摘要
[目的]建立茶叶中氯噻啉残留量的液相色谱-串联质谱检测方法。[方法]茶叶样品经乙腈提取,提取液通过TPT固相萃取柱净化后进行仪器分析。对样品提取、净化及仪器条件参数进行优化。[结果]氯噻啉在1~500ng/mL线性关系良好(R2>0.999);检出限为1.5μg/kg,定量限为5.0μg/kg;在0.005、0.010、0.050和3.000mg/kg条件下,回收率可达88.8%~109.1%,相对标准偏差(RSD)≤5.4%(n=6)。[结论]通过方法学考察和实验室间验证表明,该方法灵敏、准确,适用于各种茶叶中氯噻啉残留量的定性和定量分析。
[Objective] The research aimed to establish a liquid chromatography-tandem mass spectrometry method for the determination of chlorothiazide residues in tea.[Method]Tea sample was extracted by acetonitrile and purified by TPT solid phase extraction before instrumental analysis. This study optimized extraction method, clean up method and instrumental parameters.[Result] The linear relationship of chlorothiazide in 1-500 ng/mL is good ( R 2 > 0.999);the limit of detection (LOD) and limit of quantification (LOQ) were 1.5 μg/kg and 5.0 μg/kg, respectively. The recoveries were 88.8%-109.1% with relative standard deviations (RSD) lower than 5.4%( n =6).[Conclusion] Based on the results of method validation and inter-laboratory validation, this method has proven to be sensitive, accurate and suitable for the qualitative and quantitative determination of imidaclothiz residue in tea.
作者
徐潇颖
罗金文
刘柱
金绍强
朱炳祺
XU Xiao-ying;LUO Jin-wen;LIU Zhu(Zhejiang Institute for Food and Drug Control,Hangzhou,Zhejiang 310000)
出处
《安徽农业科学》
CAS
2019年第15期201-204,共4页
Journal of Anhui Agricultural Sciences
基金
国家重点研发计划项目(2018YFC1603400)
关键词
氯噻啉
液相色谱-串联质谱
茶叶
固相萃取
Imidaclothiz
Liquid chromatography-tandem mass spectrometry(LC-MS/MS)
Tea
Solid phase extraction