| 姚奕然,吕广云,黄赛燕,等.基于 UPLC-MRM-IDA-EPI法筛查保健品中 50种非法添加的化学药物[J].安徽医药,2025,29(10):1967-1975. |
| 基于 UPLC-MRM-IDA-EPI法筛查保健品中 50种非法添加的化学药物 |
| High-throughput monitoring of 50 illegally added chemical drugs from health food by UPLC-MRM-IDA-EPI |
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| DOI：10.3969/j.issn.1009-6469.2025.10.011 |
| 中文关键词: 食品污染 色谱法，高压液相 串联质谱法 非法添加 保健品 高通量 数据库筛查 |
| 英文关键词: Food contamination Chromatography, high pressure liquid Tandem mass spectrometry Illegally adding Health food High-throughput monitoring Data base screening |
| 基金项目:南通市科技基金项目( JC12022053) |
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| 摘要点击次数: 41 |
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| 中文摘要: |
| 目的基于超高效液相色谱 -多反应监测信息依赖型 -增强子离子扫描( UPLC-MRM-IDA-EPI)技术，建立保健品中 50种非法添加化学药物的增强子离子( EPI)碎片数据库及快速定性定量方法。方法 2023年 1月至 2024年 1月以 Phenomenex ki-netex C18(100×3.0 mm，2.6 μm)为色谱柱， 0.1%甲酸水溶液( A)-乙腈( B)为流动相进行梯度洗脱。采用电喷雾离子源( ESI)同时扫描正负离子，利用 UPLC-MRM-IDA-EPI技术建立对照品的 EPI信息库；将待测样本中化合物 EPI碎片信息与 EPI信息库进行对比定性，同时完成定量分析。结果该研究成功建立了 50种化学药物的 MS/MS谱库和定性定量方法。定量分析的线性范围宽，高浓度组待测物在 64~6 400 μg/L线性关系良好，低浓度组待测物在 16~1 600 μg/L线性关系良好， r值均大于 0.99；收率结果在 60%~117%，检出限在 0.1~3.0 mg/kg，定量限在 0.3~10.0 mg/kg。应用该方法在 12批送检的样本中检出 4批非法添回加了化学药物。结论该研究建立的分析方法操作简单、专属性强，适用于在无对照品情况下快速筛查保健品中非法添加的 50种化学药物。 |
| 英文摘要: |
| Objective To establish an EPI fragment database and a rapid qualitative and quantitative method for 50 illeagally addedchemical drugs in health supplements based on ultra-performance liquid chromatography -multi-reaction monitoring information-de-pendent form -enhancer ion scanning (UPLC-MRM-IDA-EPI).Methods The samples were analyzed through a Phenomenex kinetexC18 (100×3.0 mm, 2.6 μm) column with 0.1% formic acid water solution (A) and acetonitrile (B) as the mobile phase by gradient elu-tion. The electrospray ionization (ESI) was used to simultaneously scan both positive and negative ions, and the EPI information data-base of the reference substances was established by using the UPLC-MRM-IDA-EPI technology. The EPI fragment information of thecompounds in the test samples was compared with the EPI information database for qualitative analysis, and quantitative analysis wasalso completed. Results The study successfully established MS/MS database and qualitative/quantitative method for 50 chemicaldrugs. The linear range of quantitative analysis was wide, and the measured substances in the high concentration were in the range of64-6 400 μg/L, showing a good linear relationship, and the measured substances in the low concentration group were in the range of 16-1 600 μg/L, showing a good linear relationship (all r > 0.99). The recovery rates ranged from 60% to 117%. The LOD was in the range of 0.1-3.0 mg/kg. The LOQ was in the range of 0.3-10.0 mg/kg. This method was used to detect 12 batches of samples and 4 batches of illegally added chemical drugs were found. Conclusion The analytical method established in this study is easy to operate and hasstrong specificity, and is suitable for rapid screening of 50 illeagally added chemical drugs in health supplements in the absence of ref-erence substances. |
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