直接进样-超高效液相色谱-串联质谱法测定水中莠去津及其6种代谢物  

Determination of atrazine and its six metabolites in water by direct injection-ultra high performance liquid chromatography-tandem mass spectrometry

作　　者：邵国健[1] 王晔 姚建花[1] SHAO Guo-jian;WANG Ye;YAO Jian-hua(Huzhou Municipal Centre for Disease Control and Prevention,Huzhou Key Laboratory of Public Health Emergency Detection,Zhejiang 313000,China)

机构地区：[1]湖州市疾病预防控制中心、湖州市公共卫生应急检测重点实验室,浙江313000

出　　处：《中国卫生检验杂志》2023年第1期20-23,共4页Chinese Journal of Health Laboratory Technology

摘　　要：目的 建立直接进样-超高效液相色谱-串联质谱(UPLC-MS/MS)快速测定生活饮用水中莠去津及其6种代谢物残留的方法。方法 水样经0.22μm滤膜过滤后,直接进样分析,水-乙腈作为流动相进行梯度洗脱,ACQUITYBEH C18(2.1 mm×100 mm, 1.7μm)色谱柱分离,采用电喷雾正离子电离,经多反应监测离子扫描(MRM)模式监测,以保留时间和目标物的二级质谱特征碎片离子定性,以外标法定量。结果 莠去津及其6种代谢物在0.01μg/L~10μg/L质量浓度内线性关系良好(r≥0.998),高、中、低3个浓度水平的平均加标回收率为94.2%~107%,相对标准偏差为1.2%~6.5%(n=7),方法检出限为0.001μg/L~0.02μg/L,方法定量限为0.003μg/L~0.06μg/L。结论 该方法所需样品量少、操作简便、准确度和精密度好,适用于生活饮用水及地表水中莠去津及其6种代谢物的测定。Objective This study aims to establish a method for the rapid determination of atrazine and its six metabolites in water by direct injection-ultra high performance liquid chromatography-tandem mass spectrometry. Methods Water samples were filtrated with a 0.22 μm millipore filter, and then directly injected for analysis. The analytes were separated on an ACQUITYBEH C18column(2.1 mm×100 mm, 1.7 μm) using a programmed gradient elution mode with a mobile phase consisting of water and acetonitrile. Electrospray ionization(ESI) and multi-reaction monitoring(MRM) were used for the detection. The qualification was based on retention time and MS/MS characteristic fragment ions of the targets, and the quantification was based on the external standard calibration curves. Results Good linearity was obtained in the range of 0.01 μg/L-10 μg/L for atrazine and its six metabolites, with the correlation coefficient(r) greater than 0.998. The average recoveries for the spiked levels of low, medium and high ranged from 94.2% to 107%, with relative standard deviations(RSD, n=7) of 1.2%-6.5%. The detection limits were from 0.001 μg/L to 0.02 μg/L, while the quantification limits were from 0.003 μg/L to 0.06 μg/L. Conclusion The method requires a small amount of samples, features easy operation, good accuracy and precision, and is suitable for the determination of atrazine and its six metabolites in drinking water and surface water.

关 键 词：莠去津 代谢物 直接进样 超高效液相色谱-串联质谱法 

分 类 号：O657[理学—分析化学]