GC-NCI/MS法测定含硫蔬菜中86种农药残留  

Determination of 86 Pesticide Residues in Sulfur-containing Vegetables by GC-NCI/MS

作　　者：于猛[1] 王敬[2] 段文仲[1,2] 艾连峰[2] 马育松[2] 李玮[2] 

机构地区：[1]河北农业大学食品科技学院,保定071001 [2]河北出入境检验检疫局,石家庄050051

出　　处：《食品工业》2016年第9期246-252,共7页The Food Industry

基　　金：河北检验检疫局科研项目(HE2014K018)

摘　　要：在系统优化固相萃取吸附剂填料类型和洗脱溶剂种类的基础上,建立了含硫蔬菜（青葱、韭菜和蒜薹）中86种农药残留的气相色谱-负化学离子源质谱（GC-NCI/MS）的测定方法。样品在低温冷冻的条件下,加磷酸去除大部分硫化物,然后用乙腈均质提取,经装有无水碳酸钠的石墨化碳黑/氨基固相萃取柱（ENVI-Carb/NH2）净化后,用GC-NCI/MS选择离子监测方式（SIM）进行检测,外标法定量。结果表明,86种农药在相应的范围内线性关系良好,相关系数均大于0.99,方法检出限（以3倍信噪比计）为0.05-3.33μg/kg,方法定量限（以10倍信噪比计）为0.16-9.99μg/kg,在10,50和100μg/kg的加标水平下,各目标农药的平均添加回收率为70.3%-117.5%,相对标准偏差（RSD）为4.5%-18.7%。该方法灵敏、准确,相比其他含硫蔬菜分析方法净化效果好,可用于含硫蔬菜中86种农药残留的检测。On the basis of the optimization of solid phase extraction adsorbent, eluting solvent types and amounts, a gas chromatography-negative chemical ionization mass spectrometric （GC-NCI/MS） method was been developed for analyzing 86 pesticides in sulfur-containing vegetables （green Chinese onion, leek and garlic sprout） by GC-NCI/MS. The frozen samples were treated with phosphoric acid-assisted to inactivate enzymes, and were extracted with acetonitrile, cleaned-up with an ENVI-Carb/NH2 solid-phase extractant, which was equipped with anhydrous sodium carbonate, and then determined by GCNCI/MS using external standard method at selected ion monitor mode （SIM）. The linearities of the method were good with the correlation coefficients higher than 0.99. The limits of detection （S/N=3） were in the range of 0.05-3.33 μg/kg, the limits of quantitation （S/N=10） were in the range of 0.16-9.99μg/kg. The average recoveries in different matrices were varied from 70.3 % to 117.5 % with the relative standard deviations （RSDs） of 4.5%-18.7% at the spiked levels of 10, 50 and 100 μg/kg. The method was sensitive and convenient for meeting the requirements for the simultaneous identification and quantification of the multi-residues in sulfur-containing vegetables.

关 键 词：低温磷酸处理 气相色谱-负化学离子源质谱 含硫蔬菜 农药残留 

分 类 号：O657.63[理学—分析化学]