Design of dual-effect molecules based on lysosome-targeting strategy: a mechanistic study on synergistic inhibition of ewing sarcoma and coronaviruses

✅ 全文
作者 Shimeng Zhou; Lu Xu; Wenlong Ge 期刊 Frontiers in Chemistry 发表日期 2026 卷/期/页码 Vol. 14 ISSN 2296-2646 DOI 10.3389/fchem.2026.1851116 类型 原创研究 (Original Research)

📄 英文摘要 English Abstract

EN

Introduction Addressing clinical challenges such as the toxicity of conventional chemotherapy and viral drug resistance, this study proposes and validates an innovative “host organelle-targeting” strategy. By disrupting the function of host lysosomes—an organelle commonly exploited by both tumors and viruses—we aim to develop novel therapeutic agents with dual antitumor and antiviral activity.

Methods

We rationally designed and synthesized the target compound 3-chloro-4-(4-(diethylamino)butoxy)benzaldehyde, whose core design relies on the pH-responsive property of the 4-(diethylamino)butoxy side chain to enable specific enrichment within the acidic lumen of lysosomes.

In vitro activity was evaluated against Ewing sarcoma cells (TC32), prostate cancer bone metastasis model cells, porcine epidemic diarrhea virus (PEDV), and transmissible gastroenteritis virus (TGEV). Mechanistic investigations assessed lysosomal pH, autophagic flux, endoplasmic reticulum stress-related gene expression, p53 signaling pathway, cell cycle, and apoptosis.

Results

The compound potently inhibited the proliferation of TC32 cells (IC

50 = 25 μM) and prostate cancer bone metastasis cells, and significantly suppressed the replication of PEDV and TGEV. Mechanistic studies revealed that the compound neutralizes lysosomal pH, impairs acidification, blocks autophagic flux, upregulates endoplasmic reticulum stress-related gene expression, activates the p53 signaling pathway, and inhibits the cell cycle, ultimately leading to apoptosis.

Conclusion This study reports a chemical entity with well-defined dual antitumor and antiviral activities and provides mechanistic evidence supporting the feasibility of the “host-lysosome targeting” strategy. It thus offers an important proof-of-concept and a research framework for developing broad-spectrum host-directed therapies.

📄 中文摘要 Chinese Abstract

中文
针对传统化疗的毒性和病毒耐药性等临床挑战,本研究提出并验证了一种创新的“宿主细胞器靶向”策略。尤文肉瘤是一种高度侵袭性的骨肿瘤,主要累及儿童和青少年,分子特征以EWSR1-FLI1等融合基因驱动为特点;由于广泛毒性、肿瘤异质性和获得性耐药,目前的多模式治疗对转移性或复发性疾病疗效有限。以猪流行性腹泻病毒(PEDV)为代表的冠状病毒高度依赖宿主细胞的内吞-溶酶体系统完成入侵和复制,这揭示了一种生物学平行关系:快速增殖的肿瘤细胞和高效复制的病毒均对溶酶体功能提出极高需求。 本研究选择4-羟基苯甲醛作为母核,并引入一个氯原子和一条含有叔胺基团的4-(二乙氨基)丁氧基侧链。该侧链赋予化合物溶酶体靶向能力,因为叔胺在生理pH下仍可透过细胞膜,但在溶酶体酸性腔内发生质子化并被滞留,从而在溶酶体内蓄积,并通过中和酸性环境破坏溶酶体功能。

📋 英文结构化总结 English Structured Summary

全文整理

EN

Background:

Addressing clinical challenges such as the toxicity of conventional chemotherapy and viral drug resistance, this study proposes and validates an innovative “host organelle-targeting” strategy. Ewing sarcoma is a highly aggressive bone tumor predominantly affecting children and adolescents, molecularly characterized by fusion gene drivers such as EWSR1-FLI1, and current multimodal treatment shows limited efficacy against metastatic or recurrent disease due to broad toxicity, tumor heterogeneity, and acquired resistance. Coronaviruses, exemplified by porcine epidemic diarrhea virus (PEDV), rely heavily on the host cell’s endocytic-lysosomal system for entry and replication, revealing a biological parallel in which rapidly proliferating tumor cells and efficiently replicating viruses place exceptional demands on lysosomal function.

The study selected 4-hydroxybenzaldehyde as the parent core and introduced a chlorine atom and a 4-(diethylamino)butoxy side chain containing a tertiary amine group. This side chain confers lysosome-targeting capability because the tertiary amine remains membrane-permeable at physiological pH but becomes protonated and trapped within the acidic lumen of lysosomes, where it accumulates and disrupts lysosomal function by neutralizing the acidic environment.

Methods:

We rationally designed and synthesized 3-chloro-4-(4-(diethylamino)butoxy)benzaldehyde based on the pH-responsive property of the 4-(diethylamino)butoxy side chain. In vitro activity was evaluated against Ewing sarcoma cells (TC32, A673, RD-ES), prostate cancer bone metastasis model cells (PC3, DU145), porcine epidemic diarrhea virus (PEDV), and transmissible gastroenteritis virus (TGEV). Antiproliferative activity was assessed by CCK-8 assay, colony formation assay, Annexin V-FITC/PI flow cytometry, and JC-1 mitochondrial membrane potential staining.

Mechanistic investigations integrated transcriptomics, cellular functional assays, and organelle-level detection. RNA-seq was performed on TC32 cells, followed by KEGG pathway enrichment analysis and RT-qPCR validation of ER stress, p53 signaling, lysosome biogenesis, and cell cycle genes. Antiviral assays measured EC50, CC50, and selectivity index, one-step PEDV growth curves, and qRT-PCR of early IE1 and late VP1 genes. Lysosomal targeting was assessed by Galectin-3 immunofluorescence, cathepsin B/D activity, mRFP-GFP-LC3 autophagic flux analysis, LysoSensor lysosomal pH measurement, and subcellular fractionation with LC-MS/MS quantification.

Results:

Compound 3b showed the most potent antiproliferative activity among tested analogues, inhibiting TC32 cells with IC50 = 25 μM and PC3 cells with IC50 = 38 μM, and significantly suppressed replication of PEDV and TGEV. Colony formation in TC32 cells was reduced in a dose-dependent manner and almost completely inhibited at 200 μM. Treatment with 200 μM 3b induced an apoptotic rate of 33% in TC32 cells, compared with less than 4% in DMSO control, and decreased the JC-1 red/green fluorescence ratio from 3.1 in control to 1.2 at 200 μM.

Mechanistic studies revealed that 3b neutralizes lysosomal pH, impairs acidification, blocks autophagic flux, upregulates endoplasmic reticulum stress-related gene expression, activates the p53 signaling pathway, and inhibits the cell cycle, ultimately leading to apoptosis. RNA-seq identified significant enrichment of the p53 signaling pathway, endoplasmic reticulum protein processing, and apoptosis, with lysosomal pathway genes upregulated and cell cycle pathway suppressed. RT-qPCR showed CHOP and ATF4 elevated by 6.7-fold, p21 and PUMA upregulated by approximately 6-fold, TFEB, CTSB, and LAMP1 upregulated by 2.5- to 3-fold, and CCNB1 and CDK1 suppressed to about 30% of control. In PEDV infection, 3b specifically and strongly suppressed transcription of the late viral gene VP1 while exerting a lesser effect on the early gene IE1.

Lysosomal assays showed increased Galectin-3 puncta, enhanced cathepsin B/D activity, accumulation of yellow mRFP-GFP-LC3 puncta with low red puncta similar to chloroquine, and an increase in average lysosomal pH from 4.9 to 6.6. Subcellular fractionation showed 3b concentration in the lysosomal fraction was 8.3-fold higher than in the cytoplasmic fraction.

Data Summary:

Antiproliferative IC50 values for compound 3b were 25 ± 3 μM in TC32, 28 ± 5 μM in A673, 40 ± 5 μM in RD-ES, 38 ± 6 μM in PC3, and 48 ± 4 μM in DU145, whereas DEAB was >200 μM in all lines. Antiviral activity of 3b showed PEDV EC50 = 5 μM, CC50 = 301 μM, and SI = 60.2; TGEV EC50 = 155 μM, CC50 = 685 μM, and SI = 4.4. Compound 3d showed PEDV EC50 = 2 μM, CC50 = 10.8 μM, and SI = 5.4.

Functional and mechanistic measurements included 33% apoptosis at 200 μM versus <4% control, JC-1 red/green ratios of 3.1, 2.0, and 1.2 for control, 25 μM, and 200 μM, CHOP/ATF4 6.7-fold induction, p21/PUMA approximately 6-fold induction, TFEB/CTSB/LAMP1 2.5- to 3-fold induction, CCNB1/CDK1 reduced to about 30%, Galectin-3 puncta increasing from ~6 to ~39 in TC32 cells and from ~8 to ~42 in PEDV-infected Vero cells, cathepsin B/D activity increasing 2.7-fold and 3-fold, yellow mRFP-GFP-LC3 puncta increasing from 11 to 46, lysosomal pH increasing from 4.9 to 6.6, and lysosomal fraction concentration 8.3-fold higher than cytoplasmic fraction.

Conclusions:

This study reports a chemical entity with well-defined dual antitumor and antiviral activities and provides mechanistic evidence supporting the feasibility of the “host-lysosome targeting” strategy. Compound 3b achieves pH-gradient-dependent lysosomal accumulation through its 4-(diethylamino)butoxy side chain, and its intra-lysosomal sequestration neutralizes the acidic luminal environment, disrupts autophagic flux, elicits an integrated stress response, and induces cell-cycle arrest, thereby suppressing tumor cell proliferation and viral replication.

SAR analysis indicated that the tertiary amine-containing side chain is essential for lysosomal tropism, while chlorine substitution influences the therapeutic window; compound 3b achieved an optimal balance between efficacy and safety compared with compound 3d. The work offers multidimensional proof-of-concept for a novel broad-spectrum therapeutic paradigm centered on perturbing host cellular homeostasis.

Practical Significance:

The lysosome-targeting design provides a research framework for developing broad-spectrum host-directed therapies that can simultaneously address tumor proliferation and viral replication by targeting common host vulnerabilities. This approach may help overcome limitations of conventional chemotherapy and antiviral resistance, while the identified lead compound and mechanistic evidence support further development of dual-activity therapeutic agents.

