气相色谱-质谱联用测定苹果中五氯硝基苯残留量  

Determination of Quintozene Residue in Apple by Gas Chromatography-Mass Spectrometry

作　　者：史真真 郭凯锐 汪小芳 SHI Zhenzhen;GUO Kairui;WANG Xiaofang(Zhongping Testing Co.,Ltd.,Xuchang 461100,China;Henan Senbang Environmental Testing Technology Co.,Ltd.,Xuchang 461100,China)

机构地区：[1]众平检测有限公司,河南许昌461100 [2]河南森邦环境检测技术有限公司,河南许昌461100

出　　处：《食品安全导刊》2022年第20期97-99,共3页China Food Safety Magazine

摘　　要：目的:本研究旨在建立气相色谱-质谱联用法(Gas Chromatography-Mass Spectrometer,GCMS)测定苹果中五氯硝基苯的检测方法。方法:样品经乙腈提取,固相萃取仪净化,浓缩定容后用GC-MS在SCAN和SIM模式下进行测定,通过保留时间、特征离子及其相对丰度定性,内标法定量。结果:在0.125~4.000μg/mL,五氯硝基苯的峰面积与线性关系良好,相关系数R^(2)为0.9999,方法的检出限(LOD)为0.0078 mg/kg,定量限(LOQ)为0.0250 mg/kg。在LOQ~10 LOQ添加水平,五氯硝基苯的平均回收率在83.5%~94.9%,相对标准偏差为0.71%~2.34%(n=6)。结论:该方法具有准确、高效、灵敏度高、重现性好等优势,可以满足苹果中五氯硝基苯的分析要求。Objective:In this paper,a analytical method was developed for determination of quintozene in apple by Gas Chromatography-mass Spectrometry.Method:Samples were extracted by acetonitrile and purified by solid phase extraction,after concentration and constant volume,it was determined by GC-MS in SCAN and SIM modes,Qualitative analysis by retention time,characteristic ions and their relative abundance,Internal standard method.Result:The mass concentration of quintozene ranges from 0.125~4.000μg/mL,The linear relationship is good,The correlation coefficients R^(2) were 0.9999,the LOD of quintozene was 0.0078 mg/kg,the LOQ of quintozene was 0.0250 mg/kg.The recovery of quintozene ranged from 83.5%to 94.9%at spiked level of LOQ~10 LOQ,the relative standard deviation was varied from 0.71%to 2.34%(n=6).Conclusion:The method has the advantages of accuracy,high efficiency,high sensitivity and good reproducibility.It is effective to determinate quintozene residue in apple.

关 键 词：苹果 五氯硝基苯 气相色谱-质谱联用 内标法定量 

分 类 号：O657.63[理学—分析化学] TS255.7[理学—化学]