亲水亲油平衡固相萃取小柱结合气相色谱-串联质谱法测定大果木姜子药材中禁用农药残留  

Determination of Forbidden Pesticide Residues in Cinnamomum Migao by HLB-SPE with GC-MS/MS

作　　者：汪洋 蒋礼 黎雪 朱帮会 郑林[1,2] 李勇军[1,2,3] 马雪 WANG Yang;JIANG Li;LI Xue;ZHU Banghui;ZHENG Lin;LI Yongjun;MA Xue(Guizhou Medical University Engineering Research Center for the Development and Application of Ethnic Medicine and TCM·State Key Laboratory for Functions and Applications of Medicinal Plants,Guiyang,Guizhou,China 550004;Guizhou Provincial Key Labo-ratory for Pharmaceutics·National Engineering Research Center of Miao′s Medicines,Guizhou Medical University,Guiyang,Guizhou,China 550004;College of Pharmacy,Guizhou Medical University,Guiyang,Guizhou,China 561113)

机构地区：[1]贵州医科大学民族药与中药开发应用教育部工程研究中心·省部共建药用植物功效与利用国家重点实验室,贵州贵阳550004 [2]贵州医科大学贵州省药物制剂重点实验室·国家苗药工程技术研究中心,贵州贵阳550004 [3]贵州医科大学药学院,贵州贵阳561113

出　　处：《中国药业》2025年第1期62-68,共7页China Pharmaceuticals

基　　金：国家自然科学基金委-贵州喀斯特中心项目[U1812403-5-1];贵州省科技计划项目[黔科合中引地〔2023〕006]。

摘　　要：目的建立检测大果木姜子药材中禁用农药残留量的亲水亲油平衡(HLB)固相萃取小柱结合气相色谱-串联质谱(GC-MS/MS)法。方法样品经正己烷-乙腈-饱和氯化钠水溶液三相分配除去部分杂质,农药组分转移至乙腈提取液中,以加强型HLB固相萃取小柱净化,采用GC-MS/MS多反应监测模式(MRM)进行测定,以基质内标法定量。结果大果木姜子药材中禁用农药残留物在各自质量浓度范围内与待测成分峰面积/内标峰面积线性关系良好(R2>0.99,n=6);在3个添加水平下,平均回收率为61.80%~125.53%,RSD为1.90%~14.77%(n=6)。15批大果木姜子药材中均未检出禁用农药残留。结论该方法操作简便、准确性和重复性好,可用于大果木姜子药材中禁用农药残留量的测定。Objective To establish a hydrophilic-lipophilic equilibrium(HLB)-solid-phase extraction(SPE)combined with gas chromatography-tandem mass spectrometry(GC-MS/MS)method for determination of forbidden pesticide residues in Cinnamomum migao.Methods The sample was partitioned into three-phases distribution with n-hexane-acetonitrile-saturated sodium chloride aqueous solution to remove some impurities.The pesticide components were transferred to the acetonitrile extraction solution and purified by the enhanced HLB-SPE column.GC-MS/MS with multi-reaction monitoring mode(MRM)was used for determination,with matrix internal standard method for quantification.Results There was a good linear relationship between the peak area of the tested component and the peak area of the internal standard within the respective mass concentration ranges of the forbidden pesticide residues in Cinnamomum migao(R2>0.99,n=6).At three levels of addition,the average recoveries were in the range of 61.80%-125.53%,with RSDs of 1.90%-14.77%(n=6).No forbidden pesticide residue was detected in the 15 batches of Cinnamomum migao.Conclusion This method is simple,accurate,and has good repeatability,which can be used for the determination of forbidden pesticide residues in Cinnamomum migao.

关 键 词：大果木姜子 气相色谱-串联质谱法 亲水亲油平衡 固相萃取 禁用农药残留 

分 类 号：R932[医药卫生—生药学] R284.1[医药卫生—药学] R286.0