📋 中文结构化总结 Chinese Structured Summary

中文

背景:

针对传统化疗的毒性和病毒耐药性等临床挑战,本研究提出并验证了一种创新的“宿主细胞器靶向”策略。尤文肉瘤是一种高度侵袭性的骨肿瘤,主要累及儿童和青少年,分子特征以EWSR1-FLI1等融合基因驱动为特点;由于广泛毒性、肿瘤异质性和获得性耐药,目前的多模式治疗对转移性或复发性疾病疗效有限。以猪流行性腹泻病毒(PEDV)为代表的冠状病毒高度依赖宿主细胞的内吞-溶酶体系统完成入侵和复制,这揭示了一种生物学平行关系:快速增殖的肿瘤细胞和高效复制的病毒均对溶酶体功能提出极高需求。

本研究选择4-羟基苯甲醛作为母核,并引入一个氯原子和一条含有叔胺基团的4-(二乙氨基)丁氧基侧链。该侧链赋予化合物溶酶体靶向能力,因为叔胺在生理pH下仍可透过细胞膜,但在溶酶体酸性腔内发生质子化并被滞留,从而在溶酶体内蓄积,并通过中和酸性环境破坏溶酶体功能。

方法:

我们基于4-(二乙氨基)丁氧基侧链的pH响应特性,合理设计并合成了3-氯-4-[4-(二乙氨基)丁氧基]苯甲醛。在体外活性方面,分别对尤文肉瘤细胞(TC32、A673、RD-ES)、前列腺癌骨转移模型细胞(PC3、DU145)、猪流行性腹泻病毒(PEDV)和传染性胃肠炎病毒(TGEV)进行了评价。抗增殖活性通过CCK-8实验、克隆形成实验、Annexin V-FITC/PI流式细胞术以及JC-1线粒体膜电位染色进行评估。

机制研究整合了转录组学、细胞功能实验和细胞器水平检测。对TC32细胞进行RNA-seq测序,随后开展KEGG通路富集分析,并通过RT-qPCR验证内质网应激、p53信号通路、溶酶体生物发生和细胞周期相关基因。抗病毒实验测定了EC50、CC50和选择性指数,绘制PEDV单步生长曲线,并对早期IE1基因和晚期VP1基因进行qRT-PCR检测。溶酶体靶向性通过Galectin-3免疫荧光、组织蛋白酶B/D活性、mRFP-GFP-LC3自噬流分析、LysoSensor溶酶体pH测定以及亚细胞分级分离联合LC-MS/MS定量进行评估。

结果:

在受试类似物中,化合物3b表现出最强的抗增殖活性,对TC32细胞的IC50为25 μM,对PC3细胞的IC50为38 μM,并显著抑制PEDV和TGEV的复制。TC32细胞的克隆形成随剂量增加而减少,在200 μM时几乎被完全抑制。200 μM 3b处理使TC32细胞凋亡率达到33%,而DMSO对照组低于4%;JC-1红/绿荧光比值由对照组的3.1降至200 μM处理组的1.2。

机制研究显示,3b可中和溶酶体pH、损害溶酶体酸化、阻断自噬流、上调内质网应激相关基因表达、激活p53信号通路并抑制细胞周期,最终诱导凋亡。RNA-seq结果显示p53信号通路、内质网蛋白质加工和凋亡通路显著富集,溶酶体通路基因上调,细胞周期通路受到抑制。RT-qPCR显示CHOP和ATF4上调6.7倍,p21和PUMA上调约6倍,TFEB、CTSB和LAMP1上调2.5至3倍,CCNB1和CDK1被抑制至对照的约30%。在PEDV感染中,3b特异性且强烈地抑制晚期病毒基因VP1的转录,而对早期基因IE1的影响较小。

溶酶体实验显示Galectin-3点状信号增加,组织蛋白酶B/D活性增强,黄色mRFP-GFP-LC3点状信号蓄积且红色点状信号较低,与氯喹处理相似;平均溶酶体pH由4.9升高至6.6。亚细胞分级分离显示,3b在溶酶体组分中的浓度比细胞质组分高8.3倍。

数据汇总:

化合物3b的抗增殖IC50值在TC32中为25 ± 3 μM,在A673中为28 ± 5 μM,在RD-ES中为40 ± 5 μM,在PC3中为38 ± 6 μM,在DU145中为48 ± 4 μM;而DEAB在所有细胞系中均>200 μM。3b的抗病毒活性显示:PEDV EC50 = 5 μM,CC50 = 301 μM,SI = 60.2;TGEV EC50 = 155 μM,CC50 = 685 μM,SI = 4.4。化合物3d对PEDV的EC50 = 2 μM,CC50 = 10.8 μM,SI = 5.4。

功能和机制测量包括:200 μM处理组凋亡率为33%,对照组<4%;JC-1红/绿比值在对照组、25 μM组和200 μM组分别为3.1、2.0和1.2;CHOP/ATF4诱导6.7倍;p21/PUMA诱导约6倍;TFEB/CTSB/LAMP1诱导2.5至3倍;CCNB1/CDK1降至约30%;Galectin-3点状信号在TC32细胞中由约6个增加至约39个,在PEDV感染的Vero细胞中由约8个增加至约42个;组织蛋白酶B/D活性分别增加2.7倍和3倍;黄色mRFP-GFP-LC3点状信号由11个增加至46个;溶酶体pH由4.9升高至6.6;溶酶体组分中浓度比细胞质组分高8.3倍。

结论:

本研究报道了一种具有明确抗肿瘤和抗病毒双重活性的化学实体,并提供了支持“宿主溶酶体靶向”策略可行性的机制证据。化合物3b通过其4-(二乙氨基)丁氧基侧链实现pH梯度依赖性溶酶体蓄积;其在溶酶体内的滞留中和酸性腔内环境,破坏自噬流,引发整合应激反应,并诱导细胞周期阻滞,从而抑制肿瘤细胞增殖和病毒复制。

构效关系分析表明,含叔胺侧链对溶酶体趋向性至关重要,而氯取代影响治疗窗;与化合物3d相比,化合物3b在疗效和安全性之间实现了更优的平衡。该工作为一种以扰动宿主细胞稳态为核心的新型广谱治疗范式提供了多维度概念验证。

实际意义:

溶酶体靶向设计为开发广谱宿主导向疗法提供了研究框架,该疗法可通过靶向共同宿主易感点同时应对肿瘤增殖和病毒复制。这一方法有助于克服传统化疗的局限性和抗病毒耐药问题,同时所鉴定的先导化合物及机制证据支持进一步开发具有双重活性的治疗药物。

📖 英文全文 English Full Text

EN

TYPE Original Research PUBLISHED 19 June 2026 DOI 10.3389/fchem.2026.1851116

Design of dual-effect molecules based on lysosome-targeting strategy: a mechanistic study on synergistic inhibition of ewing sarcoma and coronaviruses

Shimeng Zhou1*, Lu Xu2 and Wenlong Ge1 1Cangzhou Integrated Traditional Chinese and Western Medicine Hospital, Hebei Key Laboratory of

Integrated Traditional and Western Medicine in Osteoarthrosis Research (Preparing), Cangzhou, Hebei,

China, 2Cangzhou People’s Hospital, Cangzhou, Hebei, China

Introduction:

Addressing clinical challenges such as the toxicity of conventional chemotherapy and viral drug resistance, this study proposes and validates an innovative “host organelle-targeting” strategy. By disrupting the function of host lysosomes—an organelle commonly exploited by both tumors and viruses—we aim to develop novel therapeutic agents with dual antitumor and antiviral activity.

Methods: We rationally designed and synthesized the target compound 3- chloro-4-(4-(diethylamino)butoxy)benzaldehyde, whose core design relies on the pH-responsive property of the 4-(diethylamino)butoxy side chain to enable specific enrichment within the acidic lumen of lysosomes. In vitro activity was evaluated against Ewing sarcoma cells (TC32), prostate cancer bone metastasis model cells, porcine epidemic diarrhea virus (PEDV), and transmissible gastroenteritis virus (TGEV). Mechanistic investigations assessed lysosomal pH, autophagic flux, endoplasmic reticulum stress-related gene expression, p53 signaling pathway, cell cycle, and apoptosis.

Results: The compound potently inhibited the proliferation of TC32 cells (IC50 =

25 μM) and prostate cancer bone metastasis cells, and significantly suppressed the replication of PEDV and TGEV. Mechanistic studies revealed that the compound neutralizes lysosomal pH, impairs acidification, blocks autophagic flux, upregulates endoplasmic reticulum stress-related gene expression, activates the p53 signaling pathway, and inhibits the cell cycle, ultimately leading to apoptosis.

Conclusion: This study reports a chemical entity with well-defined dual antitumor and antiviral activities and provides mechanistic evidence supporting the feasibility of the “host-lysosome targeting” strategy. It thus offers an important proof-of- concept and a research framework for developing broad-spectrum host-directed therapies.

KEYWORDS antitumor, antiviral, dual activity, Hostorganelletargeting, Lysosometargeting

OPEN ACCESS EDITED BY Ahmed A. Al-Karmalawy, University of Mashreq, Iraq

REVIEWED BY Beom Jin Kim, University of Ulsan, Republic of Korea

Ning Yang, Louisiana State University Health Shreveport, United States

*CORRESPONDENCE Shimeng Zhou, m19331789399@163.com

RECEIVED 09 April 2026 REVISED 27 May 2026 ACCEPTED 04 June 2026

PUBLISHED 19 June 2026 CITATION Zhou S, Xu L and Ge W (2026) Design of dual-effect molecules based on lysosome-targeting strategy: a mechanistic study on synergistic inhibition of ewing sarcoma and coronaviruses.

Front. Chem. 14:1851116. doi: 10.3389/fchem.2026.1851116

COPYRIGHT © 2026 Zhou, Xu and Ge. 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.

Frontiers in Chemistry frontiersin.org 01 1 Introduction

In the context of interdisciplinary integration in biomedical sciences, orthopedic oncology is continuously incorporating new scientific perspectives to address persistent clinical challenges (Siegel et al., 2013; Watts et al., 2017). Ewing sarcoma, a highly aggressive bone tumor predominantly affecting children and adolescents, is molecularly characterized by fusion gene drivers such as EWSR1- FLI1 (Gartrell and Rodriguez-Galindo, 2021; Kim and Park, 2016). The current multimodal treatment, primarily based on intensive chemotherapy, surgery, and radiotherapy, shows limited efficacy against metastatic or recurrent disease. This therapeutic impasse largely stems from the broad toxicity of conventional chemotherapy, coupled with tumor heterogeneity and acquired resistance (De Las Rivas et al., 2021; Pan et al., 2021).

Consequently, there is an urgent need for agents with novel mechanisms of action. Ideally, such agents should circumvent existing resistance mechanisms or target more fundamental, common cellular processes essential for tumor cell survival (Buck et al., 2021; Daniyal et al., 2021). In parallel, the field of virology faces analogous challenges. Coronaviruses, exemplified by the porcine epidemic diarrhea virus (PEDV), rely heavily on the host cell’s endocytic-lysosomal system for entry and replication (Turlewicz- Podbielska and Pomorska-Mól, 2021; Wang et al., 2016). This reveals a profound biological parallel: both rapidly proliferating tumor cells and efficiently replicating viruses place exceptional demands on, and actively remodel, fundamental host cell resources and regulatory networks, such as lysosomal function.

Building on this, shifting the therapeutic strategy from the traditional “direct targeting of pathogens or oncoproteins” to

“targeting host factors that are commonly exploited by both tumors and viruses” has emerged as a promising direction (Ghimire et al., 2018; Zhou and Zhang, 2016). Among these, the lysosome—a cellular “digestion and recycling center” and signaling hub—may become vulnerable under the intense pressure imposed by rapid proliferation or viral hijacking, thereby representing a novel and potentially broad-spectrum intervention point (Perera and Zoncu,

2016; Yang and Wang, 2021). This leads to a core scientific hypothesis:

Can a small molecule be designed to specifically disrupt the function of this shared host organelle, the lysosome, thereby exerting a synergistic dual inhibitory effect on tumor cell proliferation and viral replication? Such a “host-directed” dual-activity molecule not only holds promise for overcoming the limitations of conventional therapies but may also reveal a fundamental cell biological principle.

To test this hypothesis, this study proposes and implements an innovative “host organelle targeting” drug design strategy. We selected 4-hydroxybenzaldehyde—a structurally simple and readily derivatizable scaffold—as the parent core and performed rational structural optimization by introducing key pharmacophores: a chlorine atom was introduced onto the benzene ring to modulate physicochemical properties, while a 4-(diethylamino)butoxy side chain containing a tertiary amine group was designed and incorporated. This side chain confers a unique “lysosome- targeting” capability: the tertiary amine group remains membrane- permeable at physiological pH but becomes protonated and trapped within the acidic lumen of the lysosome, where it accumulates and disrupts lysosomal function by neutralizing the acidic environment (Khan et al., 2018; Stewart et al., 2025).

