液相色谱-串联质谱法测定土壤和氯化钙水溶液中莠去津的残留量

Determination of Atrazine Residues in Soil and CaCl_(2) aq by Liquid Chromatography-Tandem Mass Spectrometry

【目的】建立超高效液相色谱-串联质谱法检测土壤和氯化钙水溶液中莠去津残留量的分析方法,为土壤中莠去津的检测和吸附提供理论依据和技术手段。【方法】样品中莠去津经乙腈提取,采用QuEChERS技术净化,使用Acquity UPLC®BEH C18色谱柱进行分离,以乙腈和0.2%甲酸水溶液为流动相进行梯度洗脱,超高效液相色谱-串联质谱检测,外标法定量。【结果】莠去津在0.001~5.0 mg/L线性关系较好(r>0.99),在0.05~0.50 mg/kg的添加水平下,莠去津在土壤和0.01 mol/L氯化钙水溶液中的回收率为80.9%~115.4%,相对标准偏差为1.5%~3.5%,定量限(LOQ)为0.3、0.06μg/kg。【结论】该方法操作简便、灵敏度高、快速准确,适用于土壤和氯化钙水溶液中莠去津的检测。

This study aims to establish the residue analysis method of atrazine on soil and CaCaCl_(2) aq by UPLC-MS/MS in order to provide theoretical basis and technical means for the detection and adsorption of atrazine in soil.The samples were extracted with acetonitrile and purified with C18 powder by QuEChERS technology,they were separated on the Acquity UPLC®BEH C18 column,gradient eluted with acetonitrile and 0.2%formic acid,then detected by UPLC-MS/MS and quantified by external standard method.Atrazine showed a good linear relationship in the range of 0.001-5.0 mg/L(r>0.99).At addition levels of 0.05-0.50 mg/kg,the recoveries of atrazine in soil and 0.01 mol/L CaCaCl_(2) aq were in the range of 80.9%-115.4%with relative standard deviations of 1.5%-3.5%.The limit of quantifications(LOQ)were 0.15μg/kg and 0.08μg/kg The method is simple,high sensitivity,fast and accurate,which is suitable for the determination of atrazine in soil and CaCaCl_(2) aq.