彭名军，林子豪，曾豪威，周庆琼，钱振杰，曾 羲^*，戚 平^*

（广州市食品检验所，广东广州 511400）

摘要：建立超高效液相色谱-串联质谱法（UPLC-MS/MS）负离子模式测定保健品中氢氯噻嗪的分析方法。用甲醇作为样品中氢氯噻嗪的提取液，超声提取15 min，离心机10 000 r/min离心3 min，过0.22 μm聚四氟乙烯滤膜后，经C18色谱柱（50 mm×2.1 mm，2.6 μm）分离，用乙腈与10 mmol/L乙酸铵溶液为流动相，梯度洗脱。在负电喷雾离子（ESI-）源采用多反应监测（MRM）模式，外标法定量检测。氢氯噻嗪在0～100 ng/mL范围，待测物浓度和色谱峰面积成正比例线性关系，氢氯噻嗪线性方程为：y＝61.43x＋26.18，相关系数r＝0.999。氢氯噻嗪的方法检出限为0.059 μg/g。在 0.10 μg/g、0.50 μg/g、1.00 μg/g 三个水平进行加标回收与精密度实验，氢氯噻嗪的回收率分别为97.0%、103.4%、104.7%，精密度分别为6.3%、4.6%、3.7%。该方法回收率与精密度符合GB/T 27404-2008《实验室质量控制规范 食品理化检测》的要求，满足保健品中非法添加物氢氯噻嗪的检测。

关键词：超高效液相色谱-串联质谱法；负离子模式；保健品；氢氯噻嗪；检测

中图分类号：TS207.3   文献标识码：A   文章编号：1674-506X（2021）04-0122-0006

Determination of Hydrochlorothiazide in Health Products by Ultra Performance Liquid Chromatography-tandem Mass Spectrometry

PENG Ming-jun, LIN Zi-hao, ZENG Hao-wei, ZHOU Qing-qiong,

QIAN Zhen-jie, ZENG Xi^*, QI Ping^*

（Guangzhou Inspection of Food Control, Guangzhou Guangdong 511400, China）

Abstract：To establish the method for the determination of hydrochlorothiazide in health products by ultra performance liquid chromatography-tandem mass spectrometry (UPLC-MS/MS) negative ion mode Methanol was used as the extract of hydrochlorothiazide in the sample, ultrasonic extraction for 15 min, centrifuge at 10 000 r/min for 3 min, after 0.22 μm polytetrafluoroethylene filtration membrane, the separation was performed on C18 chromatographic column (50 mm×2.1 mm, 2.6 μm), the mobile phase was 10 mmol/L ammonium acetate solution and acetonitrile, gradient elution was performed. In the negative electrospray ionization (ESI-) source, multiple reaction monitoring mode was used to detection, quantification by external standard method. The results showed that in the range of 0～100 ng/mL, the concentration of hydrochlorothiazide was proportional to the size of the chromatographic peak area. The linear equation of hydrochlorothiazide is y＝61.43x＋26.18. The correlation coefficient was 0.999. The detection limit of hydrochlorothiazide method was 0.059 μg/g. The standard recovery test and precision test were carried out at three levels of 0.10 μg/g, 0.50 μg/g and 1.00 μg/g, the recovery rate of hydrochlorothiazide were 97.0%, 103.4% and 104.7%, respectively, the precision were 6.3%, 4.6% and 3.7%, respectively. The recovery and precision of this method conforms to the requirements of GB/T 27404-2008 Laboratory quality control standard for food physical and chemical testing, meet the health products in the illegal addition of hydrochlorothiazide detection.

Keywords：ultra performance liquid chromatography-tandem mass spectrometry; negative ion mode; health products; hydrochlorothiazide；detection

doi：10.3969/j.issn.1674-506X.2021.04-018

收稿日期：2021-04-09

基金项目：广州市科技计划项目（201707010372）；广州市市场监督管理局科技项目（2020kj51）;广东省食药局科技创新团队项目（2019TDB04）

作者简介：彭名军（1981-），男，硕士，高级工程师。研究方向：食品分析检验。

*通信作者

引文格式：彭名军,林子豪,曾豪威,等.超高效液相色谱-串联质谱法测定保健品中的氢氯噻嗪[J].食品与发酵科技,2021,57(4):122-126,130.