Sin-QuEChERS-GC-MS/MS法快速测定人参中47种残留农药  

Rapid determination of 47 kinds of pesticide residues in Ginseng Radix et Rhizoma by Sin-QuEChERS-GC-MS/MS

作　　者：高娜 乔颖 刘雪红 李军 葛祥武 孙楠 朱殿龙 阮维斌[2] 郑丽新 GAO Na;QIAO Ying;LIU Xue-hong;LI Jun;GE Xiang-wu;SUN Nan;ZHU Dian-long;RUAN Wei-bin;ZHENG Li-xin(Dalian Center for Food and Drug Control and Certification,Dalian 116037,China;College of Life Science,Nankai University,Tianjin 300071,China)

机构地区：[1]大连市检验检测认证技术服务中心,大连116037 [2]南开大学生命科学学院,天津300071

出　　处：《药物分析杂志》2022年第12期2145-2154,共10页Chinese Journal of Pharmaceutical Analysis

基　　金：辽宁省重点研究计划项目(2020JH2/10200002)。

摘　　要：目的:建立Sin-QuEChERS技术结合气相色谱串联质谱法同时快速测定人参中47种残留的农药。方法:人参粉末样品加水经1%甲酸乙腈提取,采用QuEChERS提取盐包进行盐析,提取液经Sin-QuEChERS-Nano净化管1步净化,浓缩,加入内标磷酸三苯酯,采用GC-MS/MS进行检测。选用DB-5MS色谱柱进行分离,进样口温度为250℃,初始流速为1.2 mL·min^(-1),电子轰击离子源,多反应监测模式,内标法定量。结果:47种目标化合物在一定的含量范围内线性关系良好,相关系数均大于0.9931,低、中、高3个水平加样回收率均在72.5%~116.0%,RSD为0.70%~13.9%,定量下限为0.01 mg·kg^(-1);对30批人参样品进行测定,共检出9种农药,其中五氯硝基苯检出率最高为56.7%。结论:该方法高效、灵敏、准确,适合于人参中多种农药的快速筛查和定量检测,具有较强的实用价值。Objective:To establish a rapid analysis method of Sin-QuEChERS technology combined with gas chromatography-tandem mass spectrometry(GC-MS/MS)to detect 47 pesticide residues in Ginseng Radix et Rhizoma.Methods:Ginseng Radix et Rhizoma powder was treated with water and extracted with 1%formic acid-acetonitrile,salted out by the QuEChERS package and purified with Sin-QuEChERS tube in one step,after concentrating internal standard triphenyl phosphate was added,then detected by GC-MS/MS.DB-5MS column was used,the inlet temperature was set to 250℃,the initial velocity was 1.2 mL·min^(-1),the electron impact ion source was applied with multiple reaction monitoring(MRM)modes,and internal standard method wasused for quantification.Results:The 47 target compounds showed good linearities within a certain content ranges,with the correlation coefficients(r^(2))above 0.9931.At the low,medium,and high addition levels,the average recoveries were in the range of 72.5%-116.0%with the relative standard deviations(RSDs)within 0.70%-13.9%.And the limits of quantitation(LOQs)for the 47 compounds were 0.01 mg·kg^(-1).Thirty batches of Ginseng Radix et Rhizoma samples were tested and nine pesticides were detected,among them,quintozene showed the highest detection rate of 56.7%.Conclusion:The detecting method is efficient,sensitive,and accuracy,which can be used for rapid screening and quantitative detection of various pesticide residues in ginseng,and has strong practical value.

关 键 词：Sin-QuEChERs 气相色谱-串联质谱法 人参 农药残留 五氯硝基苯 快速分析 内标法 

分 类 号：R917[医药卫生—药物分析学]