pharmaceutical, Taizhou 225300, China Correspondence: yqian@njau.edu.cn (Y.Q.); ysjung@njau.edu.cn (Y.-S.J.); Tel.: +86-25-8439-9102 (Y.Q. & Y.-S.J.)

Abstract: Porcine epidemic diarrhea virus (PEDV) is an alpha-coronavirus causing acute diarrhea and high mortality in neo-natal suckling piglets, resulting in huge economic losses for the global swine industry. The replication, assembly and cell egression of PEDV, an enveloped RNA virus, are mediated via altered intracellular trafficking. The underlying mechanisms of PEDV secretion are poorly understood. In this study, we found that the histone deacetylase (HDAC)-specific inhibitors, trichostatin A (TSA) and sodium butyrate (NaB), facilitate the secretion of infectious PEDV particles without interfering with its assembly. We found that PEDV N protein and its replicative intermediate dsRNA colocalize with coat protein complex II (COPII)-coated vesicles. We also showed that the colocalization of PEDV and COPII is enhanced by the HDAC-specific inhibitors. In addition, ultrastructural analysis revealed that the HDAC-specific inhibitors promote COPII-coated vesicles carrying PEDV virions and the secretion of COPII-coated vesicles. Consistently, HDAC-specific inhibitors-induced PEDV particle secretion was abolished by Sec24B knockdown, implying that the HDAC-specific inhibitors-mediated COPII-coated vesicles are required for PEDV secretion. Taken together, our findings provide initial evidence suggesting that PEDV virions can assemble in the endoplasmic reticulum (ER) and bud off from the ER in the COPII-coated vesicles. HDAC-specific inhibitors promote PEDV release by hijacking the COPII-coated vesicles.

Virus via the COPII-Coated Vesicles. Viruses 2023, 15, 1874. https:// doi.org/10.3390/v15091874

Keywords: HDAC-specific inhibitors; COPII-coated vesicles; porcine epidemic diarrhea virus; viral release Academic Editor: HuaJi Qiu Received: 1 July 2023 Revised: 31 August 2023 1. Introduction Accepted: 1 September 2023

Coronaviruses (CoVs), belonging to the order Nidovirales under the family Coronaviridae, are enveloped viruses with a positive-sense single-stranded RNA genome. The Coronaviridae family includes two subfamilies: Coronavirinae and Torovirinae. The Coronavirinae subfamily is further classified into four genera, the alpha-, beta-, gamma- and deltacoronaviruses, based on genotypic and serological characterizations [1–3]. The notorious severe acute respiratory syndrome coronavirus (SARS-CoV) and severe acute respiratory syndrome coronavirus 2 (SARS-CoV-2) represent beta-coronaviruses [4]. Porcine epidemic diarrhea virus (PEDV), an alpha-coronavirus in the family Coronaviridae, causes severe watery diarrhea, vomiting, dehydration, and high mortality in neonatal suckling piglets, resulting in huge economic losses in the global swine industry [5–7]. CoVs and others enveloped viruses, use and modify intracellular compartments of the secretory pathway to facilitate their replication, assembly and egression by hijacking the

Copyright: © 2023 by the authors. Licensee MDPI, Basel, Switzerland. This article is an open access article distributed under the terms and conditions of the Creative Commons Attribution (CC BY) license (https:// creativecommons.org/licenses/by/ 4.0/).

Viruses 2023, 15, 1874. https://doi.org/10.3390/v15091874 https://www.mdpi.com/journal/viruses Viruses 2023, 15, 1874 2 of 16

host cell´s transport machinery [8]. Viral particles assemble in the ER-Golgi intermediate compartment (ERGIC)/Golgi compartment, and is a general hallmark of CoVs [8,9]. Previous reports revealed that alpha-coronaviruses (TGEV, HCoV-NL36) and beta-coronaviruses (MHV) assemble in the ER during the late stages of virus infection. Other studies have indicated that PEDV particles assemble in both the ER and Golgi apparatus [8,10–13]. The egress pathway of PEDV is triggered by the interaction between the nucleocapsid (N) protein loaded with the newly synthesized genomic RNA and the structural spike (S), envelope (E), and membrane (M) proteins, budding into the lumen of the ER and the ERGIC. Virus particles reach the Golgi and trans-Golgi network (TGN) by vesicular transport for glycosylation and other post-translational modifications. Mature virions are subsequently released via fusion of smooth-walled vesicles with the plasma membrane similar to exocytosis [13,14]. However, the underlying mechanisms of PEDV secretion have yet to be fully understood. In eukaryotic cells, the conventional secretory transport pathway is characterized by the sequential transport of newly synthesized lipids and proteins from the ER to the plasma membrane by transport vesicles via the ERGIC and the Golgi apparatus [15,16]. Intracellular trafficking vesicles are mainly composed of COPI-, COPII-, and clathrincoated vesicles (CCVs) [17,18]. COPII-coated vesicles mediate the transport of cargo from the ER to the Golgi apparatus [19]. COPI-coated vesicles mediate cargo transport from the Golgi apparatus to the ER, or between Golgi cisternae [20,21]. CCVs mediate cargo transport from the TGN to the endosomes and the endocytosis of cargo at the plasma membrane [17,22]. The COPII-coated machinery is composed of five cytosolic proteins: Sar1, Sec23, Sec24, Sec13 and Sec31 [23]. The assembly of COPII-coated vesicle is initiated by the recruitment and activation of the small cytoplasmic GTPase Sar1 by the GTP exchange factor (GEF) Sec12. Sar1-GTP inserts into the ER membrane and recruits the Sec23/Sec24 heterodimer by binding to the Sec23. Sec23 acts as a GTPase activating protein (GAP) for Sar1 and Sec24 participates in cargo selection. Sar1 carrying a cargo-loaded Sec23/Sec24 heterodimer forms a so-called “pre-budding complex” and in turn recruits the Sec13/Sec31 heterotetramer onto the “pre-budding complex” to complete vesicle formation [16,23–27]. As the canonical secretory pathway for ER export, COPII-coated vesicles are frequently hijacked for viral genome replication and transport of viral particles. For example, poliovirus uses COPII-coated vesicles for the formation of replication complexes (RCs) [28,29]. Parvovirus particles [30], hepatitis B subviral envelope particles [31], hepatitis C virus (HCV) lipoviroparticles [32], rotavirus NSP4 [33], and Ebola and Marburg virus matrix protein VP40 utilize the COPII transport system for intracellular transport [34]. HDAC inhibitors are approved by the United States Food and Drug Administration (FDA) as cancer therapeutics and are candidate therapies for other diseases, including arthritis, cardiac disease, inflammatory diseases, and a few neurological disorders [35–37]. In addition, HDAC inhibitors have been found to exert antiviral effects. TSA and Suberoylanilide hydroxamic acid (SAHA) suppress respiratory syncytial virus (RSV) and HCV replication [38–40]. Romidepsin prevents the entry of SARS-CoV-2 [41]. In addition, class I-selective HDAC inhibitors enhance HIV latency reversal [42]. This study investigated the relationship between HDAC-specific inhibitors and COPIIcoated vesicles during PEDV infection. We showed that the HDAC-specific inhibitors, TSA and NaB, facilitate the secretion of infectious PEDV particles. We also found that PEDV particles utilize the COPII-coated vesicles for intracellular transport. In addition, transmission electron microscopy (TEM) and immunoelectron microscopy (IEM) revealed that secretion of COPII-coated vesicles carrying PEDV virions is promoted by HDACspecific inhibitors treatment. Finally, we also demonstrated that the knockdown of Sec23A or Sec24B suppresses HDAC-specific inhibitors-induced PEDV secretion. Taken together, this study establishes that HDAC-specific inhibitors-induced COPII-coated vesicles are essential for PEDV release.

