微量QuEChERS-超高效液相色谱-串联质谱法检测凉茶中59种非法添加化学药物
Determining the 59 Chemical Drugs Illegally Added in Herbal Tea by a Micro-QuEChERS-Based UPLC-MS/MS
戴尽波 1沈洁 1董文静 1何啸峰 1聂荣荣 1梁沁娴 1叶彩平1
作者信息
- 1. 梅州市食品药品监督检验所,广东梅州 514071
- 折叠
摘要
目的:建立一种微量QuEChERS(micro-QuEChERS)结合超高效液相色谱-串联质谱(UPLC-MS/MS)同时检测凉茶中 59种非法添加药物的分析方法.方法:样品用乙腈超声提取 5 min,提取液用 NaCl及无水Na2SO4 进行盐析分层,上清液用C18 吸附剂进行净化后,经ACQUITY HSS T3(100 mm×2.1 mm,1.8 μm)色谱柱分离,以 0.01%甲酸水溶液(A)-乙腈:甲醇(8:2)(B)为流动相进行梯度洗脱,并采用电喷雾正负离子多反应监测模式检测,空白基质外标法定量.结果:59种化合物在其线性浓度范围内,线性关系良好,决定系数均大于 0.999,检出限为 5.0～10.0 μg/L,定量限为 10.0～25.0 μg/L.在 25.0、50.0、100.0 μg/L 3个添加水平下,平均回收率为 60.3%～128.8%(n=6),相对标准偏差(RSD)1.0%～13.7%.结论:该方法操作简单,净化效果好,灵敏度高,可用于凉茶中59种非法添加化学药物的快速分析.
Abstract
Objective:An analysis method for simultaneous determination of 59 kinds of chemical drugs illegally added in herbal tea by micro-QuEChERS method combined with ultra performance liquid chromatography-tandem mass spect-rometric(UPLC-MS/MS)was established.Method:The samples were extracted by ultrasonic extraction from acetonitrile solution for 5 min and salted out with sodium chloride(NaCl)and anhydrous sodium sulfate(Na2SO4).Supernatant was purified with C18 sorbent and separated on a ACQUITY HSS T3 column(100 mm×2.1mm,1.8 μm)by gradient elution using a mixture of 0.01%formic acid and acetonitrile:methanol(8:2)as the mobile phase.Then the analytes were quantified by UHPLC-MS/MS in multiple reaction monitoring mode(MRM)via positive and negative electrospray ionization quantified by external standard method.Result:The coefficient of determination of the standard calibration curves for the 59 analytes were all above 0.9990.The limit of detection(LOD,S/N≥3)and the limit of quantitation(LOQ,S/N≥10)were 5.0～10.0 and 10.0～25 μg/L.At three spiked of 25.0,50.0 and 100.0 μg/L,the average recoveries of 59 analytes were 60.3%～128.8%(n=6)with the relative standard deviations in the range of 1.0%～13.7%.Conclusion:The method developed was simple,sensitive,and had good purification effect.It could be applied for the rapid determination of 59 chemical drugs illegally added in herbal tea.
关键词
QuEChERS/超高效液相色谱-串联质谱法/凉茶/非法添加/化学药物Key words
QuEChERS/UPLC-MS/MS/herbal tea/illegal added/chemical drugs引用本文复制引用
基金项目
梅州市社会发展科技计划项目(2020B084)
出版年
2024
国家科技期刊平台
NSTL
万方数据