基于GPC/UPLC-MS/MS定量分析鬼伞菌属中的鬼伞菌素  

Quantitative Analysis of Coprine in Coprinus Based on GPC/UPLC-MS/MS

作　　者：瞿广胜 李显娱 戴乾[1,2] 徐林 韦刚[1,2] 刘钰洁 蔡贵香[1,2] 赵连伟 QU Guang-sheng;LI Xian-yu;DAI Qian;XU Lin;WEI Gang;LIU Yu-jie;CAI Gui-xiang;ZHAO Lian-wei(Anshun Centers For Disease Control And Prevention,Anshun 561000,China;Anshun Key Laboratory of Food Safety Risk Monitoring,Anshun 561000,China)

机构地区：[1]安顺市疾病预防控制中心,贵州安顺561000 [2]安顺市食品安全风险监测重点实验室,贵州安顺561000

出　　处：《中国食物与营养》2024年第11期41-47,共7页Food and Nutrition in China

基　　金：贵州省科学技术基金项目(项目编号:黔科合支撑[2021]一般023);安顺市科技计划项目(项目编号:安市科社[2021]16号);安顺市科技创新平台建设项目(项目编号:安市科平[2022]1号)。

摘　　要：目的:建立基于凝胶净化色谱(GPC)前处理方法的鬼伞菌素超高效液相色谱串联质谱(UPLC-MS/MS)和信息依赖增强型子离子扫描(MRM-IDA-EPI)分析方法,为鬼伞菌属类食源性中毒定量检测、快速筛查提供参考依据。方法:鬼伞菌属或血液样本经甲醇水-乙腈混合溶剂超声提取,GPC分离净化UPLC-MS/MS定量检测和MRM-IDA-EPI筛查分析。结果:对鬼伞菌素进行低、中、高浓度水平加标回收试验,加标回收率为87.3%~93.7%、精密度(RSD)为0.9%~4.2%;鬼伞菌素在50~500μg/L浓度范围内相关系数(r)>0.9990;方法检出限(LOD,S/N=3)和定量限(LOQ)分别为2、6μg/kg,GPC前处理净化方法基质效应系数K=1.007。结论:所建立的鬼伞菌素GPC净化方法基质干扰小,UPLC-MS/MS和MRM-IDA-EPI分析方法结果准确、重现性好、灵敏度高,适用多种样本类型的分析和筛查。【Objective】The analytical methods of ultrahigh performance liquid chromatography tandem mass spectrometry(UPLC-MS/MS)and information dependent enhanced sub ion scanning(MRM-IDA-EPI)for coprine based on the pretreatment method of gel purification chromatography(GPC)were established to provide reference basis for quantitative detection and rapid screening of coprinus food borne poisoning.【Method】The samples of coprinus or blood were extracted by ultrasonic extraction with methanol-water-acetonitrile mixed solvent,separated and purified by GPC,quantitatively detected by UPLC-MS/MS,and screened and analyzed by MRM-IDA-EPI.【Result】The yield of coprine obtained by this purification method was 128 mg/kg,and the purity was HPLC level.The recoveries of low,medium and high concentrations of coprine were 87.3%—93.7%,and the precision(RSD)was 0.9%—4.2%.The linear correlation coefficient(r)of the coprine standard curve was>0.9990.The limit of detection(LOD,S/N=3)and limit of quantitation(LOQ)were 2μg/kg and 6μg/kg,respectively.The matrix effect coefficient of the GPC pre-treatment purification method was K=1.007.【Conclusion】The established GPC purification method for anamorph species of coprine had low matrix interference,and the UPLC-MS/MS and MRM-IDAEPI analysis methods had accurate results,good reproducibility,and high sensitivity,making them suitable for analysis and screening of multiple sample types.

关 键 词：鬼伞菌属 鬼伞菌素 凝胶净化色谱 超高效液相色谱串联质谱 MRM-IDA-EPI 

分 类 号：TS219[轻工技术与工程—粮食、油脂及植物蛋白工程] O657.63[轻工技术与工程—食品科学与工程]