2. Materials and Methods 2.1. Cell Culture African green monkey Cercopithecus aethiops kidney epithelial cells (Vero-E6 cells) were cultured in Dulbecco’s Modified Eagle Medium (DMEM) (Invitrogen, Carlsbad, CA, USA) supplemented with 8% fetal bovine serum (Pan-Biotech, Inc. Aidenbach, Germany) and 1% penicillin and streptomycin (MDBio, Qingdao, China) at 37 ◦ C in a 5% CO2 incubator. 2.2. Antibodies and Reagents Rabbit polyclonal anti-Sec21p was supplied by Agrisera (Vännäs, Sweden). Rabbit polyclonal anti-COPII was purchased from Invitrogen (Carlsbad, CA, USA). Rabbit polyclonal anti-clathrin was provided by Abcam (Cambridge, UK). Rabbit monoclonal anti-Sec24B (D7D6S) was obtained from Cell Signaling Technology, Inc. (Danvers, MA, USA). Rabbit polyclonal anti-Ac-Histone H3 (Lys 9/14) was ordered from Santa Cruz (Dallas, TX, USA). Rabbit polyclonal anti-actin (A2066) antibodies were purchased from Merck, Inc. (Darmstadt, Germany). Mouse polyclonal anti-PEDV-N and rabbit polyclonal anti-PEDV-N antibodies were previously generated in the lab [3]. The horseradish peroxidase (HRP)conjugated goat anti-rabbit IgG and HRP-conjugated goat anti-mouse IgG antibodies were ordered from MiliporeSigma (Merck Inc., Darmstadt, Germany). Alexa 488-conjugated goat anti-rabbit IgG (A-11001) and Alexa 555-conjugated goat anti-mouse IgG (A-21428) antibodies were supplied by Thermo Fisher Scientific, Inc. (Waltham, MA, USA). The 10 nm labeled goat anti-rabbit secondary antibody (G7402) was purchased from Sigma-Aldrich (St. Louis, MO, USA). TSA, and NaB were provided by Selleck (Houston, TX, USA). Glutaraldehyde (2.5%, pH 7.4) and paraformaldehyde (4%)-glutaraldehyde (0.5%) mixture, (pH 7.4) were purchased from Yuanye Bio-Technology Co., Ltd., (Shanghai, China). Ethanol was obtained from Sinaopharm Group Chemical Reagent Co. LTD (Shanghai, China). LR White Resin was supplied by HaideBio (Beijing, China). Enhanced chemiluminescence (ECL) reagent was purchased from Youqing Biology (Nanjing, China). 2.3. Viral Infection and Titer Determination PEDV (strain HLJBY) was cultured in Vero-E6 cells. The cells were infected with PEDV in DMEM without FBS and incubated at 37 ◦ C for 1 h. After incubation, the cells were washed with phosphate-buffered saline (PBS) and transferred to DMEM containing 2% FBS and 17.5 ng of trypsin per mL. The virus titer was determined using the plaque formation assay. Briefly, 6-well plates were seeded with 1 × 106 Vero-E6 cells/well the day before inoculation. The cells were washed with PBS, and 10-fold serial dilutions (102 to 107 ) of viruses were incubated with a confluent monolayer of Vero-E6 cells at 37 ◦ C for 1 h. After incubation, the cells were washed with PBS, followed by the addition of 2 mL overlay medium (2% low-melting-point agarose (Lonza Inc., Basel, Switzerland) in 2 × DMEM with 2% FBS and 17.5 ng of trypsin per mL). The plates were incubated at 37 ◦ C with 5% CO2 for 2 to 3 days. The cells were stained with 0.5% crystal violet. 2.4. Western Blotting Analysis Whole-cell extracts were prepared with 2 × SDS sample buffer (4% SDS, 0.1 M Tris HCI pH 6.8, 20% glycerol, 2% bromophenol blue, and 10% β-mercaptoethanol) and boiled for 10 min at 98 ◦ C. Next, the samples were subjected to sodium dodecyl sulfate-polyacrylamide gel electrophoresis (SDS-PAGE) and then transferred to a nitro-cellulose transfer membrane (Pall Corporation, Port Washington, NY, USA) using a Mighty Small Trans-fer Tank system (Hoefer, MA, USA). Then, the membranes were blocked with 3% non-fat milk in PBS with 0.5% Tween 20 (PBST) for 30 min at room temperature and then incubated with a specific primary antibody overnight at 4 ◦ C followed by incubation with secondary antibodies for 4 h at 4 ◦ C. The positive bands were visualized with the enhanced chemiluminescence (ECL) reagent, and imaged using a BioSpectrum Imaging System (UVP, Upland, CA, USA).

2.5. Knockdown of Sec23A/Sec24B Expression The siRNA oligonucleotides against Sec24B and a nontargeting control siRNA were purchased from Biotend, Inc. (Shanghai, China). For siRNA gene knockdown experiments, 3.6 × 105 Vero-E6 cells were seeded into 6-well plates/well for 18 h and transfected with 50 nM siRNA oligonucleotide using 7.5 µL Mirus following the manufacturer’s instructions (Madison, WI, USA). After 48 h of transfection, the cells were analyzed by immunoblotting to determine the knockdown efficiency. The Sec23A and Sec24B RNA interference (RNAi) target sequences were as follows: siSec23A-1, 50 -AAG GAA UCA GUU UCC ACC UAG UUA U-30 , siSec23A-2,50 -CCU ACA GCU UUG GUU GGA CUU AUU A-30 ; siSec24B-1,50 CGG UAU AUU CUG GAU UCC AAC AGU A-30 , siSec24B-2,50 -CCC GAU CUU AUG GAG AGC CUC AUA A-30 . 2.6. Immunofluorescence Microscopy The Vero-E6 cells were grown on coverslips and pretreated with or without TSA for 2 h, and then infected with PEDV for different durations. The cells on the coverslips were fixed and permeabilized with 4% formaldehyde and 0.1% Triton X-100 at 37 ◦ C for 30 min. After washing with glycine-PBS, the cells were blocked with 3% BSA in PBS at 37 ◦ C for 30 min. The coverslips were incubated with primary antibody (1:200) at 37 ◦ C for 1 h, followed by secondary antibody (1:500) at 37 ◦ C for 30 min. Unbound antibodies were removed by washing with PBST three times. The nuclei were stained with 40 ,6-diamidino2-phenylindole (DAPI) containing the anti-fade Dabco solution (Thermo Fisher Scientific, Waltham, MA, USA). Images of Figures 3 and 4A were obtained with a confocal microscopy (Nikon Eclipse Ti, A1, Tokyo, Japan) and Figure 6C,D and Figure S2 were obtained using a fluorescence microscopy (Nikon Eclipse Ti-U, Tokyo, Japan). 2.7. Transmission Electron Microscopy/Immunoelectron Microscopy Vero-E6 cells were pretreated with or without TSA and NaB for 2 h and then mock infected or infected with PEDV at a MOI = 0.1. After 12 or 24 h, cells were collected and centrifuged into a cell mass. First, the cell mass was fixed in cold glutaraldehyde (2.5%, pH 7.4, TEM) or cold paraformaldehyde (4%)-glutaraldehyde (0.5%) glutaraldehyde mixture, (pH 7.4, IEM) at 4 ◦ C overnight, followed by additional steps including cleaning, fixation, dehydration, resin penetration, embedding, solidification, polymerization, microtomy, and staining. The precipitation was washed three times in 0.1 M PB (pH 7.4), for 10 min each time. It was fixed with 1% osmic acid and then cleaned. The fixed cell mass was gradient dehydrated in different concentrations of ethanol. Resin penetration with different concentrations of embedding agent was performed. An embedding capsule was used for embedding, at 4 ◦ C. The solidification step was performed in a 55◦ C incubator for 48 h for TEM. For more than 48 h, polymerization was conducted at −20 ◦ C with low temperature UV polymerizer-UVCC2515 (Zhongjingkeyi Technology, Beijing, China) for IEM. Ultrathin sections (70–80 nm) from the resin blocks were obtained using a Leica UC7ultramicrotome (Wetzlar, Germany), and the tissues were fished out onto 150-meshes nickel grids (Zhongjingkeyi Technology, Beijing, China) with Formvar film; the sections were stored at 4 ◦ C. Immunolabelling was performed by incubating with an anti-COPII antibody overnight at 4 ◦ C, followed by incubation with 10 nm labeled goat anti-rabbit secondary antibody (20 min at room temperature; 1 h at 37 ◦ C; 30 min at room temperature) for IEM. For TEM/IEM, sample was stained with 2% uranyl acetate and lead citrate. Sections were examined with a Hitachi H-7650 (Hitachi, Tokyo, Japan) TEM at an accelerating voltage of 80 kV. 2.8. Cell Viability Analysis The cytotoxicity of HDAC-specific inhibitors was measured via a Cell Counting Kit8 (CCK-8) assay, following the manufacturer’s instructions (APExBIO Technology, Inc., Houston, TX, USA). In brief, Vero-E6 cells were seeded in the 96-well plate and cultured for 24 h and then treated with an increased dose of HDAC inhibitors for 12 or 24 h, followed

by incubation with CCK-8 reagent (10 µL/well) at 37 ◦ C for 4 h. Finally, the absorbance at 450 nm was measured in an enzyme-linked immunosorbent assay reader. 2.9. Statistical Analysis The results shown are representative of three replicate experiments. All statistical tests were conducted using GraphPad Prism 7.0 software (San Diego, CA, USA) and are presented as means plus or minus standard deviation (SDs). Statistical significance was determined using the Student’s t test. p values of <0.05 were considered statistically significant. 3. Results 3.1. HDAC-Specific Inhibitors Facilitate PEDV Particle Secretion HDAC inhibitors, such as TSA and SAHA, suppress HCV and RSV replication [38–40], whereas romidepsin inhibits the entry of SARS-CoV-2 [41]. This finding prompted us to investigate whether HDAC inhibitors regulate PEDV infection. To verify this possibility, Vero-E6 cells were pretreated with or without TSA and NaB, inhibitors of class I and II HDACs [43,44], and then infected with PEDV. The culture medium and the infected cells were harvested separately. To test the cytotoxicity of the HDAC-specific inhibitors we performed CCK-8 assay. We found that the HDAC-specific inhibitors at concentrations used in this study did not affect the cell viability (Figure 1A,B). To determine the functionality of HDAC-specific inhibitors, the infected cell lysates were analyzed via Western blotting analysis of acetylated histone H3. The protein level of acetylated histone H3 was increased by the HDAC-specific inhibitors treatment (Figure 1C,F). The infected cell lysates and the culture medium were subjected to Western blotting to analyze the intracellular and extracellular PEDV N protein levels. We found that the HDAC-specific inhibitors decreased the intracellular PEDV-N protein levels but increased the extracellular PEDV-N protein levels (Figure 1C,F and Figure S1). Cells treated with TSA secreted about 2.0-fold higher levels of infectious virus particles in the supernatant than the DMSO-treated cells (Figure 1D,E). Cells treated with NaB secreted infectious virus particles in the supernatant about 2.3-fold higher than the control cells (Figure 1G,H). These data suggested that the HDAC-specific inhibitors facilitate the secretion of PEDV virus particles into the extracellular medium. To further analyze the effect of HDAC-specific inhibitors on PEDV infection, Vero-E6 cells were pretreated with or without TSA and NaB and then infected with PEDV. The intracellular and extracellular virus titers were determined by plaque formation assay (PFU). PFU results showed that the HDAC-specific inhibitors treatment decreased the intracellular virus titer and increased the extracellular virus titer (Figure 2A,B,D,E). We used the ratio of virus titers in extracellular and intracellular compartments to evaluate virus release. The results showed that the TSA treatment resulted in an approximately 3.3-fold increase in the release of infectious virus particles (Figure 2C) compared with the approximately 2.7-fold increased by NaB treatment (Figure 2F). However, the total virus titer of HDAC-specific inhibitors-treated cells did not change significantly compared with the control (Figure 2G,H). These data indicated that the HDAC-specific inhibitors promote PEDV release without affecting its assembly.