We successfully synthesized the target compound 3-chloro-4-(4- (diethylamino)butoxy)benzaldehyde, aiming to systematically evaluate whether it could achieve the predicted “dual activity.”

For the antitumor assessment, we selected Ewing sarcoma (TC32,

A673, RD-ES) and prostate cancer bone metastasis model (PC3,

DU145) cell lines to evaluate its anti-proliferative activity. For the antiviral assessment, we employed PEDV and transmissible gastroenteritis virus (TGEV) infection models to measure its efficacy in inhibiting viral replication.

Furthermore, by integrating transcriptomics, cellular functional assays, and organelle-level detection, we deeply investigated the common molecular mechanism underlying its simultaneous antitumor and antiviral effects across multiple dimensions, including lysosomal acidification status, autophagic flux, endoplasmic reticulum stress, the p53 signaling pathway, and the cell cycle. This study not only reports a novel chemical entity with dual activity but also aims, through mechanism-driven exploration, to provide a proof-of- concept and a new framework for developing broad-spectrum therapeutic strategies based on “host organelle targeting.”

2 Results and discussion 2.1 Chemical synthesis Based on a “host organelle-targeting” strategy, we successfully designed and synthesized the compound

3-chloro-4-(4- (diethylamino)butoxy)benzaldehyde. This molecule utilizes 4- hydroxybenzaldehyde-readily derivatizable and possessing favorable membrane permeability—as its core scaffold. A chlorine atom was introduced at the para position of the benzene ring to modulate lipophilicity and potentially engage in halogen- bonding interactions. The central design feature is the incorporation of a 4-(diethylamino)butoxy side chain. The tertiary amine group within this chain remains uncharged and membrane-permeable at physiological pH but becomes protonated and positively charged in acidic compartments such as lysosomes, leading to its specific

“trapping” and accumulation within these organelles, thereby achieving pH gradient-dependent lysosomal targeting (Kroemer and Galluzzi, 2017; Liu et al., 2021). We hypothesized that the high intra-lysosomal concentration of this compound might disrupt lysosomal homeostasis via mechanisms such as compromising membrane integrity, neutralizing the acidic pH, or interfering with autophagic flux.

This dual perturbation could simultaneously affect the survival of tumor cells reliant on lysosomal function and the lifecycle of viruses dependent on lysosomes for entry. The specific synthetic route is illustrated in

Figure 1, starting from 4-hydroxybenzaldehyde, followed by the introduction of a linear carbon chain at the hydroxyl group, and subsequent reaction with the appropriate amine derivative to yield the final product 3.

2.2 Antiproliferative screening of compounds Guided by the innovative strategy of “targeting host organelles,” we first systematically evaluated the antiproliferative activity of novel compounds, designed based

Frontiers in Chemistry frontiersin.org 02 Zhou et al.

10.3389/fchem.2026.1851116 on the 4-hydroxybenzaldehyde scaffold, against two representative tumor models (Fu and Wang, 2023). Ewing sarcoma cell lines (TC32, A673, RD-ES) and prostate cancer bone metastasis model cell lines (PC3, DU145) were selected for assessment, with the parent core molecule and the weakly active

4-Diethylaminobenzaldehyde (DEAB) serving as references. Initial screening results demonstrated that the modified compounds exhibited significantly superior inhibitory activity compared to the reference agents (Table 1). Among them, the lead compound 3b showed the most potent activity against the

Ewing sarcoma TC32 cells (IC50 = 25 µM), representing an over 8- fold increase in potency compared to the parent core. Compound

3b also displayed strong and specific inhibition against prostate cancer PC3 cells (IC50 = 38 µM). Based on these findings, subsequent investigations were focused on the lead compound

3b to delve deeper into its antitumor mechanism.

FIGURE 1 Design and synthesis of 4-(diethylamino)butoxy derivative. Conditions and reagents: i) acetone, K2CO3, 50 °C, yield 70%–82%; ii) acetone, different aldehyde groups, 50 °C, yield 61%–80%.

TABLE 1 Antiproliferative effect of DEAB analogues on various cancer cell lines.

Compounds IC50 (μM M) R1 R2 TC32 A673 RD-ES PC3 DU145

DEAB — — >200 >200 >200 >200 >200 3a H 89 ± 4 70 ± 6

80 ± 5 76 ± 5 60 ± 3 3b Cl 25 ± 3 28 ± 5 40 ± 5 38 ± 6

48 ± 4 3c H 101 ± 6 28 ± 5 40 ± 5 38 ± 6 51 ± 4 3d

Cl 70 ± 6 37 ± 4 51 ± 6 50 ± 7 55 ± 3 Data are presented as mean ± SD from three independent experiments (n = 3).

FIGURE 2 (A) Statistical graph of the relative colony formation rate in TC32 cells; (B) Significant induction of apoptosis by compound 3b in TC32 cells; (C) JC-1 analysis of mitochondrial membrane potential. Data are presented as mean ± SEM from three independent experiments (n = 3). Compared with the

Control group, *P < 0.05, **P < 0.01, and ***P < 0.001.

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10.3389/fchem.2026.1851116 FIGURE 3 (A) Bar graph showing the significance of pathway enrichment. Key differentially expressed genes were validated according to functional modules. (B,C) Representative gene expression levels of the endoplasmic reticulum stress response, (D,E) the p53 signaling pathway, (F–H) lysosome biogenesis, and (I,J) cell cycle progression are shown. Data are presented as mean ± SEM from three independent experiments (n = 3). *p < 0.05, **p < 0.01, ***p <

0.001 compared with the Control group.

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10.3389/fchem.2026.1851116 2.3 Compound 3b inhibits TC32 cell proliferation and induces apoptosis

A colony formation assay was performed to evaluate the effect of compound 3b on TC32 cells at concentrations of 25, 50, 100, and

200 μM. As shown in Figure 2A, treatment with 3b at this concentration gradient significantly reduced the number of cell colonies in a dose-dependent manner. Colony formation was almost completely inhibited at the concentration of 200 μM.

Furthermore, analysis of apoptosis by flow cytometry indicated that treatment with 200 μM 3b induced an apoptotic rate of 33% in TC32 cells, whereas the proportion of apoptotic cells in the

DMSO control group was very low (less than 4%) (Figure 2B). The detailed distribution of live, early apoptotic, late apoptotic, and necrotic cells is provided in Supplementary Table S1. To further validate the apoptosis-inducing effect, we measured the mitochondrial membrane potential using the JC-1 probe. As shown in Figure 2C, compound 3b decreased the red/green fluorescence ratio in a concentration-dependent manner. The ratio decreased from 3.1 in the control group to 2.0 in the

25 μM group, and further to 1.2 in the 200 μM group. These results indicate that compound 3b causes a loss of mitochondrial membrane potential, an early event in the apoptotic cascade.

Collectively, these results demonstrate that compound 3b significantly inhibits the proliferation of TC32 cells.

2.4 Antitumor mechanism of the compound 3b KEGG pathway enrichment analysis revealed that the most significantly activated pathways upon compound 3b treatment (ranked by

FDR) included the p53 signaling pathway, endoplasmic reticulum protein processing, and apoptosis (FDR <0.001) (Figure 3A). Consistently, genes associated with the lysosomal pathway were also significantly upregulated (FDR <0.01). In contrast, the cell cycle pathway was markedly suppressed. To validate the RNA-seq data and further delineate the action profile of compound 3b, we performed quantitative analysis of hallmark genes in these key pathways (Figures 3B,C).

Within the ER stress pathway, compound 3b treatment elevated the expression levels of CHOP and ATF4 by 6.7-fold (p < 0.001), an induction comparable to that elicited by BafA1 treatment (ns).

Similarly, in the p53 signaling pathway, its downstream effectors p21 and PUMA were robustly upregulated by approximately 6-fold (p < 0.001) (Figures 3D,E). Notably, the expression of TFEB—the master transcriptional regulator of lysosomal biogenesis—and its target genes CTSB and LAMP1 exhibited a consistent and significant co-upregulation (2.5- to 3-fold, p < 0.001) (Figures 3F–H), indicating the activation of a transcriptional reprogramming likely aimed at compensating for lysosomal functional impairment. In sharp contrast, the expression of key drivers of cell cycle progression, CCNB1 and CDK1, was significantly suppressed to about 30% of the control level (p < 0.001) (Figures

3I,J). It should be noted that these findings are based on transcriptional analysis; protein-level validation of ER stress markers (e.g., ATF4 and CHOP) was not performed in this study. For all genes examined, no statistically significant differences were observed between the compound 3b- and

BafA1-treated groups, confirming at the transcriptional level that both treatments triggered highly similar, widespread cellular stress and growth arrest responses by disrupting lysosomal function.

2.5 Initial screening of antiviral activity To verify the potential broad-spectrum antiviral activity of the compounds designed based on the host-lysosome-targeting strategy, we evaluated their efficacy against porcine epidemic diarrhea virus (PEDV) and transmissible gastroenteritis virus (TGEV) (Yang et al.,

2017). As shown in Table 2, the compound 3b exhibited significant inhibitory activity against both PEDV and TGEV at non-cytotoxic concentrations, effectively reducing viral replication markers.

Specifically, compound 3b exhibited a CC50 of 301 μM in normal

Vero cells, which was approximately 12-fold higher than its IC50 in

TC32 cancer cells (25 μM), indicating a favorable therapeutic window with preferential cytotoxicity toward tumor cells. The half-maximal effective concentration (EC50) fell within a range similar to that observed for its antitumor activity. These parallel activity data indicate that the biological effect of the compound 3b is not confined to tumor cells but extends to viral infections that also critically depend on lysosomal function. Therefore, the results in this section not only independently confirm the definite antiviral efficacy of the compound, but more importantly, they effectively link the

“lysosomal perturbation” mechanism previously established in tumor models to a new pathological context—viral infection.

This strongly supports our core hypothesis that by targeting the host lysosome as a common cellular hub, 3b can simultaneously exert dual antitumor and antiviral effects, thereby providing key experimental evidence for the development of a broad-spectrum, host-directed therapeutic strategy.

2.6 3b inhibits late-stage viral gene transcription

To assess the effect of compound 3b on PEDV replication, we measured the time-course changes in viral titer in infected cells treated with the compound. Vero cells were pretreated with compound 3b or DMSO control and then infected with PEDV at the same multiplicity of infection (MOI). Virus-containing supernatants were collected at various time points post-infection (0, 6, 12, 24, 36, 44, and 52 h), and viral titers were determined by the

TCID50 assay. The one-step growth curve (Figure 4A) showed that

PEDV could still complete a full replication cycle in the presence of the compound. After a latent period of approximately 6 h post- infection, the viral titer rose sharply, entering the exponential phase and peaking at 44 h (7.33 Log10 TCID50), followed by a plateau phase. Subsequent qPCR results (Figures 4B,C) revealed that compound

3b specifically and strongly suppressed the transcription of the late viral gene (VP1), while exerting a lesser effect on the early gene (IE1). We therefore conclude that compound

3b disrupts the host cellular environment required for viral replication, particularly during the late stage.

2.7 Targeting lysosomes To quantitatively assess the effect of the compound 3b on the autophagy process, we measured both the number of puncta of the

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10.3389/fchem.2026.1851116 autolysosome marker Galectin-3 and the activity of key lysosomal enzymes.

