凝胶渗透色谱净化-高效液相色谱-串联质谱法测定土壤中的阿特拉津  

HPLC-MS/MS Determination of Atrazine in Soil with GPC Purification

作　　者：余卫娟[1] 胡文凌[1] 俞丽琅 朱静娜[1] 江胜良 李莉[1] 

机构地区：[1]嘉兴市环境保护监测站,嘉兴314000

出　　处：《理化检验（化学分册）》2016年第11期1310-1314,共5页Physical Testing and Chemical Analysis(Part B:Chemical Analysis)

摘　　要：提出了快速溶剂萃取、凝胶渗透色谱净化浓缩样品前处理,高效液相色谱-串联质谱测定土壤中阿特拉津的方法。土壤样品（10g）用二氯甲烷快速溶剂萃取,萃取液经凝胶渗透色谱净化,溶剂由二氯甲烷转换成甲醇,采用ZORBAX Eclipse XDB-C18柱作固定相进行色谱分离,以不同体积比的0.1%（φ）甲酸溶液和甲醇的混合液作流动相进行梯度洗脱。质谱测定中采用电喷雾正离子方式,多反应监测模式,外标法定量。结果表明：不同土壤样品无明显基质效应,阿特拉津的线性范围在0.2-75.0μg·kg-1之间,方法的检出限（3S）为0.01μg·kg-1。在3个浓度水平上作加标回收试验,测得回收率在71.5%-91.1%之间,测定值的相对标准偏差（n=6）在1.3%-5.6%之间。HPLC-MS/MS was proposed for determination of atrazine in soil by accelerated solvent extraction （ASE） and gel permeation chromatography （GPC） for purification and concentration of sample. Soil sample （10 g） was extracted by ASE with dichloromethane, and the extract was purified by GPC. The solvent of dichloromethane was displaced by methanol, and the methanol solution was separated by LC using ZORBAX Eclipse XDB-C18 column as stationary phase, and mixtures of 0. 1% （φ） formic acid solution and methanol in various ratios as mobile phase in gradient elution- Ion source of ESI＋ and the mode of multi-reaction monitoring were adopted in MS/MS. External standard method was used for quantification. As shown by the experimental results, no significant matrix effect was observed for different soil samples. Linearity range was found between 0. 2-- 75. 0 μg·kg-1 for mass fraction of atrazine, and the detection limit （3S） found was 0, 01 μg·kg-1. Test for recovery was made by standard addition method at 3 concentration levels, giving results in the range of 71.5 %- 91. 1 %, with RSDs （n = 6） ranged from 1.3% to 5.6%.

关 键 词：高效液相色谱-串联质谱法 快速溶剂萃取 凝胶渗透色谱 阿特拉津 土壤 

分 类 号：O657.63[理学—分析化学]