高效液相色谱-串联质谱法同时测定茶叶中氯酸盐、高氯酸盐、溴酸盐和次磷酸盐  

Simultaneous determination of chlorate,perchlorate,bromate and hypophosphite in tea by high performance liquid chromatography-tandem mass spectrometry

作　　者：史谢飞[1,2] 冯德建 邹燕[1,2] 吴微 孙登峰[1,2] 李怀平 叶善蓉 SHI Xiefei;FENG Dejian;ZOU Yan;WU Wei;SUN Dengfeng;LI Huaiping;YE Shanrong(National Institute of Measurement and Testing Technology,Chengdu 610021,China;Standard and Testing Technology of Tea Key Laboratory of Sichuan Province,Chengdu 610021,China)

机构地区：[1]中国测试技术研究院,四川成都610021 [2]茶叶标准与检测技术四川省重点实验室,四川成都610021

出　　处：《中国测试》2024年第12期125-131,146,共8页China Measurement & Test

基　　金：四川省重点研发项目(2023YFS0398);成都市重点研发支撑计划项目(2022-YF05-00994-SN);中国测试技术研究院“人才计划”项目(RC202407)。

摘　　要：该文建立了高效液相色谱-串联质谱法同时测定茶叶中氯酸盐、高氯酸盐、溴酸盐和次磷酸盐含量的方法。试样采用纯水超声提取,Waters Anionic Polar Pesticide色谱柱分离,负离子多反应监测模式测定,基质匹配曲线外标法定量。各待测目标物线性范围良好,相关系数均>0.99,方法检出限为0.003~0.08 mg/kg,定量限为0.01~0.25 mg/kg,平均加标回收率为87.0%~115.2%,相对标准偏差为2.7%~8.4%。20份茶叶样品氯酸盐检出率为15%,高氯酸盐检出率为80%。该方法可满足欧盟对茶叶中氯酸盐和高氯酸盐限量的检测要求,实现茶叶中氯酸盐、高氯酸盐、溴酸盐和次磷酸盐含量的同时准确测定。A method was developed for the simultaneous determination of chlorate,perchlorate,bromate and hypophosphite in tea by high performance liquid chromatography-tandem mass spectrometry.The samples were extracted by ultrasonic extraction with pure water,separated on a Waters Anionic Polar Pesticide column,determined in negative ion multiple reaction monitoring mode,and quantified by matrix external standard method.The linear ranges of the targets to be measured were good with the correlation coefficients>0.99.The limits of detection of the method were from 0.003 mg/kg to 0.08 mg/kg,and the limits of quantification were from 0.01 mg/kg to 0.25 mg/kg,and the average recoveries of the method ranged from 87.0%to 115.2%.The relative standard deviation ranged from 2.7%to 8.4%.20 tea samples were analyzed by the method,the detection rate of chlorate was 15%and that of perchlorate was 80%.The method can meet the requirements of European Union for the determination of chlorate and perchlorate residue limits in tea,and realize the simultaneous and accurate determination of chlorate,perchlorate,bromate and hypophosphite in tea.

关 键 词：茶叶 氯酸盐 高氯酸盐 溴酸盐 次磷酸盐 高效液相色谱-串联质谱法 测定 

分 类 号：TB99[一般工业技术—计量学] O657.63[机械工程—测试计量技术及仪器]