First, quantitative analysis of Galectin-3 immunofluorescence (Figures 5A,B) showed that compound 3b treatment significantly increased the average number of Galectin- 3 puncta per cell compared with the respective solvent control (DMSO) in both TC32 cells and PEDV-infected Vero cells (from

~6 to ~39 puncta/cell in TC32 cells, and from ~8 to ~42 puncta/cell in PEDV-infected Vero cells). This indicates that the compound 3b effectively induced the accumulation of Galectin-3-positive structures. To further investigate the functional status of lysosomes downstream of autophagy, we detected the activity of cytosolic cathepsin B/D. As shown in Figures 5C,D, compound 3b treatment also markedly enhanced the relative fluorescent activity of cathepsins in both cell models. When the activity of each control group was set as 1, compound 3b treatment increased the enzymatic activity to 2.7-fold and 3-fold, respectively (*p < 0.001). Together, these quantitative data demonstrate that the compound 3b not only promotes the formation of autolysosome-related structures but is also accompanied by enhanced lysosomal degradative activity. To clarify the effect of the compound 3b on autophagic flux, we performed quantitative analysis of cells labeled with the mRFP- GFP-LC3 probe. As shown in Figure 5E, compared with the DMSO control, treatment with the autophagy inducer Torin1 dramatically increased the number of red puncta (41 vs. 7), while yellow puncta showed only a moderate increase, consistent with successful activation and completion of autophagic flux. In contrast, treatment with the lysosomal inhibitor chloroquine (CQ) exhibited a distinctly different pattern: yellow puncta accumulated sharply (52 vs. 11), whereas red puncta were suppressed. Importantly, our compound 3b treatment completely reproduced this characteristic pattern of CQ: it similarly induced a pronounced accumulation of yellow puncta (46 vs. 11) and kept the number of red puncta at a low level, showing no statistical difference from the CQ group and being significantly lower than the Torin1- treated group. These quantitative data indicate that the compound

3b does not promote smooth autophagic flux but, similar to CQ, causes accumulation of autophagosomes (yellow puncta) and a reduction in autolysosome (red puncta) formation, strongly suggesting that autophagic flux is blocked at the lysosomal degradation stage. MThe acidic environment of lysosomes is a prerequisite for their degradative function. To directly investigate whether the compound 3b affects lysosomal acidification, we

TABLE 2 Antiviral activity of DEAB analogues against PEDV and TGEV.

Compounds PEDV EC50 a (μM M) PEDV CC50 b (μM M) PEDV SIc

TGEV EC50 (μM M) TGEV CC50 (μM M) TGEV SI DEAB >200

>200 — >200 >200 — 3a 72 603 8.4 >200 >200 — 3b 5 301

60.2 155 685 4.4 3c >200 >200 — >200 >200 — 3d 2 10.8

5.4 187 895 4.8 Data are presented as mean ± SD, from three independent experiments (n = 3). aEC50 = 50% effective concentration (concentration at which 50% inhibition of TGEV, or PEDV, are observed). bCC50 = 50% cytostatic/cytotoxic concentration (concentration at which 50% adverse effect is observed on the host cell). cSI: selectivity index (CC50/EC50).

FIGURE 4 (A) One-step growth curve of PEDV in the presence of compound 3b. (B) Relative mRNA expression levels of the viral early gene (IE1), measured by qRT-PCR at 12 h post-infection in cells pretreated with compound 3b or DMSO and infected with PEDV. (C) Relative mRNA expression levels of the viral late gene (VP1), measured by qRT-PCR at 24 h post-infection. Data are presented as mean ± SEM from three independent experiments (n = 3). Compared with control, *p < 0.05, **p < 0.01, ***p < 0.001.

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10.3389/fchem.2026.1851116 employed the pH-sensitive fluorescent probe LysoSensor for detection. As shown in Figure 5F, in DMSO-treated control cells, lysosomes displayed bright punctate fluorescent signals, indicating that their lumen maintained strong acidity. Quantitative analysis confirmed that compound 3b treatment significantly raised the average lysosomal pH from 4.9 in the control group to 6.6. This result directly proves that the compound 3b effectively disrupts the acidic environment of lysosomes. Together with the previous findings—that compound 3b treatment elevated cathepsin activity and that autophagic flux was blocked at the lysosomal stage (mRFP- GFP-LC3 assay)—we conclude that the compound 3b neutralizes the intra-lysosomal acidity, impairing its essential biochemical and degradative functions, thereby preventing the completion of autophagic flux.

2.8 Subcellular fractionation directly validates lysosomal targeting

To directly verify the lysosomal localization of compound 3b, organelle fractions were isolated by Percoll density gradient centrifugation and analyzed by LC-MS/MS. The results showed that the concentration of 3b in the lysosomal fraction was 8.3-fold higher than that in the cytoplasmic fraction (Figure 6). These findings directly demonstrate that 3b undergoes specific lysosomal accumulation via the ion-trapping mechanism.

3 Conclusion and discussion This study successfully translated the therapeutic concept of

“host organelle targeting” into a defined chemical entity with dual biological activities. A systematic structure-activity relationship (SAR) analysis revealed that each structural component contributes distinctively to the overall pharmacological profile.

The tertiary amine-containing 4-(diethylamino)butoxy side chain is essential for lysosomal tropism, enabling pH-gradient-dependent accumulation within acidic organelles. The chlorine atom on the benzene ring modulates lipophilicity and may facilitate halogen- bonding interactions with putative targets, but its substitution pattern critically influences the therapeutic window: while compound 3d exhibited the most potent anti-PEDV activity (EC50 = 2 µM), its high cytotoxicity (CC50 = 10.8 µM) yielded a poor selectivity index (SI = 5.4); in contrast, compound 3b achieved an optimal balance between efficacy and safety (EC50 = 5 μM, CC50 =

FIGURE 5 (A,B) Analysis of Galectin-3 immunofluorescent puncta. (A) TC32 cells and (B) PEDV-infected Vero cells were treated with DMSO or compound 3b (50 µM, 24 h), followed by immunofluorescence staining for Galectin-3. (C,D) Measurement of cytosolic cathepsin B/D activity. (C) TC32 cells and (D)

PEDV-infected Vero cells were treated under the same conditions as in (A,B). Cytosolic protein fractions were isolated, and their enzymatic activity was determined using a cathepsin B/D-specific fluorescent substrate. (E) Analysis of autophagic flux using the mRFP-GFP-LC3 tandem fluorescent probe. The average numbers of yellow and red puncta per cell were quantified. (F) Quantitative analysis of intralysosomal pH. Lysosomal pH was quantified using the pH-sensitive fluorescent probe LysoSensor Yellow/Blue. Data are presented as fold change relative to the DMSO control group. Data are presented as mean ± SEM from three independent experiments (n = 3). Compared with control, *p < 0.05, **p < 0.01, ***p < 0.001.

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10.3389/fchem.2026.1851116 301 μM, SI = 60.2), suggesting that moderate lysosomal accumulation with reduced off-target toxicity is preferable. The aldehyde moiety may also contribute as a weak electrophile, potentially engaging in reversible covalent interactions with lysosomal proteins.

By virtue of its rationally designed 4-(diethylamino)butoxy side chain, 3-chloro-4-(4-(diethylamino)butoxy)benzaldehyde achieves pH-gradient-dependent targeting and accumulation in lysosomes.

Its intra-lysosomal sequestration, which neutralizes the acidic luminal environment, acts as the initial trigger for the subsequent cascade of cellular events. Ultimately, this action disrupts autophagic flux, elicits an integrated stress response, and induces cell-cycle arrest, thereby synergistically suppressing both tumor cell proliferation and viral replication—processes that are highly dependent on functional lysosomes. Notably, we observed shared early organelle-dysfunction phenotypes and similar downstream signaling activation in two distinct pathological models (tumor and viral infection), providing strong support for the inherent logic of targeting common host vulnerabilities. Therefore, this work not only identifies a promising lead compound, but more importantly, offers multidimensional proof-of-concept—from chemical design to biological mechanism and pharmacological outcome—for a novel broad-spectrum therapeutic paradigm centered on perturbing host cellular homeostasis. From a pharmaceutical perspective, we acknowledge that the tertiary amine functionality present in compound 3d may pose potential risks related to the formation of genotoxic impurities such as nitrosamines during synthesis or storage. In the current study,

HPLC purity analysis (>95%) did not reveal any significant peaks corresponding to such impurities. For future development, comprehensive impurity profiling and risk assessment in accordance with ICH M7 guidelines will be essential to ensure safety.

4 Experimental section 4.1 Chemical synthesis Under a nitrogen atmosphere, compound 1 (1 mmol) was dissolved in 10 mL of anhydrous acetone containing potassium carbonate (3 mmol). 1,4-Dibromobutane (3 mmol) was then added, and the mixture was heated under reflux for 6 h. After the reaction was confirmed to be complete by TLC monitoring, the solvent was removed under reduced pressure. The crude product was purified by silica gel column chromatography to afford compound 2.

Subsequently, compound 2 (1 mmol) was dissolved in 10 mL of anhydrous acetone. Diethylamine (0.5 mL) was added, and the reaction was stirred at 50 °C for 6 h. Upon completion, the mixture was washed twice with brine. The organic layer was dried, and the solvent was evaporated under reduced pressure.

Purification by column chromatography yielded compound 3a as a pale-yellow solid (145 mg, yield: 61%). Compounds 3b–3d were isolated using a similar procedure. The 1H and 13C NMR spectra and data of the compound are provided in the Supporting Information.

4.2 Screening for antiproliferative activity of compounds

The antiproliferative activity of the compounds was evaluated using the CCK-8 assay. Cells of TC32, A673, RD-ES, PC3, and

DU145 lines in the logarithmic growth phase were seeded into 96- well plates. After 24 h of incubation to allow cell adherence, the culture medium was replaced with fresh medium containing a series of concentrations of the test compounds (novel

4- hydroxybenzaldehyde derivatives, the parent core molecule, and

DEAB), with solvent controls included. The cells were then cultured for an additional 48 h. Following this treatment, CCK-8 solution was added to each well. After an appropriate incubation period, the absorbance of each well was measured at 450 nm using a microplate reader. Cell viability rates were calculated based on the absorbance readings, and the half-maximal inhibitory concentration (IC50) values for each compound were determined by fitting the data to a nonlinear regression model. Based on the preliminary screening results, compound 3b was selected for further investigation into its mechanism of action (Amrutha Nisthul et al., 2021; Chripkova et al., 2016).

4.3 Colony formation assay TC32 cells in the logarithmic growth phase were seeded into 6- well plates. Following cell attachment, the cultures were treated with complete medium containing 25, 50, 100, and 200 μM of compound

3b, respectively, with a DMSO solvent control group established in parallel. The compound-containing medium was replenished every

3 d. The cells were cultured for 10–14 d until distinct colonies formed in the control group. Subsequently, the culture was terminated. The medium was aspirated, and the cells were washed with PBS, fixed with 4% paraformaldehyde, and stained with 0.1% crystal violet. After air-drying, the plates were photographed, and the number of colonies in each group was counted (Liu et al., 2015; Rong et al., 2008).

FIGURE 6 Distribution of compound 3b in lysosomal and cytoplasmic fractions. Data are presented as mean ± SEM from three independent experiments (n = 3).

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10.3389/fchem.2026.1851116 4.4 Detection of cell apoptosis

TC32 cells were seeded into 6-well plates and cultured until reaching approximately 70% confluency. The culture medium was then replaced with fresh medium containing 200 μM of compound

3b; a parallel control group was treated with an equivalent concentration of DMSO. After 24 h of treatment, both the culture supernatant and the adherent cells were collected. The cells were subsequently stained using an Annexin V-FITC/PI apoptosis detection kit, following the manufacturer’s instructions, and incubated at room temperature in the dark for 15 min.

Apoptotic cell populations, including early and late apoptotic cells, were then analyzed by flow cytometry (Liu et al., 2015;

Rong et al., 2008).

