| 气相色谱－串联质谱法测定植物源化妆品中53种农药残留 |
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| 基金项目:广州市科技计划项目（202102020530） |
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| 中文摘要:采用固相萃取技术结合气相色谱－串联质谱（GC－MS/MS），建立了植物源化妆品中53种农药残留的检测方法。将不同剂型的植物源化妆品样品经乙腈提取、冷冻除脂－固相萃取净化和浓缩定容后，以Agilent VF－17ms毛细管柱（30 m × 0.25 mm × 0.25 μm）分离，在GC－MS/MS选择反应监测（SRM）模式下检测，以基质匹配外标法定量。结果表明，53种农药具有良好线性关系，相关系数（r2）为0.996 1 ~ 0.999 9；方法检出限（LOD）为0.01 ~ 0.02 mg/kg，定量下限（LOQ）为0.02 ~ 0.05 mg/kg。精华液和膏霜样品中，53种农药的平均回收率为77.1% ~ 105%，相对标准偏差（RSD，n = 6）为0.50% ~ 4.9%。应用该方法对30个植物源化妆品进行检测，共检出2例阳性样品。该方法具有简便、快速、准确及灵敏度高的优点，适用于植物源化妆品中53种农药残留的测定，可为保障化妆品的质量安全提供技术支撑。 |
| 中文关键词:气相色谱－串联质谱（GC－MS/MS） 固相萃取 植物源化妆品 农药残留 |
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| Determination of 53 Pesticide Residues in Phytocosmetics by Gas Chromatography－Tandem Mass Spectrometry |
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| Abstract:A gas chromatography－tandem mass spectrometry（GC－MS/MS） with solid phase extraction（SPE） was developed for the determination of 53 pesticides residues in phytocosmetics．The phytocosmetics samples were firstly extracted with acetonitrile，then the lipid substances in acetonitrile extract were removed by centrifugation under freezing condition．Concentration and clean-up steps were performed by solid phase extraction．After the pretreatment，the samples were separated on an Agilent VF－17ms capillary column（30 m × 0.25 mm × 0.25 μm），then detected by GC－MS/MS in selective reaction monitoring（SRM） mode and quantified by matrix-matched calibration．Results showed that there were good linear relationships for the 53 analytes with their correlation coefficients（r2） of 0.996 1－0.999 9．The limits of detection（LODs） and the limits of quantitation（LOQs） were in the range of 0.01－0.02 mg/kg and 0.02－0.05 mg/kg，respectively．The average recoveries for 53 pesticides in the samples ranged from 77.1% to 105%，with the relative standard deviations（RSDs，n = 6） of 0.50%－4.9%．The method was applied to the determination of 30 phytocosmetics samples，of which two positive samples were found．This method is simple，convenient，accurate and sensitive，which is suitable for the determination of 53 pesticide residues in phytocosmetics and could provide technical support for ensuring the quality and safety of cosmetics. |
| Key Words:gas chromatography－tandem mass spectrometry（GC－MS/MS） solid phase extraction phytocosmetics pesticide residues |
| 引用本文：梁梓洋，梁梓豪，马叶芬，罗辉泰，黄芳，吴惠勤.气相色谱－串联质谱法测定植物源化妆品中53种农药残留[J].分析测试学报,2022,41(11):1591-1599. |
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