磁固相萃取-气相色谱-质谱法测定饮料中罂粟碱  

Magnetic Solid Phase Extraction-gas Chromatography-mass Spectrometry for Analysis of Papaverine in Beverages

作　　者：田洁 曹淑瑞 苏泓滔 巫端浩 刘正宏[1] TIAN Jie;CAO Shurui;SU Hongtao;WU Duanhao;LIU Zhenghong(Forensic Identification Center,Southwest University of Political Science and Law,Chongqing 401120,China;Forensic Identification Center and Criminal Investigation School,Southwest University of Political Science and Law,Chongqing 401120,China)

机构地区：[1]西南政法大学鉴定中心,重庆401120 [2]西南政法大学鉴定中心,刑事侦查学院,重庆401120

出　　处：《现代食品科技》2023年第8期311-318,共8页Modern Food Science and Technology

基　　金：“成渝地区双城经济圈建设”科技创新项目(KJCXZD2020016);重庆市教委项目(KJZD-K202100301);重庆市自然科学基金面上项目(cstc2021jcyj-msxmX0715);重庆市自然科学基金面上项目(cstc2021jcyj-msxmX0715);重庆市渝北区科技局项目(2021(农社)13);西南政法大学人才引进项目(2021-XZRCXM005)。

摘　　要：该研究基于磁性固相萃取-气相色谱-质谱(Magnetic Solid Phase Extraction-Gas Chromatography-Mass Spectrometry,MSPE-GC-MS)建立了饮料中罂粟碱的测定方法,成功地合成了一种具有良好吸附性能的磁性氧化石墨烯纳米复合材料,对该纳米复合材料进行了多种表征。采用单因素实验和响应面优化法(Response Surface Methodology,RSM)设计实验优化了样品吸附和解吸条件(吸附时间、吸附剂用量、溶液pH值、洗脱溶剂和解吸时间),确定最优实验条件为:磁性氧化石墨烯用量15 mg,溶液pH值7,吸附时间30 min,解吸剂(甲醇:氨水=99:1),解吸剂体积2 mL,解吸时间6 min。结果表明在优化的条件下,在0.10~2.00μg/mL的浓度范围内,所得的罂粟碱线性关系良好,其相关系数R^(2)>0.999。利用该方法测定了3种饮料中罂粟碱的含量,在3个不同添加水平(0.10、1.00和2.00μg/mL)的加标回收率在98.43%~105.00%范围内,相对标准偏差在0.61%~3.50%范围内。磁性氧化石墨烯作为固相萃取材料,结合气相色谱-质谱(Gas Chromatography-Mass Spectrometry,GC-MS),既能简便快速提取目标物质,又能准确定量,回收率高,重现性好,适用于饮料中罂粟碱的检测。An effective method to detect papaverine in beverages was established based on magnetic solid phase extraction–gas chromatography–mass spectrometry(MSPE-GC-MS).A nanocomposite of magnetic graphene oxide with excellent adsorption properties was successfully synthesized,and its properties were analyzed.The adsorption and desorption conditions(adsorbent dosage,adsorption time,solution pH,elution solvent,and desorption time)were optimized using single-factor experiments,Box-Behnken design(BBD)experiments,and response surface methodology(RSM).The optimal experimental conditions were as follows:magnetic graphene oxide dosage,15 mg;pH of solution,7;adsorption time,30 min;elution solvent,2 mL methanol ammonium hydroxide(99:1);and desorption time,6 min.Under optimal conditions,a good linear detection of papaverine was obtained in the range of 0.10~2.00μg/mL(R^(2)>0.999).The content of papaverine in three beverages was determined using the proposed method.The spike recovery rates of papaverine at three different levels(0.10,1.00,and 2.00μg/mL)were 98.43%~105.00%,with relative standard deviations of 0.61%~3.50%.Solid-phase extraction using magnetic graphene oxide combined with GC-MS is a suitable approach for the detection of papaverine.This method not only facilitates efficient and rapid extraction of the target substances,but also ensures quantitative accuracy,with a high recovery rate and excellent reproducibility.

关 键 词：磁性固相萃取 气相色谱-质谱 罂粟碱 检测 

分 类 号：TS27[轻工技术与工程—农产品加工及贮藏工程] O657.63[轻工技术与工程—食品科学与工程]