4.5 Bioinformatics analysis Total RNA was extracted from TC32 cells treated with compound 3b and control cells. Strand-specific libraries were constructed and subjected to high-throughput sequencing on an

Illumina platform (RNA-seq). The raw sequencing reads were aligned to the reference genome using Hisat2, and gene expression was quantified with featureCounts. Differentially expressed genes (DEGs) were identified with the thresholds of

|fold change| > 2 and adjusted p-value (FDR) < 0.05. The list of

DEGs was then subjected to KEGG pathway enrichment analysis using tools such as KOBAS. The significance of enrichment was calculated by the hypergeometric test, and the p-values were adjusted for multiple testing using the Benjamini–Hochberg method to control the false discovery rate (FDR). Pathways with an FDR < 0.05 were considered significantly enriched (Huang et al., 2018; Zolfaghari Emameh et al., 2022).

4.6 RT-qPCR validation To validate the reliability of the RNA-seq data, quantitative analysis was performed on marker genes from key pathways.

TC32 cells from the control group, compound 3b-treated group, and the positive control (BafA1)-treated group were collected. Total

RNA was extracted using TRIzol reagent, and its concentration and purity were measured. An equal amount of RNA was reverse- transcribed into first-strand cDNA using a reverse transcription kit. Specific primers were designed with software such as Primer

Premier 5.0 and synthesized commercially. GAPDH or β-actin was used as the internal reference gene. Amplification was carried out with SYBR Green Master Mix on a real-time PCR instrument under the following cycling conditions: 95 °C for 5 min; followed by

40 cycles of 95 °C for 10 s and 60 °C for 30 s. Each sample was run in triplicate, and a no-template control was included in each run.

The relative expression levels of the target genes were calculated using the 2−ΔΔCT method. The experiment was independently repeated three times (Huang et al., 2018; Zolfaghari Emameh et al., 2022).

4.7 Antiviral activity screening assay Cytotoxicity Assay of Compounds (CC50): To evaluate compound cytotoxicity, host cells (Vero E6) were seeded into 96- well plates. After adherence, the culture medium was replaced with medium containing a series of concentrations of the test compounds, and the cells were incubated for 48–72 h. Cell viability was measured using the CCK-8 assay. The half-maximal cytotoxic concentration (CC50) was calculated by fitting the dose- response curve.

Antiviral Activity Assay of Compounds (EC50): To assess the inhibitory activity of compounds on viral replication, porcine epidemic diarrhea virus (PEDV) or transmissible gastroenteritis virus (TGEV) was simultaneously added with a series of compound concentrations to a monolayer of cells in 96-well plates. After co-cultivation for a specified period, the level of viral replication was evaluated by observing the cytopathic effect (CPE) or detecting virus-specific antigen expression. The viral inhibition rate at each concentration was calculated, and the half- maximal effective concentration (EC50) was derived by curve fitting.

Calculation of Selectivity Index: The selectivity index (SI), representing the therapeutic window for each compound against the respective virus in vitro, was calculated using the formula: SI =

CC50/EC50. All experiments were independently repeated at least three times (Bhattacharya et al., 2021; Salata et al., 2017).

4.8 One-step growth curve assay To evaluate the effect of compound 3b on the replication kinetics of PEDV, a one-step viral growth curve assay was performed. Briefly, Vero cells were pretreated with a specified concentration of compound 3b or an equal volume of DMSO (control) for a predetermined duration. Subsequently, the cells were infected with PEDV at the same multiplicity of infection (MOI). Cell culture supernatants were collected at various time points post-infection (0, 6, 12, 24, 36, 44, and 52 h). The viral titers in all samples were determined using the 50% tissue culture infectious dose (TCID50) assay on Vero cells and expressed as Log10 TCID50/ mL (Bhattacharya et al., 2021; Salata et al., 2017).

4.9 Quantitative PCR (qPCR) detection of viral gene transcription

To analyze the effect of compound 3b on the transcription of viral genes at different stages, quantitative real-time PCR (qRT- PCR) was performed. Vero cells were pretreated with compound 3b or DMSO and then infected with PEDV at a consistent multiplicity of infection (MOI). Cells were harvested at 12 and 24 h post- infection, and total RNA was extracted. Subsequently, qRT-PCR was used to specifically detect the mRNA levels of the viral early gene (IE1) and the late gene (VP1). The relative expression of each gene was calculated using the 2−ΔΔCt method and expressed as fold change relative to the DMSO control group (Ma et al., 2020).

4.10 Galectin-3 immunofluorescence staining analysis

TC32 cells or PEDV-infected Vero cells were seeded into confocal dishes and treated with DMSO and compound 3b for the indicated duration. After treatment, the cells were fixed, permeabilized, and blocked. Subsequently, the cells were incubated with a primary antibody against Galectin-3, followed

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10.3389/fchem.2026.1851116 by incubation with an appropriate fluorescent secondary antibody.

Nuclei were counterstained with DAPI. Images were captured randomly under a confocal microscope, and the number of fluorescent puncta per cell was quantified (Fritsch et al., 2016).

4.11 Cathepsin B/D activity assay TC32 cells or PEDV-infected Vero cells subjected to identical treatments were collected and lysed to extract cytosolic proteins. Equal amounts of protein were then incubated with specific fluorescent substrates for Cathepsin B or Cathepsin D under light-protected conditions. The relative enzymatic activity was determined by measuring the fluorescence intensity using a microplate reader at an excitation wavelength of 400 nm and an emission wavelength of

505 nm (Mehanna et al., 2016; Yu et al., 2014).

4.12 mRFP-GFP-LC3 autophagic flux analysis Cells stably expressing the mRFP-GFP-LC3 tandem fluorescent probe were seeded into confocal dishes. They were then treated with

DMSO (control), compound 3b, the autophagy inducer Torin1, or the lysosomal inhibitor chloroquine (CQ). Following treatment, the cells were observed and imaged under a confocal microscope.

Yellow puncta (mRFP+GFP+) represented autophagosomes, while red puncta (mRRP+GFP−) represented autolysosomes. The puncta were counted, and the average number per cell was calculated for each condition (Bonavita et al., 2025).

4.13 Determination of lysosomal lumen pH Lysosomal pH was measured using the LysoSensor Yellow/Blue staining reagent. Treated cells were incubated with the probe, washed, and then observed under a fluorescence microscope.

Quantification was performed using the dual-emission wavelength ratio (Ex/Em: 335/440 nm) characteristic of this probe. The fluorescence ratio was converted to specific pH values based on a standard calibration curve (Ponsford et al., 2021; Xia et al., 2021).

4.14 Subcellular fractionation and LC-MS/ MS quantification

TC32 cells were treated with 25 μmol/L compound 3b or DMSO (control) for 6 h. Cells were collected and resuspended in homogenization buffer (0.25 mol/L sucrose, 10 mmol/L HEPES- NaOH, pH 7.2) and disrupted using a Dounce homogenizer. Crude lysosomal fractions were enriched by differential centrifugation, followed by Percoll density gradient centrifugation at 70,000 g for 40 min to purify lysosomes. Fractions were collected, proteins were precipitated with acetonitrile, and compound

3b concentrations were quantified by LC-MS/MS and normalized to protein content. Three independent replicates were performed.

4.15 JC-1 staining for mitochondrial membrane potential

TC32 cells were treated with DMSO, 25 μM compound 3b or

200 μM compound 3b for 6 h. Cells were collected, washed once with

PBS, and resuspended in JC-1 working solution prepared according to the manufacturer’s protocol. After incubation at 37 °C for 20 min in the dark, cells were washed twice with cold JC-1 staining buffer and resuspended in 500 μL of staining buffer. Fluorescence was immediately measured using a flow cytometer with 488 nm excitation. Green fluorescence (JC-1 monomer) was detected in the FITC channel (530 nm), and red fluorescence (JC-1 aggregates) was detected in the PE channel (590 nm). The red/green fluorescence ratio was calculated to indicate mitochondrial membrane potential. Data were analyzed from three independent experiments (n = 3).

4.16 Statistical analysis The above results are presented as the mean ± SEM (Standard

Error of the Mean) from three independent experiments. Statistical analysis was performed using SPSS 21.0 software, and differences between groups were assessed by one-way analysis of variance (ANOVA).

Data availability statement The original contributions presented in the study are included in the article/Supplementary Material, further inquiries can be directed to the corresponding author.

Author contributions SZ: Data curation, Writing – original draft, Visualization,

Methodology, Validation, Investigation, Conceptualization,

Writing – review and editing, Supervision, Software. LX:

Writing – review and editing, Validation, Supervision, Software,

Visualization, Funding acquisition, Resources. WG: Funding acquisition, Data curation, Methodology, Writing – review and editing, Formal Analysis.

Funding The author(s) declared that financial support was not received for this work and/or its publication.

Conflict of interest The author(s) declared that this work was conducted in the absence of any commercial or financial relationships that could be construed as a potential conflict of interest.

Generative AI statement The author(s) declared that generative AI was not used in the creation of this manuscript.

Any alternative text (alt text) provided alongside figures in this article has been generated by Frontiers with the support of artificial

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10.3389/fchem.2026.1851116 intelligence and reasonable efforts have been made to ensure accuracy, including review by the authors wherever possible. If you identify any issues, please contact us.

Publisher’s note All claims expressed in this article are solely those of the authors and do not necessarily represent those of their affiliated organizations, or those of the publisher, the editors and the reviewers. Any product that may be evaluated in this article, or claim that may be made by its manufacturer, is not guaranteed or endorsed by the publisher.

Supplementary material The Supplementary Material for this article can be found online at: https://www.frontiersin.org/articles/10.3389/fchem.2026.

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Frontiers in Chemistry frontiersin.org 11 Zhou et al.

10.3389/fchem.2026.1851116

📖 中文全文 Chinese Full Text

中文

以下为中文译文(保留原文结构、表格、图注及关键技术术语):

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**类型**:原创研究 **发表日期**:2026年6月19日 **DOI**:10.3389/fchem.2026.1851116

**基于溶酶体靶向策略的双效分子设计:对尤文肉瘤和冠状病毒协同抑制的机制研究** Shimeng Zhou¹*、Lu Xu² 和 Wenlong Ge¹

¹ 沧州市中西医结合医院,河北省骨关节炎中西医结合研究重点实验室(筹),中国河北沧州; ² 沧州市人民医院,中国河北沧州

**引言:** 针对传统化疗毒性、病毒耐药等临床挑战,本研究提出并验证了一种创新的“宿主细胞器靶向”策略。通过破坏宿主溶酶体的功能——溶酶体是肿瘤和病毒共同利用的细胞器——我们旨在开发具有双重抗肿瘤和抗病毒活性的新型治疗药物。

**方法:** 我们合理设计并合成了目标化合物 3-氯-4-(4-(二乙氨基)丁氧基)苯甲醛,其核心设计依赖于 4-(二乙氨基)丁氧基侧链的 pH 响应特性,使其能够在溶酶体酸性腔内特异性富集。体外活性评估对象包括尤文肉瘤细胞(TC32)、前列腺癌骨转移模型细胞、猪流行性腹泻病毒(PEDV)和传染性胃肠炎病毒(TGEV)。机制研究评估了溶酶体 pH、自噬流、内质网应激相关基因表达、p53 信号通路、细胞周期和凋亡。

**结果:** 该化合物强效抑制 TC32 细胞(IC₅₀ = 25 μM)和前列腺癌骨转移细胞增殖,并显著抑制 PEDV 和 TGEV 复制。机制研究表明,该化合物中和溶酶体 pH、损害酸化、阻断自噬流、上调内质网应激相关基因表达、激活 p53 信号通路并抑制细胞周期,最终导致凋亡。

