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
瞿广胜 1李显娱 1戴乾 1徐林 1韦刚 1刘钰洁 1蔡贵香 1赵连伟2
作者信息
- 1. 安顺市疾病预防控制中心,贵州安顺 561000;安顺市食品安全风险监测重点实验室,贵州安顺 561000
- 2. 安顺市疾病预防控制中心,贵州安顺 561000
- 折叠
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.
Abstract
[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 purifica-tion 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 coef-ficient (r) of the coprine standard curve was>0.9990. The limit of detection (LOD,S/N=3) and limit of quantitation (LOQ) were 2 μg/kg and 6 μg/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-IDA-EPI 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-EPIKey words
coprinus/coprine/gel permeation chromatography(GPC)/ultra performance liquid chromatography-tandem mass spectrometry(UPLC-MS/MS)/MRM-IDA-EPI引用本文复制引用
出版年
2024
国家科技期刊平台
NSTL
万方数据