摘要
10.00g样品经15mL乙酸-乙腈(1+99)混合液匀浆提取1min后,加入氯化钠4~6g,再匀浆30s,离心后取上清液1.5~2.0mL于装有25mg N-丙基乙二胺、150mg无水硫酸镁的QuEChERS净化管中,涡旋振荡30s,离心后取上清液1.0mL,于40℃氮吹至近干,用正己烷定容至1.0mL。采用DB-5/DB-35色谱柱(30m×0.25mm,0.25μm)进行分离,电子捕获检测器(ECD)进行测定。12种农药的质量浓度在0.080~1.60mg·L^(-1)内与峰面积呈线性关系,检出限(3S/N)为0.10~1.5μg·kg^(-1),测定下限(10S/N)为0.33~5.0μg·kg^(-1)。加标回收率为85.6%~119%,测定值的相对标准偏差(n=6)为3.2%~8.0%。
The sample （10.00g） was extracted with 15 mL of a mixture of acetic acid and acetonitrile （1＋99） by homogenate for 1 min,then 4-6g of NaCl was added to the solution.After homogenate treatment for 30 s and followed centrifugation,1.5-2.0 mL of the supernatant was transferred to the QuEChERS purification tube filled with 25 mg of N-propyl ethylenediamine and 150 mg of anhydrous magnesium sulfate,and treated by vortex oscillation for 30 s.After centrifugation,1.0 mL of the supernatant was dried at 40 ℃ by N2 blowing,and the residue was diluted to 1.0mL with N-hexane.DB-5/DB-35 columns （30m×0.25 mm,0.25μm） were used for seperation,and ECD was used for detection.Linear relationships were found between the peak areas and the mass concentrations of 12 kinds of pesticides in the range of 0.080-1.60mg·L^-1,with detection limits （3S/N） in the range of 0.10-1.5μg·kg^-1,and the lower limits of determination （10S/N） in the range of 0.33-5.0μg·kg^-1.Recovery rates obtained by standard addition method were 85.6%-119%,and RSDs （n=6） were 3.2%-8.0%.
出处
《理化检验（化学分册）》
CSCD
北大核心
2017年第9期1036-1041,共6页
Physical Testing and Chemical Analysis(Part B:Chemical Analysis)
基金
惠州市科技计划项目(2014B040008003)