Figure 1. HDAC-specific promote the promote secretion PEDV of virus particles into the Figure 1. inhibitors HDAC-specific inhibitors theofsecretion PEDV virus particles intoextracelthe extracellulular compartment. (A,B) Determination of the cell viability following treatment with TSA and NaB lar compartment. (A,B) Determination of the cell viability following treatment with TSA and NaB via via CCK-8 test. Vero-E6 cellsVero-E6 were pretreated with or without TSA (40 and and NaBNaB (2 mM) forfor 2 h, CCK-8 test. cells were pretreated with or without TSAng/mL) (40 ng/mL) (2 mM) 2 h, and then mock-infected or infected HLJBY (MOI =(MOI 0.1).=After HLJBY adsorption forfor1 1h.h. The and then mock-infected orwith infected with HLJBY 0.1). After HLJBY adsorption The cells were further cultured fresh medium in theinpresence of TSA and 12or or2424h.h. The cells were furtherin cultured in fresh medium the presence of TSA andNaB NaB at at 12 The infected cellwere lysates were prepared, and AC-H3, intracellular N, actin and actin were detected Western-blot infected cell lysates prepared, and AC-H3, intracellular N, and were detected byby Western(C,F). medium The culture medium wasinto divided twoone parts; onewas partanalyzed was analyzed by Western blotting blot (C,F). The culture was divided twointo parts; part by Western blotof extracellular N (C,F), and the other was titrated by plaque formation assay to measure the ting of extracellular N (C,F), and the other part waspart titrated by plaque formation assay to measure 5 ), 24 h 5),10 extracellular titers (D,G).show Graphs show changes in titers virus titers (E,H); h (× 24 the extracellular PEDV virus PEDV titers virus (D,G). Graphs changes in virus (E,H); 12 h12(×10 6 ). Student’s t test was used for statistical analysis. **, p < 0.01; ***, p < 0.001. The error bars was used for statistical analysis. **, p < 0.01; ***, p < 0.001. The error bars h (×106). Student’s(×t10test standard from three independent experiments. In; intracellular, Ex; extracellular. indicate standardindicate deviation from deviation three independent experiments. In; intracellular, Ex; extracellular.

To further analyze the effect of HDAC-specific inhibitors on PEDV infection, VeroE6 cells were pretreated with or without TSA and NaB and then infected with PEDV. The intracellular and extracellular virus titers were determined by plaque formation assay (PFU). PFU results showed that the HDAC-specific inhibitors treatment decreased the intracellular virus titer and increased the extracellular virus titer (Figure 2A,B,D,E). We used the ratio of virus titers in extracellular and intracellular compartments to evaluate virus

HDAC-specific inhibitors-treated cells did not change significantly compared with the control (Figure 2G,H). These data indicated that the HDAC-specific inhibitors promote PEDV release without affecting its assembly.

7 of 16

Figure 2. HDAC-specific inhibitors facilitatefacilitate the secretion of infectious particles. Vero-E6 cells Vero-E6 cells Figure 2. HDAC-specific inhibitors the secretion of PEDV infectious PEDV particles. were pretreated with or without TSA (40 ng/mL) and NaB (2 mM) for 2 h, and then mock-infected were pretreated with or without TSA (40 ng/mL) and NaB (2 mM) for 2 h, and then mock-infected or or infected with HLJBY (MOI = 0.1). After HLJBY adsorption for 1 h, the cells were further cultured infected withinHLJBY (MOI of = 0.1). After HLJBY adsorption for 1 h,medium the cellswas were further in fresh medium the presence TSA and NaB at 12 or 24 h. The culture first col- cultured in lected, and the infected cells were washed thrice with phosphate-buffered saline (PBS) before addfresh medium in the presence of TSA and NaB at 12 or 24 h. The culture medium was first collected, ing and freshthe medium, and then lysed via three freeze/thaw cycles to obtain the saline intracellular infected cells were washed thrice with phosphate-buffered (PBS) PEDV. before adding fresh (A,D): The virus titers (intracellular and extracellular) were detected by plaque formation assay. medium, and then lysed via three freeze/thaw cycles to obtain the intracellular PEDV. (A,D): The (B,E): Graphs show changes in virus titers (intracellular and extracellular); 12 h (×105), 24 h (×106). virus titers (intracellular and extracellular) were detected by plaque formation assay. (C,F): Graphs how PEDV release (ratio of extracellular to intracellular virus titers). (G,H): Graphs (B,E): Graphs 6 ). (C,F): Graphs show changes in total virus titers titer. Student’s t test and was extracellular); used for statistical show changes in virus (intracellular 12 hanalysis. (×105 ),The 24 herror (×10bars indicate standard deviation from three independent experiments. ns, p > 0.05; *, p < 0.05; ***, p

in total virus titer. Student’s t test was used for statistical analysis. The error bars indicate standard deviation from three independent experiments. ns, p > 0.05; *, p < 0.05; ***, p < 0.001.

3.2. Colocalization of PEDV N Proteins and Its Replication Complex with COPII-Coated Vesicles It has been reported that PEDV utilizes smooth-walled vesicles to egress [14]. Previous studies have shown that intracellular trafficking vesicles in eukaryotic cells are mainly composed of COPI, COPII and CCVs [17,18]. To determine the vesicular transport involved in PEDV transport, Vero-E6 cells were infected with PEDV. At different time points, VeroE6 cells were stained with anti-Sec21p (γ subunit of COPI), anti-COPII and anti-clathrin antibodies to detect transport vesicles. The subcellular localization of PEDV N protein and trafficking vesicle markers was examined using a confocal microscopy. The confocal microscopic images showed that only COPII colocalized with PEDV N protein and the

It has been reported that PEDV utilizes smooth-walled vesicles to egress [14]. Previous studies have shown that intracellular trafficking vesicles in eukaryotic cells are mainly composed of COPI, COPII and CCVs [17,18]. To determine the vesicular transport involved in PEDV transport, Vero-E6 cells were infected with PEDV. At different time points, Vero-E6 cells were stained with anti-Sec21p (γ subunit of COPI), anti-COPII and 8 of 16 anti-clathrin antibodies to detect transport vesicles. The subcellular localization of PEDV N protein and trafficking vesicle markers was examined using a confocal microscopy. The confocal microscopic images showed that only COPII colocalized with PEDV N protein PEDV infection enhanced the colocalization of COPIIofand PEDV in a time-dependent and the PEDV infection enhanced the colocalization COPII andNPEDV N in a time-demanner Neither nor clathrin colocalized with PEDV protein at the pendent(Figure manner3B). (Figure 3B). COPI Neither COPI nor clathrin colocalized with N PEDV N protein indicated time points 3A,C). Vero-E6 cells were stained with anti-dsRNA at the indicated time (Figure points (Figure 3A,C). Vero-E6 cellsalso were also stained with antiantibody to detecttothe virus replication complex. We found that COPII colocalized with dsRNA antibody detect the virus replication complex. We found that COPII colocalized PEDV replicative intermediate dsRNA (Figure 3D). These findings suggested that COPIIwith PEDV replicative intermediate dsRNA (Figure 3D). These findings suggested that coated vesiclesvesicles mediatemediate PEDV trafficking. COPII-coated PEDV trafficking.

Figure3.3. PEDV PEDV N N protein protein and and its itsreplicative replicative intermediate intermediate dsRNA dsRNA colocalize colocalize with with COPII-coated COPII-coated Figure vesicles. Vero-E6 cells infected with HLJBY (MOI = 0.1) for 0, 6, 12 and 24 h. The cells were fixedfixed and vesicles. Vero-E6 cells infected with HLJBY (MOI = 0.1) for 0, 6, 12 and 24 h. The cells were stained with Sec21p (γ subunit of COPI) antibody (A); COPII antibody (B); clathrin antibody (C); and stained with Sec21p (γ subunit of COPI) antibody (A); COPII antibody (B); clathrin antibody and Alexa 488-conjugated goat anti-rabbit IgG antibodies (green) and then stained with PEDV-N (C); and Alexa 488-conjugated goat anti-rabbit IgG antibodies (green) and then stained with PEDV-N antibody and Alexa 555-conjugated goat anti-mouse IgG antibody (red). The nuclei were stained antibody and AlexaImages 555-conjugated goat with anti-mouse antibody (red). The nucleipanel were shows staineda with DAPI (blue). were acquired a NikonIgG confocal microscopy. Bottom with DAPI (blue). Images were acquired with a Nikon confocal microscopy. Bottom panel shows a magnified view of the boxed area in panels (A–C) (Merged). For quantitative colocalization analysis (QCA), Pearson correlation coefficient (PCC) values were calculated and represent the mean ± SD. (D) Vero-E6 cells infected with HLJBY (MOI = 0.1) for 24 h. The cells were fixed and stained with COPII antibody and Alexa 488-conjugated goat anti-rabbit IgG anti-bodies (green), and then stained with dsRNA antibody and Alexa 555-conjugated goat anti-mouse IgG antibody (red). The nuclei were stained with DAPI (blue). Images were acquired with a Nikon confocal microscopy. Bottom panel shows a magnified view of the boxed area in panel (D) (Merge). For quantitative colocalization analysis (QCA), PCC values were calculated and represent the mean ± SD.