**结论:** 本研究报道了一种具有明确双重抗肿瘤和抗病毒活性的化学实体,并为“宿主溶酶体靶向”策略的可行性提供了机制证据。因此,它为开发广谱宿主导向疗法提供了重要的概念验证和研究框架。

**关键词** 抗肿瘤、抗病毒、双重活性、宿主细胞器靶向、溶酶体靶向

**开放获取**

**编辑** Ahmed A. Al-Karmalawy,伊拉克马什雷克大学

**审稿人** Beom Jin Kim,韩国蔚山大学 Ning Yang,美国路易斯安那州立大学健康什里夫波特分校

**通讯作者** Shimeng Zhou,m19331789399@163.com

**收稿日期**:2026年4月9日 **修回日期**:2026年5月27日 **接受日期**:2026年6月4日 **发表日期**:2026年6月19日

**引用格式** Zhou S, Xu L and Ge W (2026) Design of dual-effect molecules based on lysosome-targeting strategy: a mechanistic study on synergistic inhibition of ewing sarcoma and coronaviruses. *Front. Chem.* 14:1851116. doi: 10.3389/fchem.2026.1851116

**版权** © 2026 Zhou, Xu and Ge。本文为开放获取文章,依据知识共享署名许可(CC BY)条款发布。允许在其他平台使用、分发或复制,但须按照学术惯例注明原作者和版权所有者,并引用本文在本期刊中的原始发表。任何不符合上述条款的使用、分发或复制均不被允许。

*Frontiers in Chemistry* frontiersin.org 01

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## 1 引言

在生物医学科学跨学科融合的背景下,骨肿瘤学正不断引入新的科学视角,以应对持续存在的临床挑战(Siegel 等,2013;Watts 等,2017)。尤文肉瘤是一种高度侵袭性的骨肿瘤,主要累及儿童和青少年,其分子特征包括 EWSR1-FLI1 等融合基因驱动(Gartrell 和 Rodriguez-Galindo,2021;Kim 和 Park,2016)。目前以强化化疗、手术和放疗为主的多模式治疗,对转移性或复发性疾病疗效有限。这一治疗困境主要源于传统化疗的广泛毒性,以及肿瘤异质性和获得性耐药(De Las Rivas 等,2021;Pan 等,2021)。因此,迫切需要具有新作用机制的药物。理想情况下,这类药物应绕过现有耐药机制,或靶向对肿瘤细胞存活更为根本、更普遍的细胞过程(Buck 等,2021;Daniyal 等,2021)。与此同时,病毒学领域也面临类似挑战。以猪流行性腹泻病毒(PEDV)为代表的冠状病毒,高度依赖宿主细胞的内吞—溶酶体系统完成入侵和复制(Turlewicz-Podbielska 和 Pomorska-Mól,2021;Wang 等,2016)。这揭示了一个深刻的生物学平行关系:快速增殖的肿瘤细胞和高效复制的病毒,都会对宿主细胞的基本资源和调控网络——例如溶酶体功能——施加异常压力,并主动重塑这些网络。

基于此,将治疗策略从传统的“直接靶向病原体或癌蛋白”转向“靶向肿瘤和病毒共同利用的宿主因子”,已成为一个有前景的方向(Ghimire 等,2018;Zhou 和 Zhang,2016)。其中,溶酶体作为细胞“消化与回收中心”和信号枢纽,在快速增殖或病毒劫持造成的强烈压力下可能变得脆弱,从而成为一个新颖且可能具有广谱性的干预位点(Perera 和 Zoncu,2016;Yang 和 Wang,2021)。由此引出一个核心科学假说:能否设计一种小分子,特异性破坏这一共同宿主细胞器——溶酶体——的功能,从而对肿瘤细胞增殖和病毒复制产生协同的双重抑制作用?这种“宿主导向”的双重活性分子不仅有望克服传统疗法的局限,还可能揭示一个基本的细胞生物学原理。为检验这一假说,本研究提出并实施了一种创新的“宿主细胞器靶向”药物设计策略。我们选择 4-羟基苯甲醛——一种结构简洁且易于衍生化的骨架——作为母核,并通过引入关键药效团进行合理的结构优化:在苯环上引入氯原子以调节理化性质,同时设计并引入含有叔胺基团的 4-(二乙氨基)丁氧基侧链。该侧链赋予分子独特的“溶酶体靶向”能力:叔胺基团在生理 pH 下保持膜通透性,但在溶酶体酸性腔内发生质子化并被截留,从而在溶酶体内蓄积,并通过中和酸性环境破坏溶酶体功能(Khan 等,2018;Stewart 等,2025)。

我们成功合成了目标化合物 3-氯-4-(4-(二乙氨基)丁氧基)苯甲醛,旨在系统评估其是否能实现预期的“双重活性”。在抗肿瘤评估中,我们选择尤文肉瘤细胞系(TC32、A673、RD-ES)和前列腺癌骨转移模型细胞系(PC3、DU145)评估其抗增殖活性。在抗病毒评估中,我们采用 PEDV 和传染性胃肠炎病毒(TGEV)感染模型,测定其抑制病毒复制的效力。此外,通过整合转录组学、细胞功能实验和细胞器水平检测,我们从多个维度深入探究其同时发挥抗肿瘤和抗病毒作用的共同分子机制,包括溶酶体酸化状态、自噬流、内质网应激、p53 信号通路和细胞周期。本研究不仅报道了一种具有双重活性的新型化学实体,还旨在通过机制驱动探索,为基于“宿主细胞器靶向”的广谱治疗策略开发提供概念验证和新框架。

## 2 结果与讨论

### 2.1 化学合成

基于“宿主细胞器靶向”策略,我们成功设计并合成了化合物 3-氯-4-(4-(二乙氨基)丁氧基)苯甲醛。该分子以 4-羟基苯甲醛为核心骨架,该骨架易于衍生化且具有较好的膜通透性。在苯环对位引入氯原子,以调节脂溶性并可能参与卤键相互作用。核心设计特征是引入 4-(二乙氨基)丁氧基侧链。该侧链中的叔胺基团在生理 pH 下不带电荷且可透过膜,但在溶酶体等酸性区室中质子化并带正电荷,从而在这些细胞器内发生特异性“截留”和蓄积,实现 pH 梯度依赖的溶酶体靶向(Kroemer 和 Galluzzi,2017;Liu 等,2021)。我们假设,该化合物在溶酶体内的高浓度可能通过损害膜完整性、中和酸性 pH 或干扰自噬流等机制破坏溶酶体稳态。这种双重扰动可能同时影响依赖溶酶体功能存活的肿瘤细胞和依赖溶酶体完成入侵的病毒生命周期。具体合成路线见图 1:以 4-羟基苯甲醛为起始原料,先在羟基上引入直链碳链,随后与相应胺衍生物反应,得到最终产物 3。

### 2.2 化合物抗增殖筛选

在“靶向宿主细胞器”这一创新策略指导下,我们首先系统评估了基于 4-羟基苯甲醛骨架设计的新化合物对两种代表性肿瘤模型的抗增殖活性(Fu 和 Wang,2023)。评估对象包括尤文肉瘤细胞系(TC32、A673、RD-ES)和前列腺癌骨转移模型细胞系(PC3、DU145),并以母核分子和活性较弱的 4-二乙氨基苯甲醛(DEAB)作为参照。初步筛选结果显示,修饰化合物的抑制活性显著优于参照化合物(表 1)。其中,先导化合物 3b 对尤文肉瘤 TC32 细胞表现出最强活性(IC₅₀ = 25 μM),其效力较母核提高 8 倍以上。化合物 3b 还对前列腺癌 PC3 细胞表现出强效且特异性的抑制作用(IC₅₀ = 38 μM)。基于上述发现,后续研究聚焦于先导化合物 3b,以深入探究其抗肿瘤机制。

**图 1** 4-(二乙氨基)丁氧基衍生物的设计与合成。条件与试剂:i) 丙酮,K₂CO₃,50 °C,产率 70%–82%;ii) 丙酮,不同醛基,50 °C,产率 61%–80%。

**表 1** DEAB 类似物对多种癌细胞系的抗增殖作用。

| 化合物 | R₁ | R₂ | IC₅₀(μM)TC32 | A673 | RD-ES | PC3 | DU145 | |---|---|---|---|---|---|---|---| | DEAB | — | — | >200 | >200 | >200 | >200 | >200 | | 3a | H | | 89 ± 4 | 70 ± 6 | 80 ± 5 | 76 ± 5 | 60 ± 3 | | 3b | Cl | | 25 ± 3 | 28 ± 5 | 40 ± 5 | 38 ± 6 | 48 ± 4 | | 3c | H | | 101 ± 6 | 28 ± 5 | 40 ± 5 | 38 ± 6 | 51 ± 4 | | 3d | Cl | | 70 ± 6 | 37 ± 4 | 51 ± 6 | 50 ± 7 | 55 ± 3 |

数据以三次独立实验(n = 3)的均值 ± 标准差表示。

**图 2** (A) TC32 细胞相对集落形成率统计图;(B) 化合物 3b 在 TC32 细胞中显著诱导凋亡;(C) JC-1 分析线粒体膜电位。数据以三次独立实验(n = 3)的均值 ± 标准误表示。与对照组相比,*P < 0.05,**P < 0.01,***P < 0.001。

*Frontiers in Chemistry* frontiersin.org 02 Zhou 等 10.3389/fchem.2026.1851116

**图 3** (A) 通路富集显著性柱状图。根据功能模块对关键差异表达基因进行验证。(B、C) 内质网应激反应代表性基因表达水平;(D、E) p53 信号通路;(F–H) 溶酶体生物发生;(I、J) 细胞周期进程。数据以三次独立实验(n = 3)的均值 ± 标准误表示。与对照组相比,*p < 0.05,**p < 0.01,***p < 0.001。

*Frontiers in Chemistry* frontiersin.org 03 Zhou 等 10.3389/fchem.2026.1851116

### 2.3 化合物 3b 抑制 TC32 细胞增殖并诱导凋亡

我们进行集落形成实验,评估化合物 3b 在 25、50、100 和 200 μM 浓度下对 TC32 细胞的作用。如图 2A 所示,在该浓度梯度下,3b 处理以剂量依赖方式显著减少细胞集落数量。在 200 μM 浓度下,集落形成几乎被完全抑制。此外,流式细胞术凋亡分析显示,200 μM 3b 处理诱导 TC32 细胞凋亡率为 33%,而 DMSO 对照组凋亡细胞比例很低(低于 4%)(图 2B)。活细胞、早期凋亡细胞、晚期凋亡细胞和坏死细胞的详细分布见补充表 S1。为进一步验证诱导凋亡作用,我们使用 JC-1 探针测定线粒体膜电位。如图 2C 所示,化合物 3b 以浓度依赖方式降低红/绿荧光比值。该比值从对照组的 3.1 降至 25 μM 组的 2.0,并进一步降至 200 μM 组的 1.2。这些结果表明,化合物 3b 导致线粒体膜电位丧失,这是凋亡级联反应的早期事件。综上,这些结果证明化合物 3b 显著抑制 TC32 细胞增殖。

