尿中三氯卡班和三氯生测定的QuEChERS-超高效液相色谱-串联质谱法
Determination of triclocarban and triclosan in urine by QuEChERS extraction and ultra-performance liquid chromatography-tandem mass spectrometry
邱巧丽 1陈晓红 1姚珊珊 1姚浔平 1方兰云 1金米聪1
作者信息
- 1. 宁波市疾病预防控制中心理化检验所,浙江省微量有毒化学物健康风险评估技术研究重点实验室,宁波 315010
- 折叠
摘要
目的 建立QuEChERS净化后超高效液相色谱-三重四极杆质谱联用(UPLC-MS/MS)法测定尿液中三氯卡班(TCC)和三氯生(TCS)含量.方法 于2022年5月,将尿液样品经乙腈提取,QuEChERS净化,Waters Acquity UPLC BEH C18柱(100 mm×2.1 mm,1.7 μm)分离,以水-乙腈体系为流动相梯度洗脱,流速为0.3 ml/min,采用电喷雾负离子模式和多反应监测扫描方式检测,内标法定量分析,对建立的方法进行方法学验证.结果 TCC和TCS的线性范围为分别为0.5～100.0 μg/L和1.0～100.0μg/L,相关系数分别为0.999 7、0.999 1;方法检出限分别为0.17和0.33 μg/L,定量限分别为0.5和1.0 μg/L;在2.0、10.0、80.0 μg/L 3个加标水平下,TCC和TCS的加标回收率分别为100.1％～102.8％和96.7％～108.6％,相对标准偏差分别为4.9％～6.7％和4.1％～8.3％.结论 QuEChERS-UPLC-MS/MS法操作简便、快速、灵敏、重现性好,可用于职业人群TCC和TCS暴露水平的同时快速准确检测.
Abstract
Objective To establish a method for the determination of triclocarban(TCC)and triclosan(TCS)in urine by ultra-performance liquid chromatography-tandem mass spectrometry(UPLC-MS/MS)after purification by QuEChERS.Methods In May 2022,urine samples were extracted by acetonitrile,purified by QuEChERS,separated by Waters Acquity UPLC BEH C18 column(100 mm×2.1 mm,1.7 μm),and eluated with water-acetonitrile as mobile phase gradient at a flow rate of 0.3 ml/min.The detection was conducted in negative ion mode(ESI-)and multiple reaction monitoring(MRM)scanning,it was quantified with a internal standard method,and the methodology was verified.Results The linear ranges of TCC and TCS were 0.5-100.0 μg/L and 1.0-100.0 µg/L,and the correlation coefficients were 0.9997 and 0.9991,respectively.The limits of detection and quantitation of TCC and TCS were 0.17 and 0.33 μg/L,and 0.5 and 1.0 μg/L,respectively.The recoveries of TCC and TCS were 100.1％-102.8％and 96.7％-108.6％,and the relative standard deviations were 4.9％-6.7％and 4.1％-8.3％,respectively,at 2.0,10.0 and 80.0 μg/L.Conclusion QuEChERS-UPLC-MS/MS method is simple,rapid,sensitive and reproducible,and can be used for rapid and accurate simultaneous detection of TCC and TCS exposure levels in occupational population.
关键词
三氯生/三氯卡班/尿/QuEChERS/超高效液相色谱/串联质谱法Key words
Triclosan/Triclocarban/Urine/QuEChERS/Ultra-performance liquid chromatography/Tandem mass spectrometry引用本文复制引用
基金项目
宁波市医学重点学科建设项目(2022-B18)
浙江省基础公益研究计划(LGC22H260002)
宁波市公益重点项目(2022S091)
出版年
2024
NETL
NSTL
维普
万方数据