尿中乙草胺及其代谢物的液相色谱-串联质谱法

Determination of acetochlor and its metabolites in urine using liquid chromatography-tandem mass spectrometry

目的:建立了液相色谱-串联质谱法(LC-MS/MS)测定尿样中乙草胺及其3种代谢物。方法:于2021年4月,尿液经HLB小柱净化,1%乙酸乙腈溶液洗脱。以0.01%甲酸溶液-乙腈作为流动相,梯度洗脱,目标物使用ACQUITY UPLC?HSS T3色谱柱(2.1 mm×100 mm×1.8 μm)作为分离柱,采用LC-MS/MS在正离子模式下进行测定。结果:4种目标物在1~50 μg/L范围内线性关系良好,相关系数( r)均>0.997,各目标物质在空白尿样中3个浓度添加水平下的回收率为107.6%~129.1%,相对标准偏差( RSD)为1.5%~9.9%( n=6),方法检出限和定量限分别为0.04~0.11 μg/L和0.15~0.42 μg/L。乙草胺职业接触人群尿样中所有目标物均有检出。 结论:该方法操作简单、快速、灵敏度高、特异性好,适用于尿样中乙草胺及其代谢物浓度的快速检测。

Objective A method for the determination of acetochlor and its metabolites in urine by liquid chromatography-tandem mass spectrometry(LC-MS/MS)was established.Methods After cleaned-up by a HLB extraction cartridges,the urine was eluted with 1%acetic acid acetonitrile solution.The target compounds were separated by ACQUITY UPLC®HSS T3 Column(2.1 mm×100 mm×1.8μm)by using 1%formic acid solution and acetonitrile as mobile phase with gradient elution program,and analyzed in positive electrospray ionization mode by liquid chromatography tandem mass spectrometry.Results All the target compounds showed good linear relationships in the range of 1-50μg/L,and the correlation coefficients(r)were higher than 0.997.The recoveries rates at three different spiked levels for all target compounds in blank matrices were 107.6%-129.1%,and the relative standard deviations(RSD)were 1.5%-9.9%(n=6).The limits of detection and quantitation of the method were 0.04-0.11μg/L and 0.15-0.42μg/L,respectively,and target substances were detected in all urine samples from occupational exposure workers to acetochlor.Conclusion This method is suitable for rapid screening and analysis of acetochlor and metabolites in urine with the advantages of accuracy,rapidity,simplicity,high sensitivity and good specificity.