### 2.4 化合物 3b 的抗肿瘤机制

KEGG 通路富集分析显示,化合物 3b 处理后最显著激活的通路(按 FDR 排序)包括 p53 信号通路、内质网蛋白加工和凋亡(FDR < 0.001)(图 3A)。与此一致,溶酶体通路相关基因也显著上调(FDR < 0.01)。相反,细胞周期通路被显著抑制。为验证 RNA-seq 数据并进一步界定化合物 3b 的作用谱,我们对这些关键通路中的标志基因进行了定量分析(图 3B、C)。在内质网应激通路中,化合物 3b 处理使 CHOP 和 ATF4 表达水平升高 6.7 倍(p < 0.001),其诱导程度与 BafA1 处理相当(ns)。类似地,在 p53 信号通路中,其下游效应分子 p21 和 PUMA 被显著上调约 6 倍(p < 0.001)(图 3D、E)。值得注意的是,溶酶体生物发生的主转录调控因子 TFEB 及其靶基因 CTSB 和 LAMP1 的表达呈现一致且显著的协同上调(2.5–3 倍,p < 0.001)(图 3F–H),提示可能发生了旨在代偿溶酶体功能受损的转录重编程。与之形成鲜明对比的是,细胞周期进程关键驱动因子 CCNB1 和 CDK1 的表达被显著抑制至对照水平的约 30%(p < 0.001)(图 3I、J)。需要指出的是,上述发现基于转录水平分析;本研究未对内质网应激标志物(如 ATF4 和 CHOP)进行蛋白水平验证。对所有检测基因而言,化合物 3b 处理组与 BafA1 处理组之间未观察到统计学显著差异,从而在转录水平上证实两种处理均通过破坏溶酶体功能触发了高度相似、广泛的细胞应激和生长停滞反应。

### 2.5 抗病毒活性初步筛选

为验证基于宿主溶酶体靶向策略设计的化合物是否具有潜在广谱抗病毒活性,我们评估了其对猪流行性腹泻病毒(PEDV)和传染性胃肠炎病毒(TGEV)的效力(Yang 等,2017)。如表 2 所示,化合物 3b 在非细胞毒性浓度下对 PEDV 和 TGEV 均表现出显著抑制活性,有效降低病毒复制标志物。具体而言,化合物 3b 在正常 Vero 细胞中的 CC₅₀ 为 301 μM,约为其在 TC32 癌细胞中 IC₅₀(25 μM)的 12 倍,表明其具有有利的治疗窗口,且对肿瘤细胞具有优先细胞毒性。半数有效浓度(EC₅₀)处于与其抗肿瘤活性相似的范围。这些平行活性数据表明,化合物 3b 的生物学效应不仅限于肿瘤细胞,还延伸至同样高度依赖溶酶体功能的病毒感染。因此,本节结果不仅独立证实了该化合物明确的抗病毒效力,更重要的是,将先前在肿瘤模型中确立的“溶酶体扰动”机制有效联系到新的病理背景——病毒感染。这有力支持了我们的核心假说:通过靶向宿主溶酶体这一共同细胞枢纽,3b 可同时发挥双重抗肿瘤和抗病毒作用,从而为开发广谱宿主导向治疗策略提供了关键实验证据。

### 2.6 3b 抑制病毒晚期基因转录

为评估化合物 3b 对 PEDV 复制的影响,我们测定了化合物处理感染细胞中病毒滴度的时间变化。Vero 细胞先用化合物 3b 或 DMSO 对照预处理,随后以相同感染复数(MOI)感染 PEDV。在感染后不同时间点(0、6、12、24、36、44 和 52 h)收集含病毒上清,并通过 TCID₅₀ 法测定病毒滴度。单步生长曲线(图 4A)显示,在化合物存在下,PEDV 仍能完成完整复制周期。感染后约 6 h 的潜伏期后,病毒滴度急剧上升,进入指数期,并在 44 h 达到峰值(7.33 Log₁₀ TCID₅₀),随后进入平台期。后续 qPCR 结果(图 4B、C)显示,化合物 3b 特异性且强效抑制晚期病毒基因(VP1)转录,而对早期基因(IE1)影响较小。因此,我们得出结论:化合物 3b 破坏病毒复制所需的宿主细胞环境,尤其是在晚期阶段。

### 2.7 靶向溶酶体

为定量评估化合物 3b 对自噬过程的影响,我们同时测定了自噬溶酶体标志物 Galectin-3 的斑点数量和关键溶酶体酶活性。首先,Galectin-3 免疫荧光定量分析(图 5A、B)显示,与各自溶剂对照(DMSO)相比,化合物 3b 处理显著增加 TC32 细胞和 PEDV 感染 Vero 细胞中每个细胞的 Galectin-3 斑点平均数量(TC32 细胞中从约 6 个/细胞增至约 39 个/细胞;PEDV 感染 Vero 细胞中从约 8 个/细胞增至约 42 个/细胞)。这表明化合物 3b 有效诱导 Galectin-3 阳性结构蓄积。为进一步研究自噬下游溶酶体的功能状态,我们检测了胞质组织蛋白酶 B/D 活性。如图 5C、D 所示,化合物 3b 处理还显著增强两种细胞模型中组织蛋白酶的相对荧光活性。当每组对照活性设为 1 时,化合物 3b 处理分别将酶活性提高至 2.7 倍和 3 倍(*p < 0.001)。综上,这些定量数据表明,化合物 3b 不仅促进自噬溶酶体相关结构形成,还伴随溶酶体降解活性增强。为明确化合物 3b 对自噬流的影响,我们对使用 mRFP-GFP-LC3 探针标记的细胞进行定量分析。如图 5E 所示,与 DMSO 对照相比,自噬诱导剂 Torin1 处理显著增加红色斑点数量(41 对 7),而黄色斑点仅中度增加,与自噬流成功激活并完成一致。相反,溶酶体抑制剂氯喹(CQ)处理呈现明显不同模式:黄色斑点急剧蓄积(52 对 11),而红色斑点被抑制。重要的是,我们的化合物 3b 处理完全重现了 CQ 的特征性模式:同样诱导黄色斑点显著蓄积(46 对 11),并使红色斑点数量保持在低水平,与 CQ 组无统计学差异,且显著低于 Torin1 处理组。这些定量数据表明,化合物 3b 并不促进自噬流顺畅进行,而是类似 CQ,导致自噬体(黄色斑点)蓄积和自噬溶酶体(红色斑点)形成减少,强烈提示自噬流在溶酶体降解阶段被阻断。溶酶体的酸性环境是其降解功能的前提。为直接探究化合物 3b 是否影响溶酶体酸化,我们采用 pH 敏感荧光探针 LysoSensor 进行检测。如图 5F 所示,在 DMSO 处理对照细胞中,溶酶体显示明亮点状荧光信号,表明其腔内维持强酸性。定量分析证实,化合物 3b 处理将平均溶酶体 pH 从对照组的 4.9 显著升高至 6.6。该结果直接证明化合物 3b 有效破坏溶酶体酸性环境。结合先前发现——化合物 3b 处理升高组织蛋白酶活性,且自噬流在溶酶体阶段被阻断(mRFP-GFP-LC3 实验)——我们得出结论:化合物 3b 中和溶酶体腔内酸性,损害其基本生化与降解功能,从而阻止自噬流完成。

**表 2** DEAB 类似物对 PEDV 和 TGEV 的抗病毒活性。

| 化合物 | PEDV EC₅₀ᵃ(μM) | PEDV CC₅₀ᵇ(μM) | PEDV SIᶜ | TGEV EC₅₀(μM) | TGEV CC₅₀(μM) | TGEV SI | |---|---:|---:|---:|---:|---:|---:| | DEAB | >200 | >200 | — | >200 | >200 | — | | 3a | 72 | 603 | 8.4 | >200 | >200 | — | | 3b | 5 | 301 | 60.2 | 155 | 685 | 4.4 | | 3c | >200 | >200 | — | >200 | >200 | — | | 3d | 2 | 10.8 | 5.4 | 187 | 895 | 4.8 |

数据以三次独立实验(n = 3)的均值 ± 标准差表示。 ᵃ EC₅₀ = 50% 有效浓度(观察到 50% TGEV 或 PEDV 抑制的浓度)。 ᵇ CC₅₀ = 50% 细胞生长抑制/细胞毒性浓度(观察到宿主细胞 50% 不良效应的浓度)。 ᶜ SI:选择性指数(CC₅₀/EC₅₀)。

**图 4** (A) 化合物 3b 存在下 PEDV 的单步生长曲线。(B) 通过 qRT-PCR 测定经化合物 3b 或 DMSO 预处理并感染 PEDV 的细胞在感染后 12 h 的病毒早期基因(IE1)相对 mRNA 表达水平。(C) 通过 qRT-PCR 测定感染后 24 h 的病毒晚期基因(VP1)相对 mRNA 表达水平。数据以三次独立实验(n = 3)的均值 ± 标准误表示。与对照组相比,*p < 0.05,**p < 0.01,***p < 0.001。

*Frontiers in Chemistry* frontiersin.org 04 Zhou 等 10.3389/fchem.2026.1851116

### 2.8 亚细胞分级直接验证溶酶体靶向

为直接验证化合物 3b 的溶酶体定位,我们通过 Percoll 密度梯度离心分离细胞器分级,并用 LC-MS/MS 分析。结果显示,溶酶体分级中 3b 的浓度是胞质分级的 8.3 倍(图 6)。这些发现直接证明 3b 通过离子捕获机制发生特异性溶酶体蓄积。

## 3 结论与讨论

本研究成功将“宿主细胞器靶向”的治疗概念转化为具有双重生物活性的明确化学实体。系统构效关系(SAR)分析表明,每个结构组分对整体药理学特征均有独特贡献。含叔胺的 4-(二乙氨基)丁氧基侧链对溶酶体趋向性至关重要,使其能够在酸性细胞器内实现 pH 梯度依赖的蓄积。苯环上的氯原子调节脂溶性,并可能促进与潜在靶点的卤键相互作用,但其取代模式对治疗窗口有重要影响:化合物 3d 表现出最强的抗 PEDV 活性(EC₅₀ = 2 μM),但其高细胞毒性(CC₅₀ = 10.8 μM)导致选择性指数较差(SI = 5.4);相比之下,化合物 3b 在效力与安全性之间达到最佳平衡(EC₅₀ = 5 μM,CC₅₀ = 301 μM,SI = 60.2),提示适度溶酶体蓄积并降低脱靶毒性更为可取。醛基也可能作为弱亲电基团发挥作用,可能与溶酶体蛋白发生可逆共价相互作用。

凭借其合理设计的 4-(二乙氨基)丁氧基侧链,3-氯-4-(4-(二乙氨基)丁氧基)苯甲醛实现了对溶酶体的 pH 梯度依赖靶向和蓄积。其在溶酶体内的截留中和酸性腔内环境,作为后续细胞事件级联反应的初始触发因素。最终,这一作用破坏自噬流,引发整合应激反应,并诱导细胞周期停滞,从而协同抑制高度依赖功能性溶酶体的肿瘤细胞增殖和病毒复制。值得注意的是,我们在两种不同病理模型(肿瘤和病毒感染)中观察到共同的早期细胞器功能障碍表型和相似的下游信号激活,这为靶向共同宿主脆弱性的内在逻辑提供了有力支持。因此,本研究不仅鉴定了一个有前景的先导化合物,更重要的是,从化学设计到生物机制和药理学结果,为以扰动宿主细胞稳态为核心的新型广谱治疗范式提供了多维度概念验证。从药学角度看,我们承认化合物 3d 中存在的叔胺功能基团可能在合成或储存过程中带来亚硝胺等遗传毒性杂质的潜在风险。在本研究中,HPLC 纯度分析(>95%)未发现与该类杂质相对应的显著峰。对于未来开发,按照 ICH M7 指南进行全面杂质谱分析和风险评估将是确保安全所必需的。

