高效液相色谱-三重四级杆质谱法同时测定水产品中6种苯二氮卓类镇静剂残留
Simultaneous determination of six benzodiazepine sedatives residue in aquatic products by high performance liquid chromatography-triple quadrupole mass spectrometry
张律 1朱波 1赖少阳 1岳亚军 1游杰1
作者信息
- 1. 深圳市罗湖区疾病预防控制中心,深圳 518020
- 折叠
摘要
目的 建立高效液相色谱-三重四级杆质谱法同时测定水产品中6种苯二氮卓类镇静剂残留的方法.方法 样品用乙腈提取后经C18固相萃取柱净化,待测液经 Waters ACQUITY UPLC BEH C18 色谱柱(2.1mm×50mm,1.7μm)分离,以0.1％甲酸水溶液和甲醇为流动相进行梯度洗脱,采用多反应监测模式检测,内标法定量.结果 6种苯二氮卓类镇静剂在1.0～50.0 μg/L浓度范围内线性关系良好,相关系数r均＞0.9990,检出限和定量限分别为0.3和1.0 µg/kg,在3个浓度加标水平下的平均回收率为74.2％～108.0％,相对标准偏差为1.1％～6.7％(n=6).结论 该方法简便快捷、灵敏度高、结果准确,可用于水产品中6种苯二氮卓类镇静剂残留的同时检测.
Abstract
OBJECTIVE To establish a method for the simultaneous determination of 6 benzodiazepine sedatives residue in aquatic products by high performance liquid chromatography-triple quadrupole mass spectrometry.METHODS The samples were extracted with acetonitrile and purified by C18 solid phase extraction column.The sample solution was separated by Waters ACQUITY UPLC BEH C18 column(2.1 mm×50 mm,1.7 μm)using 0.1％formic acid and methanol as mobile phase for gradient elution,determined in multiple reaction monitoring mode and quantified by internal standard method.RESULTS Six benzodiazepine sedatives had a good linear relationship in the range of 1.0-50.0 µg/L with r＞0.9990,the limits of detection and limits of quantification were 0.3 and 1.0 pg/kg.Average recoveries for the analytes at 3 spiked levels ranged from 74.2％-108.0％with relative standard deviations of 1.1％-6.7％(n=6).CONCLUSION The method is simple,rapid,sensitive and accurate,which is suitable for simultaneous determination of 6 benzodiazepine sedatives residue in aquatic products.
关键词
高效液相色谱-三重四级杆质谱法/水产品/苯二氮卓/镇静剂Key words
highperformanceliquidchromatography-triplequadrupolemass spectrometry/aquatic products/benzodiazepine/sedative引用本文复制引用
基金项目
深圳市罗湖区软科学研究计划(LX20211104)
出版年
2024
NETL
NSTL
万方数据