摘要
为建立一种QUECHERS气相色谱-质谱法(GC/MS)同时检测农作物水环境二甲戊灵、甲霜灵、丁草胺、联苯肼酯、莠去津、毒死蜱6种常用农药残留的检测方法,农作物水环境样品用QUECHERS萃取剂提取,无水硫酸镁盐析,经N-丙基乙二胺(PSA)和C18净化后,离心并取2 mL上清液氮气吹至近干,残渣用丙酮定容至1 mL。过滤后经GC/MS进行检测,外标法定量。结果表明,在0.02~20μg/m L线性范围内6种农药线性关系良好,相关系数(R2)<0.995;6种农药检出限范围为0.008~0.013 mg/kg,低(0.1 mg/kg)、中(0.5 mg/kg)、高(2.0 mg/kg)三个不同水平的加标回收率均在85.8%~98.9%之间;重复性RSD (n=6)在1.32~2.68%之间,精密度RSD (n=6)在1.06%~3.20%之间。研究表明,该方法具有前处理提取快速、检出限低、检测结果准确等优点,可以用于农作物水环境中常用农药的监测。
A QUECHERS pre-treat-GC/MS method for detection of pendimethalin, metalaxyl, butachlor, bifenazate, atrazine and chlorpyrifos in crops environmental water was established. Crops environmental water samples were extracted by QUECHERS absorbent, after salt out process by anhydrous magnesium sulfate, samples was purified by PSA and C18. The solution was centrifuged and 2 mL liquid supernatant was transferred blowing drying with Nitrogen. Residues were dilute with acetone to 1 mL. After filtered, samples were analyzed by GC-MS and quantified by external standard method. The result showed that in the range 0.02-20 μg/mL, concentrations of 6 pesticides showed good linear relationships, and the correlation coefficients were all above 0.995. Detection limits of 6 pesticides were between 0.008 and 0.013 mg/kg, the recoveries at low(0.1 mg/kg), medium(0.5 mg/kg) and high(2.0 mg/kg) levels were in the range 85.8% to 98.9%, and the relative standard deviation(RSD) of repeatability was 1.32%-2.68%. RSDs of precision(n=6) were between 1.06% and 3.20%. This method was proved to have quick pre-treated, low detection and with accuracy results, which could apply to determine formal pesticides in crops environmental water.
作者
邓丽
张晓云
DENG Li;ZHANG Xiaoyun(Gansu Province Environmental Monitoring Station of Zhangye City,Zhangye 734000)
出处
《食品工业》
CAS
北大核心
2019年第9期236-239,共4页
The Food Industry
关键词
QUECHERS
气相色谱
质谱
环境水
农药残留
QUECHERS
gas chromatography
mass spectrometry
crops environmental water
pesticide