**图 5** (A、B) Galectin-3 免疫荧光斑点分析。(A) TC32 细胞和 (B) PEDV 感染 Vero 细胞经 DMSO 或化合物 3b(50 μM,24 h)处理后,进行 Galectin-3 免疫荧光染色。(C、D) 胞质组织蛋白酶 B/D 活性测定。(C) TC32 细胞和 (D) PEDV 感染 Vero 细胞在 (A、B) 相同条件下处理。分离胞质蛋白分级,并使用组织蛋白酶 B/D 特异性荧光底物测定酶活性。(E) 使用 mRFP-GFP-LC3 串联荧光探针分析自噬流。定量每个细胞黄色和红色斑点的平均数量。(F) 溶酶体腔内 pH 定量分析。使用 pH 敏感荧光探针 LysoSensor Yellow/Blue 定量溶酶体 pH。数据以相对于 DMSO 对照组的倍数变化表示。数据以三次独立实验(n = 3)的均值 ± 标准误表示。与对照组相比,*p < 0.05,**p < 0.01,***p < 0.001。

**图 6** 化合物 3b 在溶酶体分级和胞质分级中的分布。数据以三次独立实验(n = 3)的均值 ± 标准误表示。

*Frontiers in Chemistry* frontiersin.org 05 Zhou 等 10.3389/fchem.2026.1851116

## 4 实验部分

### 4.1 化学合成

在氮气氛围下,将化合物 1(1 mmol)溶解于含碳酸钾(3 mmol)的 10 mL 无水丙酮中。随后加入 1,4-二溴丁烷(3 mmol),混合物加热回流 6 h。经 TLC 监测确认反应完成后,减压除去溶剂。粗产物经硅胶柱层析纯化,得到化合物 2。随后,将化合物 2(1 mmol)溶解于 10 mL 无水丙酮中。加入二乙胺(0.5 mL),反应在 50 °C 下搅拌 6 h。反应完成后,混合物用盐水洗涤两次。有机层干燥,减压蒸发溶剂。柱层析纯化后得到化合物 3a,为淡黄色固体(145 mg,产率:61%)。化合物 3b–3d 采用类似方法分离。该化合物的 ¹H 和 ¹³C NMR 谱图及数据见支持信息。

### 4.2 化合物抗增殖活性筛选

采用 CCK-8 法评估化合物的抗增殖活性。将处于对数生长期的 TC32、A673、RD-ES、PC3 和 DU145 细胞接种于 96 孔板中。培养 24 h 使细胞贴壁后,将培养基更换为含一系列浓度受试化合物(新型 4-羟基苯甲醛衍生物、母核分子和 DEAB)的新鲜培养基,并设置溶剂对照。随后继续培养 48 h。处理后,向每孔加入 CCK-8 溶液。经适当孵育后,使用酶标仪在 450 nm 处测定每孔吸光度。根据吸光度读数计算细胞存活率,并通过将数据拟合至非线性回归模型确定各化合物的半数抑制浓度(IC₅₀)。基于初步筛选结果,选择化合物 3b 进一步研究其作用机制(Amrutha Nisthul 等,2021;Chripkova 等,2016)。

### 4.3 集落形成实验

将处于对数生长期的 TC32 细胞接种于 6 孔板中。细胞贴壁后,分别用含 25、50、100 和 200 μM 化合物 3b 的完全培养基处理,并平行设置 DMSO 溶剂对照组。每 3 天更换含化合物培养基。培养 10–14 天,直至对照组形成明显集落。随后终止培养,吸去培养基,用 PBS 洗涤细胞,4% 多聚甲醛固定,0.1% 结晶紫染色。干燥后拍照,并计数每组集落数量(Liu 等,2015;Rong 等,2008)。

### 4.4 细胞凋亡检测

将 TC32 细胞接种于 6 孔板中,培养至约 70% 汇合度。随后将培养基更换为含 200 μM 化合物 3b 的新鲜培养基;平行对照组用等浓度 DMSO 处理。处理 24 h 后,收集培养上清和贴壁细胞。随后按照说明书使用 Annexin V-FITC/PI 凋亡检测试剂盒对细胞染色,室温避光孵育 15 min。然后通过流式细胞术分析凋亡细胞群体,包括早期和晚期凋亡细胞(Liu 等,2015;Rong 等,2008)。

### 4.5 生物信息学分析

提取化合物 3b 处理组和对照组 TC32 细胞的总 RNA。构建链特异性文库,并在 Illumina 平台上进行高通量测序(RNA-seq)。使用 Hisat2 将原始测序 reads 比对至参考基因组,并使用 featureCounts 进行基因表达定量。差异表达基因(DEGs)的筛选阈值为 |fold change| > 2 且校正 p 值(FDR)< 0.05。随后使用 KOBAS 等工具对 DEG 列表进行 KEGG 通路富集分析。富集显著性通过超几何检验计算,并使用 Benjamini–Hochberg 方法对 p 值进行多重检验校正以控制错误发现率(FDR)。FDR < 0.05 的通路被认为显著富集(Huang 等,2018;Zolfaghari Emameh 等,2022)。

### 4.6 RT-qPCR 验证

为验证 RNA-seq 数据的可靠性,对关键通路中的标志基因进行定量分析。收集对照组、化合物 3b 处理组和阳性对照(BafA1)处理组 TC32 细胞。使用 TRIzol 试剂提取总 RNA,并测定其浓度和纯度。使用逆转录试剂盒将等量 RNA 逆转录为第一链 cDNA。使用 Primer Premier 5.0 等软件设计特异性引物,并商业合成。GAPDH 或 β-actin 作为内参基因。使用 SYBR Green Master Mix 在实时 PCR 仪上进行扩增,循环条件如下:95 °C 5 min;随后 40 个循环,每循环 95 °C 10 s,60 °C 30 s。每个样品设三个复孔,并在每次运行中加入无模板对照。使用 2⁻ΔΔCt 法计算靶基因相对表达水平。实验独立重复三次(Huang 等,2018;Zolfaghari Emameh 等,2022)。

### 4.7 抗病毒活性筛选实验

**化合物细胞毒性实验(CC₅₀)**:为评估化合物细胞毒性,将宿主细胞(Vero E6)接种于 96 孔板中。贴壁后,将培养基更换为含一系列浓度受试化合物的培养基,细胞孵育 48–72 h。使用 CCK-8 法测定细胞存活率。通过拟合剂量—反应曲线计算半数细胞毒性浓度(CC₅₀)。

**化合物抗病毒活性实验(EC₅₀)**:为评估化合物对病毒复制的抑制活性,将猪流行性腹泻病毒(PEDV)或传染性胃肠炎病毒(TGEV)与一系列化合物浓度同时加入 96 孔板中的单层细胞中。共培养规定时间后,通过观察细胞病变效应(CPE)或检测病毒特异性抗原表达来评估病毒复制水平。计算各浓度下的病毒抑制率,并通过曲线拟合推导半数有效浓度(EC₅₀)。

**选择性指数计算**:选择性指数(SI)代表每种化合物在体外对相应病毒的治疗窗口,计算公式为:SI = CC₅₀/EC₅₀。所有实验至少独立重复三次(Bhattacharya 等,2021;Salata 等,2017)。

### 4.8 单步生长曲线实验

为评估化合物 3b 对 PEDV 复制动力学的影响,进行单步病毒生长曲线实验。简要步骤如下:Vero 细胞先用规定浓度化合物 3b 或等体积 DMSO(对照)预处理预定时间。随后,以相同感染复数(MOI)感染 PEDV。在感染后不同时间点(0、6、12、24、36、44 和 52 h)收集细胞培养上清。所有样品中的病毒滴度均使用 Vero 细胞进行 50% 组织培养感染剂量(TCID₅₀)法测定,并以 Log₁₀ TCID₅₀/mL 表示(Bhattacharya 等,2021;Salata 等,2017)。

### 4.9 病毒基因转录的定量 PCR(qPCR)检测

为分析化合物 3b 对不同阶段病毒基因转录的影响,进行定量实时 PCR(qRT-PCR)。Vero 细胞先用化合物 3b 或 DMSO 预处理,随后以一致感染复数(MOI)感染 PEDV。在感染后 12 和 24 h 收集细胞,提取总 RNA。随后使用 qRT-PCR 特异性检测病毒早期基因(IE1)和晚期基因(VP1)的 mRNA 水平。使用 2⁻ΔΔCt 法计算每个基因的相对表达,并以相对于 DMSO 对照组的倍数变化表示(Ma 等,2020)。

### 4.10 Galectin-3 免疫荧光染色分析

将 TC32 细胞或 PEDV 感染 Vero 细胞接种于共聚焦培养皿中,并用 DMSO 和化合物 3b 处理规定时间。处理后,细胞固定、透化和封闭。随后,细胞与抗 Galectin-3 一抗孵育,再与相应荧光二抗孵育。细胞核用 DAPI 复染。在共聚焦显微镜下随机采集图像,并定量每个细胞的荧光斑点数量(Fritsch 等,2016)。

### 4.11 组织蛋白酶 B/D 活性实验

收集接受相同处理的 TC32 细胞或 PEDV 感染 Vero 细胞,裂解并提取胞质蛋白。将等量蛋白与组织蛋白酶 B 或组织蛋白酶 D 的特异性荧光底物在避光条件下孵育。使用酶标仪在激发波长 400 nm、发射波长 505 nm 处测定荧光强度,以确定相对酶活性(Mehanna 等,2016;Yu 等,2014)。

### 4.12 mRFP-GFP-LC3 自噬流分析

将稳定表达 mRFP-GFP-LC3 串联荧光探针的细胞接种于共聚焦培养皿中。随后用 DMSO(对照)、化合物 3b、自噬诱导剂 Torin1 或溶酶体抑制剂氯喹(CQ)处理。处理后,在共聚焦显微镜下观察并成像。黄色斑点(mRFP⁺GFP⁺)代表自噬体,红色斑点(mRFP⁺GFP⁻)代表自噬溶酶体。计数斑点,并计算每种条件下每个细胞的平均数量(Bonavita 等,2025)。

### 4.13 溶酶体腔 pH 测定

使用 LysoSensor Yellow/Blue 染色试剂测定溶酶体 pH。处理细胞与探针孵育,洗涤后在荧光显微镜下观察。使用该探针特征性的双发射波长比值(Ex/Em:335/440 nm)进行定量。基于标准校准曲线将荧光比值转换为特定 pH 值(Ponsford 等,2021;Xia 等,2021)。

### 4.14 亚细胞分级和 LC-MS/MS 定量

TC32 细胞用 25 μmol/L 化合物 3b 或 DMSO(对照)处理 6 h。收集细胞并重悬于匀浆缓冲液(0.25 mol/L 蔗糖,10 mmol/L HEPES-NaOH,pH 7.2)中,使用 Dounce 匀浆器破碎。通过差速离心富集粗溶酶体分级,随后以 70,000 g 进行 Percoll 密度梯度离心 40 min 以纯化溶酶体。收集分级,用乙腈沉淀蛋白,并通过 LC-MS/MS 定量化合物 3b 浓度,按蛋白含量归一化。进行三个独立重复。

### 4.15 JC-1 染色检测线粒体膜电位

TC32 细胞分别用 DMSO、25 μM 化合物 3b 或 200 μM 化合物 3b 处理 6 h。收集细胞,用 PBS 洗涤一次,重悬于按厂家方案配制的 JC-1 工作液中。37 °C 避光孵育 20 min 后,用冷 JC-1 染色缓冲液洗涤两次,并重悬于 500 μL 染色缓冲液中。立即使用流式细胞仪以 488 nm 激发测定荧光。绿色荧光(JC-1 单体)在 FITC 通道(530 nm)检测,红色荧光(JC-1 聚集体)在 PE 通道(590 nm)检测。计算红/绿荧光比值以指示线粒体膜电位。数据来自三次独立实验(n = 3)。

### 4.16 统计分析

上述结果以三次独立实验的均值 ± 标准误(SEM)表示。使用 SPSS 21.0 软件进行统计分析,组间差异采用单因素方差分析(ANOVA)评估。

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