QuEChERS-超高效液相色谱-三重四极杆串联质谱法检测保健茶中18种违禁添加药物

doi:10.13305/j.cnki.jts.2021.02.006

摘要/Abstract

摘要： 建立了超高效液相色谱-三重四极杆串联质谱同时检测保健茶中西布曲明等18种违禁添加药物的方法。样品经1%甲酸-甲醇溶液超声提取20 min,采用QuEChERS分散固相萃取试剂盒净化,以0.1%甲酸-乙腈溶液为流动相,0.2 mL·min^-1流速梯度洗脱,经Agilent ZORBAX Eclipse Plus-C₁₈柱分离,电喷雾离子源正离子扫描,多反应监测模式测定,外标法定量。结果表明,18种违禁添加药物在保健茶基质中的线性良好,相关系数均大于0.999,方法检出限为0.5~5.0 μg·kg^-1,方法定量限为2~18 μg·kg^-1,RSD为0.5%~5.1%,加标回收率为87.3%~103.8%。运用本方法检测了30批次保健茶样品,其中7批次为阳性样。本方法针对性强、操作简便、准确度高、检测速度快,适用于保健茶中18种违禁添加药物含量的测定,为保健茶的质量控制和安全评价提供科学依据。

关键词: 超高效液相色谱-三重四极杆串联质谱, QuEChERS, 保健茶, 违禁药物

Abstract: A method for the simultaneous determination of Sibutramine and other 18 prohibited additives in health-protecting tea by ultra high performance liquid chromatography triple quadrupole tandem mass spectrometry (UPLC-MS/MS) was established．Samples were extracted by ultrasonic extraction from 1% formic acid methanol solution for 20 min and purified by QuEChERS dispersive solid-phase extraction kit. The mobile phase was 0.1% formic acid in acetonitrile and 0.2 mL·min^-1 flow gradient elution was used in Agilent ZORBAX Eclipse Plus-C₁₈ column．Electrospray ion source positive ion scanning, multiple reaction monitoring (MRM) mode were determined and external standard method was used for quantification. The results show that the linearity of 18 kinds of illegal additives was good, with the correlation coefficient more than 0.999. The detection limit was 0.5-5.0 μg·kg^-1. The quantitative limit of the method was 2-18 μg·kg^-1. RSD was 0.5%-5.1% and the recovery rate was 87.3%-103.8%. This method was used to analyze 30 batches of health-protecting tea samples, of which 7 batches were positive samples. This method has strong pertinence,simple operation, high accuracy and fast detection speed. It is suitable for the determination of 18 kinds of forbidden additives in health-protecting tea. This paper also provided a scientific basis for the quality control and safety evaluation of health-protecting tea.

Key words: UPLC-MS-MS, QuEChERS, health-protecting tea, contraband drugs

中图分类号:

甘凝岚, 朱晓军, 李洁莉, 周玮, 刘长宇. QuEChERS-超高效液相色谱-三重四极杆串联质谱法检测保健茶中18种违禁添加药物[J]. 茶叶科学, 2021, 41(2): 237-250. doi: 10.13305/j.cnki.jts.2021.02.006.

GAN Ninglan, ZHU Xiaojun, LI Jieli, ZHOU Wei, LIU Changyu. Detection of 18 Prohibited Additives in Health-Protecting Tea by QuEChERS Method and Ultra High Performance Liquid Chromatography Triple Quadrupole Tandem Mass Spectrometry[J]. Journal of Tea Science, 2021, 41(2): 237-250. doi: 10.13305/j.cnki.jts.2021.02.006.

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