气相色谱/质谱法检测食物中毒样品中23种有机磷类农药

王芹; 杭学宇; 宋鑫; 王露; 冯晓青; 张敏会

doi:10.13421/j.cnki.hjwsxzz.2019.02.016

气相色谱/质谱法检测食物中毒样品中23种有机磷类农药

Determination of 23 Organophosphorus Pesticides in Food Poisoning Samples by Gas Chromatography-mass Spectrometry

摘要

摘要:
目的建立气相色谱/质谱法检测食物中毒样品中有机磷类农药的方法。
方法样品经乙腈振荡提取，QuEChERS粉末净化后离心，上清液氮吹浓缩至近干后用丙酮定容至1 mL，用气相色谱/质谱仪在选择离子扫描模式下定量检测。
结果方法的线性范围为（0.1~5.0）μg/mL，线性相关系数在0.98~0.99之间，检出限（LOD）在（0.002~0.044）mg/kg，在（0.02~0.8）mg/kg添加水平下平均回收率为82.3%~124.0%，相对标准偏差（RSD）为2.5%~14.6%。
结论该方法操作简便快速，能够满足食物中毒样品中有机磷的检测。

Abstract:
Objectives To establish an analytical method for determination of organophosphorus pesticides (OPPs) in food poisoning samples by gas chromatography-mass spectrometry (GC-MS).
Methods Samples were extracted by acetonitrile oscillation and centrifuged after being purified by QuEChERS powder. The supernatants were blown by nitrogen and concentrated to near dryness with acetone to a volume of 1 mL.Then the concentrated solutions were quantitatively detected by gas chromatography-mass spectrometer in selected ion scan mode.
Results The method showed a linearity range of (0.1~5.0) μg/L with linear correlation coefficients of 0.98~0.99, and the Limit of Detection (LOD) was (0.002~0.044) mg/kg. The average recoveries were 82.3%~124.0% at the addition level of (0.02~0.8) mg/kg with the relative standard deviation (RSD) of 2.5%~14.6%.
Conclusions This method is simple and fast and can satisfy the detection of organophosphorus in food poisoning samples.

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