SD. (D) Vero-E6 cells infected with HLJBY (MOI = 0.1) for 24 h. The cells were fixed and stained with COPII antibody and Alexa 488-conjugated goat anti-rabbit IgG anti-bodies (green), and then stained with dsRNA antibody and Alexa 555-conjugated goat anti-mouse IgG antibody (red). The nuclei were stained with DAPI (blue). Images were acquired with a Nikon confocal microscopy. Bottom panel shows a magnified view of the boxed area in panel D (Merge). For quantitative colocalization analysis (QCA), PCC values were calculated and represent the mean ± SD. 9 of 16

3.3. PEDV N Protein Is Efficiently Captured by The COPII-Coated Vesicles upon HDACSpecific Inhibitors Treatment 3.3. PEDV N Protein Is Efficiently Captured by The COPII-Coated Vesicles upon HDAC-Specific Our Treatment study showed that the HDAC-specific inhibitors facilitated PEDV release (FigInhibitors ures Our 1, 2 and S1) showed and COPII was colocalized with the PEDV N facilitated protein (Figure To destudy that the HDAC-specific inhibitors PEDV3).release termine whether HDAC-specific inhibitors promote the colocalization of COPII (Figures 1, 2 and S1) and COPII was colocalized with the PEDV N protein (Figure 3).and To PEDV N protein, cells were infected with the PEDV with or without TSA NaB determine whether Vero-E6 HDAC-specific inhibitors promote colocalization of COPII andorPEDV treatment. Vero-E6 cells cellswere wereinfected stained with to TSA identify transport vesN protein, Vero-E6 with anti-COPII PEDV with antibody or without or NaB treatment. icles. The colocalization of COPII and PEDV N was analyzed with confocal microscopy. Vero-E6 cells were stained with anti-COPII antibody to identify transport vesicles. The colocalPCC values showed that the of COPII andmicroscopy. PEDV N protein was enhanced ization of COPII and PEDV N colocalization was analyzed with confocal PCC values showed by HDAC-specific inhibitors (Figure 4A,B). These findings indicated that the HDAC-spethat the colocalization of COPII and PEDV N protein was enhanced by HDAC-specific incific inhibitors PEDV N proteins capture the COPII-coated vesicles. Immuhibitors (Figure promote 4A,B). These findings indicated thatinto the HDAC-specific inhibitors promote nofluorescence inhibitors reduced PEDV N protein PEDV N proteinshowed capturethat intothe theHDAC-specific COPII-coated vesicles. Immunofluorescence showedlevels that (Figure S2). the HDAC-specific inhibitors reduced PEDV N protein levels (Figure S2).

Figure 4. 4. The The colocalization between PEDV N and COPII is enhanced by HDAC-specific inhibitors. Figure Vero-E6 cells cells were were pretreated pretreatedwith withor orwithout withoutTSA TSA(60 (60ng/mL) ng/mL) and NaB (4 (4 mM) mM) for for 22 h, h, and and then then Vero-E6 and NaB infected with HLJBY (MOI = 1) for 1 h. The cells were further cultured in fresh medium in the presinfected with HLJBY (MOI = 1) for 1 h. The cells were further cultured in fresh medium in the ence of TSA and NaB at 8 h. (A) The cells were fixed and stained with COPII antibody and Alexa presence of TSA and NaB at 8 h. (A) The cells were fixed and stained with COPII antibody and Alexa 488-conjugated goat anti-rabbit IgG antibodies (green) and then stained with PEDV-N antibody and 488-conjugated goat anti-rabbit IgG antibodies (green) and then stained with PEDV-N antibody and Alexa 555-conjugated goat anti-mouse IgG antibody (red). The nuclei were stained with DAPI Alexa goatacquired anti-mouse antibody (red). microscopy. The nuclei were (blue). (blue).555-conjugated The images were withIgG a Nikon confocal (B) stained Graphs with showDAPI the PCC of The images were acquired with a Nikon confocal microscopy. (B) Graphs show the PCC of COPII and PEDV N. For quantitative colocalization analysis (QCA), PCC values were calculated and represent the mean ± SD. Student’s t test was used for statistical analysis. ***, p < 0.001; ****, p < 0.0001.

3.4. Secretion of COPII-Coated Vesicles Carrying PEDV Virions Is Promoted by HDAC-Specific Inhibitors To establish the PEDV secretion induced by HDAC-specific inhibitors, we analyzed the inhibitory effect on PEDV compartmentation using TEM. Vero-E6 cells were infected with PEDV and treated with or without TSA and NaB. The PEDV virus particles were detected by TEM. As expected, it was found that PEDV virions mainly accumulate in

0.0001.

3.4. Secretion of COPII-Coated Vesicles Carrying PEDV Virions Is Promoted by HDAC-Specific Inhibitors Viruses 2023, 15, 1874

To establish the PEDV secretion induced by HDAC-specific inhibitors, we analyzed 10 of 16 the inhibitory effect on PEDV compartmentation using TEM. Vero-E6 cells were infected with PEDV and treated with or without TSA and NaB. The PEDV virus particles were detected by TEM. As expected, it was found that PEDV virions mainly accumulate in ERER-like luminal structures in control In contrast, virions the HDAC-specific like luminal structures in control cells.cells. In contrast, PEDVPEDV virions in thein HDAC-specific inhibitors-treated cells were weremainly mainlyenclosed enclosedwithin withintransport transport vesicles; arrows indicate inhibitors-treated cells vesicles; thethe arrows indicate some that some transport vesicles containingonly only one virion containing multithat transport vesicles containing virionand andothers others containing multiple ple virions (Figure 5A–D). These findings suggested HDAC-specific inhibitors virions (Figure 5A–D). These findings suggested thatthat the the HDAC-specific inhibitors promote promote the secretion of transport vesicles containing PEDV virions. Intorder to whether verify the secretion of transport vesicles containing PEDV virions. In order verify the whether he transport vesicles were COPII-coated we performed to analyze transport vesicles were COPII-coated vesicles, vesicles, we performed IEM toIEM analyze the COPIIthe COPII-coated PEDVPEDV virions. PEDV was to be enclosed within coated vesicles forvesicles PEDV for virions. was found to found be enclosed within COPII-coated COPII-coated vesicles (Figure 5E). The data showed that the HDAC-specific inhibitors vesicles (Figure 5E). The data showed that the HDAC-specific inhibitors promote the promote the secretion of COPII-coated vesiclesPEDV carrying PEDV virions. secretion of COPII-coated vesicles carrying virions.

Figure 5. PEDV virions localized to COPII-coated vesicles following HDAC-specific inhibitors treatFigure 5. PEDV virions localized to COPII-coated vesicles following HDAC-specific inhibitors ment. Vero-E6 cells were pretreated with or without TSA (60 ng/mL) and NaB (4 mM) for 2 h, and treatment. Vero-E6 cells were pretreated with or without TSA (60 ng/mL) and NaB (4 mM) for then mock infected or infected with HLJBY (MOI = 0.1). After HLJBY adsorption for 1 h, the cells 2were h, and then mock infected infected with HLJBYof(MOI = 0.1). further cultured in fresh or medium in the presence TSA and NaBAfter at 12 HLJBY or 24 h. adsorption (A,C): Virusfor 1 h, particles a transmission electron microscopy (TEM).of Arrows indicate transport the cells were weredetected further with cultured in fresh medium in the presence TSA and NaB at 12 or 24 h. vesicles containing virions. Graphs the percentage of vesicles carrying PEDV virions.indicate (A,C): Virus particles were (B,D): detected with show a transmission electron microscopy (TEM). Arrows Student’s t test was used for statistical analysis. ***, p < 0.001. The error bars indicate standard devitransport vesicles containing virions. (B,D): Graphs show the percentage of vesicles carrying PEDV ation from three independent experiments. (E): Detection of COPII-coated vesicles by immunoelecvirions. Student’s t test was for statistical analysis. ***, p

3.5. HDAC-Specific Inhibitor-Promoted Secretion of PEDV Is Dependent on COPII Complex The COPII complex consists of five subunits: Sar1, Sec23, Sec24, Sec13 and Sec31 [23]. Sec23 acts as a GAP for Sar1. Sec24 is a primary subunit of the COPII-coated vesicles, which is responsible for the transportation of cargos from the ER to the Golgi apparatus [23,45,46]. A schematic diagram of the COPII-coated vesicles formation is presented in Figure 6A. To further establish the correlation between the COPII-coated vesicles and virus release, we disrupted the formation of the COPII-coated vesicles by knocking down Sec23A or Sec24B. Vero-E6 cells were transfected with Sec23A or Sec24B small interfering RNA (siRNA), followed by infection with PEDV with or without TSA treatment. The

