搅拌棒吸附萃取-液相色谱-串联质谱法测定农业废水中二氯吡啶酸残留量  

Determination of Clopyralid Residues in Agricultural Wastewater by Liquid Chromatography-Mass Spectrometry Combined with Stir Bar Sorptive Extraction

作　　者：王雪平[1,2] 耿悦 朱惠斌 WANG Xueping;GENG Yue;ZHU Huibin(Yellow River Conservancy Technical Institute,Kaifeng 475004;Key Laboratory of Green Coating Materials of Kaifeng City,Kaifeng 475004)

机构地区：[1]黄河水利职业技术学院,河南开封475004 [2]开封市绿色涂层材料重点实验室,河南开封475004

出　　处：《分析科学学报》2020年第4期547-552,共6页Journal of Analytical Science

基　　金：河南省科技厅支持项目(No.172102410035);黄河水利职业技术学院2018年科技项目(No.2018XJJGLX023)。

摘　　要：建立了搅拌棒吸附萃取-液相色谱-串联质谱(SBSE-LC-MS/MS)法测定农业废水中二氯吡啶酸残留量的分析方法。样品经搅拌棒吸附萃取,以BEH C 18柱为分析柱,以乙腈和0.1%甲酸溶液为流动相进行梯度洗脱,采用质谱测定。结果表明:二氯吡啶酸质量浓度在1.0~50.0 ng/mL范围内与其质谱响应值呈线性关系,相关系数(r)为0.9998;方法检出限为0.3μg/L,方法定量限为1.0μg/L;加标回收率范围87.8%~97.8%;相对标准偏差(RSD,n=6)为0.9%~4.7%。本方法操作简便、试剂消耗少、准确度高、检出限低,适用于农业废水中二氯吡啶酸含量监测。The liquid chromatography-mass spectrometry(SBSE-LC-MS/MS)combined with stir bar sorptive extraction was established for determination of clopyralid residues in agricultural wastewater.The samples were extracted with a stir bar,and separated on BEH C 18 column with gradient elution by using acetonitrile and 0.1%formic acid solution as eluant,and determinated by mass spectrometry.The results showed that the concentration of clopyralid was linearly related to the mass spectrometry response in the range from 1.0 ng/mL to 50.0 ng/mL,and the linear regression equation is y=8127.3x+654.2,and the correlation coefficient is 0.9998.The limits of detection and the limits of quantitation were 0.3μg/L and 1.0μg/L,respectively.The recoveries ranged from 87.8%to 97.8%,and the relative standard deviations ranged from 0.9%to 4.7%.The method is simple,low reagent consumption,high accuracy,low detection limit,and is suitable for monitoring the content of clopyralid in agricultural wastewater.

关 键 词：二氯吡啶酸 搅拌棒吸附萃取 液相色谱-质谱法 农业废水 

分 类 号：O657.63[理学—分析化学]