摘要
目的建立蔬菜中氯酸盐、高氯酸盐的超高效液相色谱-串联质谱(UPLC-MS/MS)检测方法。方法蔬菜样品经水-乙腈提取,高速离心后使用Prime HLB固相萃取柱净化,Waters Torus DEA色谱柱分离,水-乙腈溶液进行梯度洗脱。以多反应监测(MRM)模式,电喷雾负离子模式,内标法定量,UPLC-MS/MS法检测。结果氯酸盐在2.0~100μg/L、高氯酸盐在1.0~50μg/L范围内所得回归方程的线性关系良好,相关系数r均大于0.999。氯酸盐的检出限和定量下限分别为6.0、20μg/kg,高氯酸盐的检出限和定量下限分别为3.0、10.0μg/kg。氯酸盐的加标浓度在40~200μg/kg范围内,回收率为90.9%~98.4%,相对标准偏差(RSD)为0.9%~2.9%。高氯酸盐的加标浓度在20~100μg/kg范围内,回收率为91.6%~105.0%,RSD为1.5%~3.9%。结论该方法简单高效、准确可靠,适用于蔬菜中氯酸盐和高氯酸盐的检测。
Objective To establish a method for the determination of chlorate and perchlorate in vegetables by ultra-high performance liquid chromatography-tandem mass spectrometry(UPLC-MS/MS).Methods The vegetable samples were extracted with water-acetonitrile,purified by Prime HLB solid phase extraction column after high-speed centrifugation,separated by waters torus DEA column,and gradient eluted with water-acetonitrile solution.The detection was carried out by UPLC-MS/MS with internal standard method,multi-reaction monitoring mode and negative ion mode of electrospray ionization source.Results The calibration curve was linear in the concentration range of 2.0-100μg/L for chlorate and 1.0-50μg/L for perchlorate(r2≥0.999).The detection limit and quantitative limit of chlorate were 6.0μg/kg and 20μg/kg,and the detection limit and quantitative limit of perchlorate were 3.0μg/kg and 10.0μg/kg.The recovery of chlorate was 90.9%~98.4%,the relative standard deviation(RSD)was 0.9%-2.9%with the spiked concentration in the range of 40-200μg/kg.The recovery of perchlorate was 91.6%~105.0%,the RSD was 1.5%-3.9%with the spiked concentration in the range of 20-100μg/kg.Conclusion The method was simple,efficient,accurate and reliable,which is suitable for the determination of chlorate and perchlorate in vegetables.
作者
胡菏
于晖
彭文芳
朱超
HU He;YU Hui;PENG Wen-fang;ZHU Chao(Nutrition and Food Safety Institute of Jiangxi Provincial Center for Disease Control and Prevention,Jiangxi Provincial Key Laboratory of Diagnosing and Tracing of Foodborne Disease,Nanchang,Jiangxi 330029,China;不详)
出处
《环境与健康杂志》
CAS
北大核心
2023年第3期262-265,共4页
Journal of Environment and Health
基金
江西省卫生健康委科技计划项目(202211297,202210078)
关键词
超高效液相色谱-串联质谱法
氯酸盐
高氯酸盐
蔬菜
Ultra-high performance liquid chromatography-tandem mass spectrometry
Chlorate
Perchlorate
Vegetables