3.5. HDAC-Specific Inhibitor-Promoted Secretion of PEDV Is Dependent on COPII Complex Viruses 2023, 15, 1874

The COPII complex consists of five subunits: Sar1, Sec23, Sec24, Sec13 and Sec31 [23]. Sec23 acts as a GAP for Sar1. Sec24 is a primary subunit of the COPII-coated vesicles, which is responsible for the transportation of cargos from the ER to the Golgi apparatus [23,45,46]. A schematic diagram of the COPII-coated vesicles formation is presented in 11 of 16 Figure 6A. To further establish the correlation between the COPII-coated vesicles and virus release, we disrupted the formation of the COPII-coated vesicles by knocking down Sec23A or Sec24B. Vero-E6 cells were transfected with Sec23A or Sec24B small interfering RNA (siRNA),levels followed by infection PEDVwere with significantly or without TSA treatment.in The en- treated endogenous of Sec23A andwith Sec24B decreased cells dogenous levels of Sec23A and Sec24B significantly in cells treated with with Sec23A/Sec24B-specific siRNAwere compared with decreased cells transfected with nontargeting Sec23A/Sec24B-specific siRNA with cells transfected scrambled siRNA (Figure 6B).compared Immunofluorescence showedwith thatnontargeting TSA reducedscramthe PEDV N bled siRNA (Figure 6B). Immunofluorescence showed that TSA reduced PEDV N level had no level in the cells transfected with non-targeting siRNA. However,the TSA treatment in the cells transfected with non-targeting siRNA. However, treatment had no signif- siRNA significant effect on PEDV N levels in cells treated withTSA Sec23A or Sec24B-specific icant effect on PEDV N levels in cells treated with Sec23A or Sec24B-specific siRNA (Fig(Figure 6C,D). The PFU data showed that TSA decreased the intracellular virus titer and ure 6C,D). The PFU data showed that TSA decreased the intracellular virus titer and inincreased the extracellular virus titer in cells with non-targeting siRNA transfected cells creased the extracellular virus titer in cells with non-targeting siRNA transfected cells (Figure 6E). PEDV release was evaluated using the ratio of extracellular-to-intracellular (Figure 6E). PEDV release was evaluated using the ratio of extracellular-to-intracellular virus titers. Wefound foundthat that PEDV release by TSA was inhibited cellsSec24B with Sec24B virus titers. We PEDV release by TSA was inhibited in cellsinwith knock- knockdown cells (Figure 6F). The above results indicated that Sec24B-containing COPII-coated down cells (Figure 6F). The above results indicated that Sec24B-containing COPII-coated vesicles are essential essentialfor forPEDV PEDVrelease release following HDAC-specific inhibitors treatment. vesicles are following HDAC-specific inhibitors treatment. In- Interestingly, we found that the decrease in PEDV N protein levels induced by HDAC-specific terestingly, we found that the decrease PEDV N protein levels induced by HDAC-speinhibitors leads to atodecrease in in Sec23A/Sec24B levels(Figure (Figure S3). cific inhibitors leads a decrease Sec23A/Sec24B protein protein levels S3).

Figure 6. Suppression of HDAC-specific inhibitors-induced PEDV secretion by Sec24B knockdown. (A): Schematic diagram of the vesicle budding process in the COPII complex. Vero-E6 cells were transfected with nontargeting scrambled siRNA or targeting Sec23A/Sec24B siRNA for 48 h, and then pretreated with or without TSA (40 ng/mL) for 2 h, followed by HLJBY (MOI = 0.1) infection. After HLJBY adsorption for 1 h, the cells were further cultured in fresh medium in the presence of TSA for 12 h. (B): Sec23A/Sec24B and actin were detected by immunoblotting. (C,D): The cells were fixed and stained with Sec24B or COPII antibody and Alexa 488-conjugated goat anti-rabbit IgG antibodies (green) and then stained with PEDV-N antibody and Alexa 555-conjugated goat anti-mouse IgG antibody (red). The nuclei were stained with DAPI (blue). The images were acquired with a Nikon immunofluorescence microscopy. (E): Virus titers were measured via plaque formation assay, and the graphs show changes in virus titers (intracellular and extracellular); 12 h (×105 ). (F): Graph shows PEDV release (ratio of extracellular to intracellular virus titers). Student’s t test was used for statistical analysis. ***, p < 0.001; ****, p < 0.0001. The error bars indicate standard deviation from three independent experiments.

antibodies (green) and then stained with PEDV-N antibody and Alexa 555-conjugated goat antimouse IgG antibody (red). The nuclei were stained with DAPI (blue). The images were acquired with a Nikon immunofluorescence microscopy. (E): Virus titers were measured via plaque formation assay, and the graphs show changes in virus titers (intracellular and extracellular); 12 h (×105). (F): Graph shows PEDV release (ratio of extracellular to intracellular virus titers). Student’s t 12 of 16 test was used for statistical analysis. ***, p < 0.001; ****, p < 0.0001. The error bars indicate standard deviation from three independent experiments.

4. Discussion Discussion 4. PED is a highly inin pigs. PEDV infection results in high morPED highlycontagious contagiousviral viraldisease disease pigs. PEDV infection results in high tality in neonatal suckling piglets [47,48]. Similar to other RNA viruses, PEDVs mortality in neonatal suckling piglets [47,48]. Similar to enveloped other enveloped RNA viruses, uses and modifies intracellular compartments of the secretory pathwaypathway to facilitate viral PEDVs uses and modifies intracellular compartments of the secretory to facilireplication and egression [13]. However, the underlying mechanisms of PEDV of secretion tate viral replication and egression [13]. However, the underlying mechanisms PEDV secretion remainunknown. largely unknown. In thiswe study, we demonstrated the HDAC-specific remain largely In this study, demonstrated that thethat HDAC-specific inhibiinhibitors the COPII-coated vesicles to promote 7). HDAC tors hijackhijack the COPII-coated vesicles to promote PEDVPEDV releaserelease (Figure(Figure 7). HDAC inhibiinhibitors have been reported to induce antiviral effects against a few enveloped RNA tors have been reported to induce antiviral effects against a few enveloped RNA viruses, viruses, including RSV, HCV and SARS-CoV-2. TSA and canRSV suppress RSVrepliand including RSV, HCV and SARS-CoV2. TSA and SAHA canSAHA suppress and HCV HCV [38–40]. Romidepsin of SARS-CoV-2 In the present cationreplication [38–40]. Romidepsin preventsprevents the entrythe ofentry SARS-CoV2 [41]. In [41]. the present study, study, we found that TSA and NaB promote the secretion PEDV virus into particles into we found that TSA and NaB promote the secretion of PEDVof virus particles the extrathe extracellular compartment andConsistently, S1). Consistently, the PFU showed cellular compartment (Figures(Figures 1 and 1S1). the PFU datadata showed thatthat the the HDAC-specific inhibitors facilitate the secretion but not assembly of infectious PEDV HDAC-specific inhibitors facilitate the secretion but not assembly of infectious PEDV parparticles (Figure ticles (Figure 2). 2).

Figure 7. The interplay between HDAC-specific inhibitors and COPII-coated vesicles during PEDV Figure 7. The interplay between HDAC-specific inhibitors and COPII-coated vesicles during PEDV infection. infection. Following Following the the entry entry of of PEDV PEDV into into host host cells cells and and replication replication in in the thecytoplasm, cytoplasm, the thenewly newly synthesized PEDV viral components and PEDV virus particles are transported to Golgi apparatus synthesized PEDV viral components and PEDV virus particles are transported to Golgi apparatus by by the theCOPII-coated COPII-coatedvesicles. vesicles. HDAC-specific HDAC-specific inhibitors inhibitors facilitate facilitate PEDV PEDV release release by by promoting promoting the the secretionof ofCOPII-coated COPII-coatedvesicles vesiclescarrying carryingPEDV PEDVvirions. virions. secretion

Virion assembly occurs in the cytoplasmic side of the ERGIC/Golgi compartments in CoVs. Alpha-coronaviruses (TGEV, HCoV-NL36) and beta-coronaviruses (MHV) can assemble in the ER at later stages of virus infection [8–12]. PEDV has been reported to assemble in both the ER and Golgi apparatus, and the newly assembled virus particles subsequently utilize the secretory pathway for egression [13]. In our study, we observed the accumulation of PEDV virions mainly in the expanded ER lumen of control cells. In contrast, PEDV virions were mainly enclosed within transport vesicles in the HDACspecific inhibitors-treated cells (Figure 5A–D). Further, we found that COPII-coated vesicles carried PEDV virions (Figure 5E). Thus, the results indicated that the HDAC-specific inhibitors promoted the secretion of COPII-coated vesicles carrying PEDV virions. HDACspecific inhibitors promote the release of PEDV, and the virus could utilize the COPII-coated vesicles for intracellular trafficking. Vesicle transport requires a group of conserved proteins, such as Rab GTPases, motor adaptors, and motor proteins to ensure vesicle transport along the cytoskeletal track [17]. HDAC inhibitors are able to affect cell transport, the promotion

of IAV virion release by tubacin via acetylated microtubules [49,50]. Therefore, whether TSA and NaB promote the movement of the COPII-coated vesicles carrying PEDV virions along cytoskeletal remains to be determined. COPII-coated vesicles promote the intracellular transport of cargos from the ER to the Golgi apparatus. COPII-coated vesicles have been reported to mediate in intracellular transport of several viruses, such as Ebola virus, Marburg virus, hepatitis B virus, HCV, parvovirus, and rotavirus [30–34]. Here, we demonstrated that the HDAC-specific inhibitors-induced COPII-coated vesicles are essential for PEDV release (Figure 6). These findings also suggest that PEDV assembly is inhibited by Sec23A or Sec24B depletion (Figure 6). This indicated that the COPII-coated vesicles not only mediate the transport of PEDV virion assembled in the ER, but also mediate the transport of PEDV viral protein from the ER to Golgi for assembly. Our study is consistent with previous studies reporting that PEDV particles can be assembled in both the ER and Golgi apparatus [13]. It is generally assumed that virions that assemble in the ER are exported via the COPII-mediated early secretory pathway; the virions first reach the Golgi apparatus and TGN, followed by transport to the plasma membrane and egress [8]. However, a few studies reported that the beta-coronavirus MHV use lysosomes for egress and that the enteroviruses (poliovirus) and classical swine fever virus (CSFV) release occurred via autophagy pathway [10,51,52]. Whether PEDV viral particles in COPII-coated vesicles may use the biosynthetic secretory pathway or autophagosomes/lysosomes to egress requires further investigation. In summary, our findings reveal that PEDV virions assemble in the ER and bud off from the ER in the COPII-coated vesicles. We provide clear evidence to show that the HDAC-specific inhibitors hijack the COPII-coated vesicles to promote PEDV release.

