摘要:
The sample (10.00 g) was extracted with 15 mL of a mixture of acetic acid and acetonitrile (1+ 99) by homogenate for 1 min,then 4-6 g 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 C by N2 blowing,and the residue was diluted to 1.0 mL with N-hexane.DB-5/DB-35 columns (30 m×0.25 mm,0.25 μm) 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 0.080-1.60 mg· L-1,with detection limits (3S/N) in the range of 0.10-1.5 μg · kg-1,and the lower limits of determination (10S/N) in the range of 0.33 5.0 μg · kg-1.Recovery rates obtained by standard addition method were 85.6%-119 %,and RSDs (n=6) were 3.2%-8.0%.%10.00 g样品经15 mL乙酸-乙腈(1+99)混合液匀浆提取1 min后,加入氯化钠4~6 g,再匀浆30 s,离心后取上清液1.5~2.0mL于装有25 mgN-丙基乙二胺、150 mg无水硫酸镁的QuEChERS净化管中,涡旋振荡30 s,离心后取上清液1.0 mL,于40°C氮吹至近干,用正己烷定容至1.0 mL.采用DB-5/DB-35色谱柱(30 m×0.25 mm,0.25 μm)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~l.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%.