📖 中文全文 Chinese Full Text

中文

# HDAC特异性抑制剂通过COPII包被小泡诱导猪流行性腹泻病毒的释放

**摘要:** 猪流行性腹泻病毒(PEDV)是一种α-冠状病毒,可引起新生仔猪急性腹泻和高死亡率,给全球养猪业造成巨大的经济负担。PEDV作为一种有包膜的RNA病毒,其复制、组装和细胞外排均通过改变细胞内运输来实现。然而,PEDV分泌的机制尚不清楚。在本研究中,我们发现组蛋白去乙酰化酶(HDAC)特异性抑制剂——曲古抑菌素A(TSA)和丁酸钠(NaB)能够促进感染性PEDV颗粒的分泌,但不干扰其组装。研究发现,PEDV N蛋白及其复制中间体dsRNA与COPII包被小泡共定位。我们还发现,HDAC特异性抑制剂增强了PEDV与COPII的共定位。此外,超微结构分析显示,HDAC特异性抑制剂促进了携带PEDV病毒粒子的COPII包被小泡的分泌。一致地,敲低Sec24B可消除HDAC特异性抑制剂诱导的PEDV颗粒分泌,表明HDAC特异性抑制剂介导的COPII包被小泡是PEDV分泌所必需的。综上所述,我们的研究结果提供了初步证据,表明PEDV病毒粒子可在内质网(ER)中组装,并通过COPII包被小泡从内质网出芽。HDAC特异性抑制剂通过劫持COPII包被小泡来促进PEDV的释放。

**关键词:** HDAC特异性抑制剂;COPII包被小泡;猪流行性腹泻病毒;病毒释放

## 1. 引言

冠状病毒(CoVs)属于冠状病毒目(Nidovirales)冠状病毒科(Coronaviridae),为具有正义单链RNA基因组的有包膜病毒。冠状病毒科包括两个亚科:冠状病毒亚科(Coronavirinae)和环曲病毒亚科(Torovirinae)。冠状病毒亚科根据基因型和血清学特征进一步分为四个属:α-、β-、γ-和δ-冠状病毒。严重急性呼吸综合征冠状病毒(SARS-CoV)和严重急性呼吸综合征冠状病毒2(SARS-CoV-2)属于β-冠状病毒。猪流行性腹泻病毒(PEDV)是冠状病毒科中的一种α-冠状病毒,可引起新生仔猪严重水样腹泻、呕吐、脱水和高死亡率,给全球养猪业造成巨大经济损失。

CoVs及其他有包膜病毒利用并修饰分泌途径的细胞内区室,通过劫持宿主细胞的运输机器来促进其复制、组装和外排。病毒颗粒在内质网-高尔基体中间区室(ERGIC)/高尔基体区室中组装,这是CoVs的一般特征。先前的研究报道,α-冠状病毒(TGEV、HCoV-NL36)和β-冠状病毒(MHV)在病毒感染晚期在内质网中组装。其他研究表明,PEDV颗粒可在内质网和高尔基体中组装。

PEDV的外排途径由携带新合成基因组的核衣壳(N)蛋白与结构蛋白——刺突蛋白(S)、包膜蛋白(E)和膜蛋白(M)之间的相互作用触发,芽生进入内质网和ERGIC的腔内。病毒颗粒通过囊泡运输到达高尔基体和反式高尔基网络(TGN),进行糖基化和其他翻译后修饰。成熟病毒粒子随后通过光滑壁小泡与质膜融合而释放,类似于胞吐作用。然而,PEDV分泌的潜在机制尚未完全阐明。

在真核细胞中,传统的分泌运输途径的特征是新合成的脂质和蛋白质通过运输小泡从内质网经ERGIC和高尔基体依次运输至质膜。细胞内运输小泡主要由COPI、COPII和网格蛋白包被小泡(CCVs)组成。COPII包被小泡介导货物从内质网向高尔基体的运输。COPI包被小泡介导货物从高尔基体向内质网的运输,或高尔基体顺面网状结构之间的运输。CCVs介导货物从TGN向内体的运输以及质膜上货物的内吞作用。

COPII包被机器由五种胞质蛋白组成:Sar1、Sec23、Sec24、Sec13和Sec31。COPII包被小泡的组装始于GTP交换因子(GEF)Sec12对小分子胞质GTP酶Sar1的招募和激活。Sar1-GTP插入内质网膜,通过与Sec23结合招募Sec23/Sec24异源二聚体。Sec23作为Sar1的GTP酶激活蛋白(GAP),Sec24参与货物选择。携带装载有货物的Sec23/Sec24异源二聚体的Sar1形成所谓的"前出芽复合物",进而招募Sec13/Sec31异源四聚体到"前出芽复合物"上,完成小泡形成。作为内质网输出的经典分泌途径,COPII包被小泡常被劫持用于病毒基因组复制和病毒颗粒的运输。例如,脊髓灰质炎病毒利用COPII包被小泡形成复制复合物(RCs)。细小病毒颗粒、乙肝亚病毒包膜颗粒、丙型肝炎病毒(HCV)脂病毒颗粒、轮状病毒NSP4以及埃博拉病毒和马尔堡病毒基质蛋白VP40均利用COPII运输系统进行细胞内运输。

HDAC抑制剂已被美国食品药品监督管理局(FDA)批准作为癌症治疗药物,并被认为是其他疾病的候选治疗药物,包括关节炎、心脏病、炎症性疾病和一些神经系统疾病。此外,研究发现HDAC抑制剂具有抗病毒作用。TSA和辛二酰苯胺异羟肟酸(SAHA)可抑制呼吸道合胞病毒(RSV)和HCV的复制。罗米地辛可阻止SARS-CoV-2的进入。此外,I类选择性HDAC抑制剂可增强HIV潜伏期逆转。

本研究探讨了HDAC特异性抑制剂与COPII包被小泡在PEDV感染过程中的关系。我们发现HDAC特异性抑制剂TSA和NaB促进感染性PEDV颗粒的分泌。我们还发现PEDV颗粒利用COPII包被小泡进行细胞内运输。此外,透射电子显微镜(TEM)和免疫电子显微镜(IEM)显示,携带PEDV病毒粒子的COPII包被小泡的分泌被HDAC特异性抑制剂处理所促进。最后,我们还证明敲低Sec23A或Sec24B可抑制HDAC特异性抑制剂诱导的PEDV分泌。综上所述,本研究证实HDAC特异性抑制剂诱导的COPII包被小泡对PEDV的释放至关重要。

## 2. 材料与方法

### 2.1. 细胞培养

非洲绿猴肾上皮细胞(Vero-E6细胞)在添加8%胎牛血清(Pan-Biotech公司,德国艾登巴赫)和1%青霉素-链霉素(MDBio公司,中国青岛)的Dulbecco改良Eagle培养基(DMEM)(Invitrogen公司,美国加利福尼亚州卡尔斯巴德)中,于37°C、5% CO₂培养箱中培养。

### 2.2. 抗体和试剂

兔多克隆抗Sec21p抗体由Agrisera公司(瑞典瓦纳斯)提供。兔多克隆抗COPII抗体购自Invitrogen公司(美国加利福尼亚州卡尔斯巴德)。兔多克隆抗网格蛋白抗体由Abcam公司(英国剑桥)提供。兔单克隆抗Sec24B(D7D6S)购自Cell Signaling Technology公司(美国马萨诸塞州丹弗斯)。兔多克隆抗乙酰化组蛋白H3(Lys 9/14)购自Santa Cruz公司(美国德克萨斯州达拉斯)。兔多克隆抗肌动蛋白(A2066)抗体购自Merck公司(德国达姆施塔特)。小鼠多克隆抗PEDV-N和兔多克隆抗PEDV-N抗体为本实验室先前制备。辣根过氧化物酶(HRP)标记的羊抗兔IgG和HRP标记的羊抗小鼠IgG抗体购自MiliporeSigma(Merck公司,德国达姆施塔特)。Alexa 488标记的羊抗兔IgG(A-11001)和Alexa 555标记的羊抗小鼠IgG(A-21428)抗体由Thermo Fisher Scientific公司(美国马萨诸塞州沃尔瑟姆)提供。10 nm标记的羊抗兔二抗(G7402)购自Sigma-Aldrich公司(美国密苏里州圣路易斯)。TSA和NaB由Selleck公司(美国德克萨斯州休斯顿)提供。戊二醛(2.5%,pH 7.4)和多聚甲醛(4%)-戊二醛(0.5%)混合液(pH 7.4)购自上海源叶生物科技有限公司。乙醇购自国药集团化学试剂有限公司。LR White树脂由海德百奥生物技术(北京)有限公司提供。增强化学发光(ECL)试剂购自南京优清生物科技有限公司。

### 2.3. 病毒感染和滴度测定

PEDV(HLJBY株)在Vero-E6细胞中培养。将细胞在无FBS的DMEM中接种PEDV,37°C孵育1 h。孵育后,用磷酸盐缓冲液(PBS)洗涤细胞,转移至含2% FBS和17.5 ng/mL胰蛋白酶的DMEM中。采用噬斑形成实验测定病毒滴度。简言之,接种前一天将1×10⁶个Vero-E6细胞接种于6孔板各孔。用PBS洗涤细胞,将10倍系列稀释(10²至10⁷)的病毒与Vero-E6细胞单层在37°C下孵育1 h。孵育后,用PBS洗涤细胞,加入2 mL覆盖培养基(含2%低熔点琼脂糖(Lonza公司,瑞士巴塞尔)、2× DMEM、2% FBS和17.5 ng/mL胰蛋白酶)。将平板在37°C、5% CO₂条件下孵育2-3天。用0.5%结晶紫对细胞进行染色。

### 2.4. Western印迹分析

用2× SDS上样缓冲液(4% SDS、0.1 M Tris-HCl pH 6.8、20%甘油、2%溴酚蓝和10% β-巯基乙醇)制备全细胞裂解物,98°C煮沸10 min。随后,将样品进行十二烷基硫酸钠-聚丙烯酰胺凝胶电泳(SDS-PAGE),然后使用Mighty Small转印槽系统(Hoefer公司,美国马萨诸塞州)将蛋白转移至硝酸纤维素转印膜(Pall Corporation公司,美国华盛顿州华盛顿港)。随后,将膜用含0.5% Tween 20的PBS(PBST)中的3%脱脂牛奶在室温下封闭30 min,然后与特异性一抗在4°C下孵育过夜,再与二抗在4°C下孵育4 h。用增强化学发光(ECL)试剂显色,使用BioSpectrum成像系统(UVP公司,美国加利福尼亚州阿普兰)成像。

### 2.5. Sec23A/Sec24B表达敲低

针对Sec24B的siRNA寡核苷酸和非靶向对照siRNA购自Biotend公司(中国上海)。对于siRNA基因敲低实验,将3.6×10⁵个Vero-E6细胞接种于6孔板各孔中培养18 h,使用7.5 µL Mirus转染试剂按照制造商说明书(美国威斯康星州麦迪逊)转染50 nM siRNA寡核苷酸。转染48 h后,通过免疫印迹分析敲低效率。Sec23A和Sec24B RNA干扰(RNAi)靶序列如下:siSec23A-1,5'-AAG GAA UCA GUU UCC ACC UAG UUA U-3';siSec23A-2,5'-CCU ACA GCU UUG GUU GGA CUU AUU A-3';siSec24B-1,5'-CGG UAU AUU CUG GAU UCC AAC AGU A-3';siSec24B-2,5'-CCC GAU CUU AUG GAG AGC CUC AUA A-3'。

### 2.6. 免疫荧光显微镜

将Vero-E6细胞生长于盖玻片上,用或不用TSA预处理2 h,然后用PEDV感染不同时间。将盖玻片上的细胞用4%甲醛和0.1% Triton X-100在37°C下固定和透化30 min。用甘氨酸-PBS洗涤后,用PBS中的3% BSA在37°C下封闭30 min。将盖玻片与一抗(1:200)在37°C下孵育1 h,然后与二抗(1:500)在37°C下孵育30 min。用PBST洗涤三次去除未结合的抗体。用含抗荧光淬灭DABCO溶液的4',6-二脒基-2-苯基吲哚(DAPI)染核(Thermo Fisher Scientific公司,美国马萨诸塞州沃尔瑟姆)。图3和图4A的图像使用共聚焦显微镜(Nikon Eclipse Ti,A1,日本东京)获取,图6C、6D和图S2使用荧光显微镜(Nikon Eclipse Ti-U,日本东京)获取。

### 2.7. 透射电子显微镜/免疫电子显微镜

将Vero-E6细胞用或不用TSA和NaB预处理2 h,然后用PEDV以MOI = 0.1模拟感染或感染。12或24 h后,收集细胞并离心成细胞团。首先,将细胞团在冷戊二醛(2.5%,pH 7.4,TEM)或冷多聚甲醛(4%)-戊二醛(0.5%)混合液(pH 7.4,IEM)中于4°C固定过夜,随后进行清洗、固定、脱水、树脂渗透、包埋、固化、聚合、超薄切片和染色等步骤。沉淀用0.1 M PB(pH 7.4)洗涤3次,每次10 min。用1%锇酸固定后清洗。将固定的细胞团在不同浓度的乙醇中进行梯度脱水。用不同浓度的包埋剂进行树脂渗透。使用包埋胶囊在4°C下进行包埋。固化步骤在55°C培养箱中进行48 h(TEM)。对于IEM,在-20°C下使用低温紫外聚合仪UVCC2515(北京中镜科仪技术有限公司)进行聚合超过48 h。使用Leica UC7超薄切片机(德国韦茨拉尔)从树脂块上获取70-80 nm的超薄切片,将组织捞至覆有Formvar膜的150目镍网(北京中镜科仪技术有限公司)上,4°C保存。免疫标记通过以下步骤进行:与抗COPII抗体在4°C下孵育过夜,然后与10 nm标记的羊抗兔二抗(室温20 min;37°C 1 h;室温30 min)孵育(IEM)。对于TEM/IEM,样品用2%醋酸铀酰和柠檬酸铅染色。在80 kV加速电压下使用Hitachi H-7650(日立公司,日本东京)TEM观察切片。

### 2.8. 细胞活力分析

通过Cell Counting Kit-8(CCK-8)实验按照制造商说明书(APExBIO Technology公司,美国德克萨斯州休斯顿)测定HDAC特异性抑制剂的细胞毒性。简言之,将Vero-E6细胞接种于96孔板中培养24 h,然后用递增剂量的HDAC抑制剂处理12或24 h,随后加入CCK-8试剂(10 µL/孔)在37°C下孵育4 h。最后,在酶标仪中测定450 nm处的吸光度。

### 2.9. 统计分析

所示结果为三次重复实验的代表性数据。所有统计检验均使用GraphPad Prism 7.0软件(美国加利福尼亚州圣地亚哥)进行,以均值±标准差(SD)表示。使用Student t检验确定统计学显著性。p值<0.05被认为具有统计学显著性。

## 3. 结果

### 3.1. HDAC特异性抑制剂促进PEDV颗粒分泌

HDAC抑制剂如TSA和SAHA可抑制HCV和RSV的复制,而罗米地辛可抑制SARS-CoV-2的进入。这一发现促使我们研究HDAC抑制剂是否调节PEDV感染。为了验证这一可能性,将Vero-E6细胞用或不用TSA和NaB(I类和II类HDAC抑制剂)预处理,然后用PEDV感染。分别收集培养基和感染细胞。为了检测HDAC特异性抑制剂的细胞毒性,我们进行了CCK-8实验。我们发现本研究中使用的浓度下的HDAC特异性抑制剂不影响细胞活力(图1A、B)。为了确定HDAC特异性抑制剂的功能,通过Western印迹分析乙酰化组蛋白H3来检测感染细胞裂解物。HDAC特异性抑制剂处理增加了乙酰化组蛋白H3的蛋白水平(图1C、F)。对感染细胞裂解物和培养基进行Western印迹分析,检测细胞内和细胞外PEDV N蛋白水平。我们发现HDAC特异性抑制剂降低了细胞内PEDV N蛋白水平,但增加了细胞外PEDV N蛋白水平(图1C、F和图S1)。经TSA处理的细胞上清中分泌的感染性病毒颗粒水平约为DMSO处理细胞的2.0倍(图1D、E)。经NaB处理的细胞上清中分泌的感染性病毒颗粒水平约为对照细胞的2.3倍(图1G、H)。这些数据表明HDAC特异性抑制剂促进PEDV病毒颗粒向细胞外培养基的分泌。

为了进一步分析HDAC特异性抑制剂对PEDV感染的影响,将Vero-E6细胞用或不用TSA和NaB预处理,然后用PEDV感染。通过噬斑形成实验(PFU)测定细胞内和细胞外病毒滴度。PFU结果显示,HDAC特异性抑制剂处理降低了细胞内病毒滴度,增加了细胞外病毒滴度(图2A、B、D、E)。我们使用细胞外和细胞外区室病毒滴度的比值来评估病毒释放。结果显示,与NaB处理约增加2.7倍相比,TSA处理导致感染性病毒颗粒释放增加约3.3倍(图2C、F)。然而,与对照组相比,HDAC特异性抑制剂处理的细胞的总病毒滴度没有显著变化(图2G、H)。这些数据表明HDAC特异性抑制剂在不影响PEDV组装的情况下促进其释放。

### 3.2. PEDV N蛋白及其复制复合物与COPII包被小泡共定位

据报道,PEDV利用光滑壁小泡进行外排。先前的研究表明,真核细胞中的细胞内运输小泡主要由COPI、COPII和CCVs组成。为了确定参与PEDV运输的囊泡运输类型,用PEDV感染Vero-E6细胞。在不同时间点,用抗Sec21p(COPI的γ亚基)、抗COPII和抗网格蛋白抗体对Vero-E6细胞进行染色以检测运输小泡。使用共聚焦显微镜检查PEDV N蛋白和运输小泡标记物的亚细胞定位。共聚焦显微镜图像显示,仅COPII与PEDV N蛋白共定位,且PEDV感染以时间依赖性方式增强了COPII与PEDV N的共定位(图3B)。COPI和网格蛋白在所检测的时间点均不与PEDV N蛋白共定位(图3A、C)。还用抗dsRNA抗体对Vero-E6细胞进行染色以检测病毒复制复合物。我们发现COPII与PEDV复制中间体dsRNA共定位(图3D)。这些发现表明COPII包被小泡介导PEDV的运输。

### 3.3. HDAC特异性抑制剂处理后PEDV N蛋白被COPII包被小泡有效捕获

我们的研究表明HDAC特异性抑制剂促进PEDV释放(图1、2和图S1),且COPII与PEDV N蛋白共定位(图3)。为了确定HDAC特异性抑制剂是否促进COPII与PEDV N蛋白的共定位,将Vero-E6细胞用或不用TSA或NaB处理后感染PEDV。用抗COPII抗体对Vero-E6细胞进行染色以鉴定运输小泡。通过共聚焦显微镜分析COPII与PEDV N的共定位。PCC值显示,HDAC特异性抑制剂增强了COPII与PEDV N蛋白的共定位(图4A、B)。这些发现表明HDAC特异性抑制剂促进PEDV N蛋白进入COPII包被小泡。免疫荧光显示HDAC特异性抑制剂降低了PEDV N蛋白水平(图S2)。

### 3.4. 携带PEDV病毒粒子的COPII包被小泡的分泌被HDAC特异性抑制剂促进

为了证实HDAC特异性抑制剂诱导的PEDV分泌,我们使用TEM分析了PEDV区室化的抑制效果。将Vero-E6细胞感染PEDV并用或不用TSA和NaB处理。通过TEM检测PEDV病毒粒子。正如预期的那样,发现PEDV病毒粒子主要积聚在细胞内囊泡中。在HDAC特异性抑制剂处理后,携带PEDV病毒粒子的COPII包被小泡的分泌增加。这些结果进一步证实了HDAC特异性抑制剂通过COPII包被小泡促进PEDV分泌。

为证实HDAC特异性抑制剂可诱导PEDV的分泌,我们利用透射电子显微镜(TEM)分析了10种抑制剂对PEDV区室化的影响。Vero-E6细胞感染PEDV后,分别给予或不给予TSA和NaB处理,随后通过TEM检测PEDV病毒颗粒。结果发现,在对照组细胞中,PEDV病毒粒子主要积聚在ER-ER样管腔结构中;相反,在经HDAC特异性抑制剂处理的细胞中,病毒粒子主要被包裹在运输囊泡内;箭头指示部分运输囊泡仅含单个病毒粒子,而另一些则含有多个病毒粒子(图5A–D)。上述结果表明,HDAC特异性抑制剂可促进携带PEDV病毒粒子的运输囊泡的分泌。为验证这些运输囊泡是否为COPII包被囊泡,我们采用免疫电子显微镜(IEM)对COPII包被的PEDV病毒粒子进行分析。结果发现,PEDV病毒粒子确实被包裹在COPII包被的囊泡内(图5E)。数据表明,HDAC特异性抑制剂可促进携带PEDV病毒粒子的COPII包被囊泡的分泌。

图5. HDAC特异性抑制剂处理后PEDV病毒粒子定位于COPII包被囊泡。Vero-E6细胞经TSA(60 ng/mL)和NaB(4 mM)预处理2小时(或不处理),随后以HLJBY毒株(MOI = 0.1)进行模拟感染或感染。HLJBY吸附1小时后,细胞在含TSA和NaB的新鲜培养基中继续培养12或24小时。(A,C):通过透射电子显微镜(TEM)检测病毒颗粒。箭头指示含有病毒粒子的运输囊泡。(B,D):图表显示携带PEDV病毒粒子的囊泡百分比。采用Student’s t检验进行统计分析。***,p < 0.001。误差线表示三次独立实验的标准偏差。(E):通过免疫电子显微镜(IEM)检测COPII包被囊泡。红色方框显示包裹在COPII阳性囊泡中的PEDV病毒粒子。黑色箭头指向标记COPII的纳米金颗粒(10 nm),白色箭头指向PEDV病毒粒子。

3.5. HDAC特异性抑制剂促进的PEDV分泌依赖于COPII复合体 COPII复合体由五个亚基组成:Sar1、Sec23、Sec24、Sec13和Sec31 [23]。Sec23作为Sar1的GAP发挥作用。Sec24是COPII包被囊泡的主要亚基,负责将货物从内质网(ER)运输至高尔基体[23,45,46]。COPII包被囊泡形成的示意图见图6A。为进一步明确COPII包被囊泡与病毒释放之间的关联,我们通过敲低Sec23A或Sec24B来干扰COPII包被囊泡的形成。将Vero-E6细胞转染Sec23A或Sec24B小干扰RNA(siRNA)后,再感染PEDV(无论是否给予TSA处理)。结果显示,与转染非靶向乱序siRNA的细胞相比,经Sec23A/Sec24B特异性siRNA处理的细胞中Sec23A和Sec24B的内源水平显著降低(图6B)。免疫荧光结果显示,在非靶向siRNA转染的细胞中,TSA可降低PEDV N蛋白水平;然而,在经Sec23A或Sec24B特异性siRNA处理的细胞中,TSA处理对PEDV N蛋白水平无显著影响(图6C,D)。空斑形成实验(PFU)数据显示,在非靶向siRNA转染的细胞中,TSA降低了细胞内病毒滴度,同时提高了细胞外病毒滴度(图6E)。通过细胞外与细胞内病毒滴度的比值评估PEDV释放情况。结果发现,TSA促进的PEDV释放在Sec24B敲低细胞中受到抑制(图6F)。上述结果表明,含有Sec24B的COPII包被囊泡对于HDAC特异性抑制剂处理后的PEDV释放至关重要。有趣的是,我们发现HDAC特异性抑制剂引起的PEDV N蛋白水平下降可导致Sec23A/Sec24B蛋白水平降低(图S3)。

图6. Sec24B敲低抑制HDAC特异性抑制剂诱导的PEDV分泌。(A):COPII复合体囊泡出芽过程示意图。Vero-E6细胞转染非靶向乱序siRNA或靶向Sec23A/Sec24B的siRNA 48小时后,再经TSA(40 ng/mL)预处理2小时(或不处理),随后以HLJBY(MOI = 0.1)感染。HLJBY吸附1小时后,细胞在含TSA的新鲜培养基中继续培养12小时。(B):通过免疫印迹检测Sec23A/Sec24B和肌动蛋白。(C,D):细胞固定后,用Sec24B或COPII抗体及Alexa 488标记的羊抗兔IgG抗体(绿色)染色,再用PEDV-N抗体及Alexa 555标记的羊抗鼠IgG抗体(红色)染色。细胞核用DAPI(蓝色)染色。图像通过尼康荧光显微镜采集。(E):通过空斑形成实验测定病毒滴度,图表显示病毒滴度(细胞内和细胞外)的变化;12小时(×10⁵)。(F):图表显示PEDV释放情况(细胞外与细胞内病毒滴度比值)。采用Student’s t检验进行统计分析。***,p < 0.001;****,p < 0.0001。误差线表示三次独立实验的标准偏差。

4. 讨论 PED是一种在猪群中高度传染的病毒性疾病。PEDV感染可导致新生仔猪高死亡率[47,48]。与其他包膜RNA病毒类似,PEDV利用并改造分泌途径的细胞内区室以促进病毒复制和释放[13]。然而,PEDV分泌的潜在机制仍 largely 未知。在本研究中,我们证明HDAC特异性抑制剂劫持COPII包被囊泡以促进PEDV释放(图7)。已有研究表明,HDAC特异性抑制剂对某些包膜RNA病毒(如RSV、HCV和SARS-CoV-2)具有抗病毒作用。TSA和SAHA可抑制RSV和HCV的复制[38–40]。罗米地辛(Romidepsin)可阻止SARS-CoV-2的进入[41]。在本研究中,我们发现TSA和NaB可促进PEDV病毒粒子向细胞外区室的分泌(图1和S1)。一致地,PFU数据表明,HDAC特异性抑制剂促进感染性PEDV颗粒的分泌而非组装(图2)。

图7. HDAC特异性抑制剂与COPII包被囊泡在PEDV感染过程中的相互作用。PEDV进入宿主细胞并在细胞质中复制后,新合成的PEDV病毒组分和病毒粒子通过COPII包被囊泡运输至高尔基体。HDAC特异性抑制剂通过促进携带PEDV病毒粒子的COPII包被囊泡的分泌来促进PEDV释放。

在冠状病毒中,病毒粒子组装发生在ERGIC/高尔基体的胞质侧。α冠状病毒(TGEV、HCoV-NL36)和β冠状病毒(MHV)可在病毒感染晚期在内质网中完成组装[8–12]。已有报道显示,PEDV可在内质网和高尔基体中组装,新组装的病毒粒子随后利用分泌途径进行释放[13]。在本研究中,我们观察到在对照组细胞中,PEDV病毒粒子主要积聚在扩张的内质网管腔内;相反,在经HDAC特异性抑制剂处理的细胞中,病毒粒子主要被包裹在运输囊泡内(图5A–D)。进一步研究发现,COPII包被囊泡携带PEDV病毒粒子(图5E)。因此,结果表明HDAC特异性抑制剂促进了携带PEDV病毒粒子的COPII包被囊泡的分泌。HDAC特异性抑制剂促进PEDV释放,且病毒可利用COPII包被囊泡进行细胞内运输。囊泡运输需要一组保守蛋白(如Rab GTP酶、马达适配体和马达蛋白)以确保囊泡沿细胞骨架轨道运输[17]。HDAC抑制剂可影响细胞运输,例如tubacin通过乙酰化微管促进IAV病毒粒子释放[49,50]。因此,TSA和NaB是否促进携带PEDV病毒粒子的COPII包被囊泡沿细胞骨架运动仍有待进一步研究。

COPII包被囊泡促进货物从内质网向高尔基体的细胞内运输。已有研究表明,COPII包被囊泡介导多种病毒的细胞内运输,如埃博拉病毒、马尔堡病毒、乙型肝炎病毒、HCV、细小病毒和轮状病毒[30–34]。本研究中,我们证明HDAC特异性抑制剂诱导的COPII包被囊泡对PEDV释放至关重要(图6)。这些发现还表明,Sec23A或Sec24B的耗竭可抑制PEDV的组装(图6)。这说明COPII包被囊泡不仅介导在内质网中组装的PEDV病毒粒子的运输,还介导PEDV病毒蛋白从内质网向高尔基体的运输以完成组装。本研究结果与先前报道一致,即PEDV颗粒可在内质网和高尔基体中组装[13]。

通常认为,在内质网中组装的病毒粒子通过COPII介导的早期分泌途径输出:病毒粒子首先到达高尔基体和TGN,随后被运输至质膜并释放[8]。然而,少数研究表明,β冠状病毒MHV利用溶酶体进行释放,而肠道病毒(脊髓灰质炎病毒)和猪瘟病毒(CSFV)则通过自噬途径释放[10,51,52]。PEDV病毒粒子在COPII包被囊泡中是否利用生物合成分泌途径或自噬体/溶酶体进行释放,仍需进一步研究。总之,我们的研究结果表明,PEDV病毒粒子在内质网中组装,并通过COPII包被囊泡从内质网出芽。我们提供了明确证据,表明HDAC特异性抑制剂劫持COPII包被囊泡以促进PEDV释放。