食品研究与开发:2026,47(2):156-163
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分散固相萃取UPLC-QTRAP-MS/MS定量分析有毒丝膜菌中奥来毒素
瞿广胜1,2,李显娱1,2*,徐林1,2,戴乾1,2,王灵秋1,2,赵连伟1,韦刚1,2,刘钰洁1,2
(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)
Quantitative Analysis of Orellanine in Poisonous Cortinarius by Dispersive Solid-Phase Extraction and UPLC-QTRAP-MS/MS
QU Guangsheng1,2,LI Xianyu1,2*,XU Lin1,2,DAI Qian1,2,WANG Lingqiu1,2,ZHAO Lianwei1,WEI Gang1,2,LIU Yujie1,2
(1.Anshun Center for Disease Control and Prevention,Anshun 561000,Guizhou,China;2.Anshun Key Laboratory of Food Safety Risk Monitoring,Anshun 561000,Guizhou,China)
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投稿时间:2024-07-31    
中文摘要: 为建立丝膜菌属类食源性中毒定量检测和快速筛查方法,丝膜菌样本经乙腈溶液超声提取,分散固相萃取净化,基于超高效液相色谱串联质谱(ultra performance liquid chromatography-tandem mass spectrometry,UPLC-MS/MS)和信息依赖采集增强子离子扫描(multiple reaction monitoring-information dependent acquisition-enhanced product ion scan,MRM-IDA-EPI)对奥来毒素进行定量分析和快速筛查。结果表明,通过对奥来毒素进行低、中、高浓度水平加标回收试验,加标回收率为91.7%~107.7%、精密度为1.1%~2.5%;奥来毒素在0.020~0.500 μg/mL浓度范围内线性相关系数大于0.999 0;方法检出限和定量限分别为10 μg/kg和30 μg/kg,前处理方法基质效应系数K值 为0.999。综上,所建立的奥来毒素UPLC-MS/MS和MRM-IDA-EPI测定方法结果准确、重现性好、灵敏度高,适用于有毒丝膜菌引起的食源性中毒定量分析和快速筛查。
Abstract:To establish a quantitative detection and rapid screening method for foodborne poisoning caused by cortinarius.Cortinarius samples were extracted using an acetonitrile solution via ultrasonic extraction and purified through dispersive solid-phase extraction.Quantitative analysis and rapid screening of orellanine were performed based on ultra performance liquid chromatography-tandem mass spectrometry (UPLC-MS/MS) and multiple reaction monitoring-information dependent acquisition-enhanced product ion scan(MRM-IDA-EPI).The results showed that through spiked recovery tests at low,medium,and high concentration levels,the spiked recovery rate of orellanine ranged from 91.7% to 107.7%,with a precision of 1.1%-2.5%.The linear correlation coefficient of orellanine was greater than 0.999 0 within the concentration range of 0.020-0.500 μg/mL.The method's detection limit and quantification limit were 10 μg/kg and 30 μg/kg,respectively,and the matrix effect coefficient K of the pretreatment method was 0.999.In summary,the established UPLC-MS/MS and MRMIDA-EPI determination methods for orellanine are accurate,with good reproducibility and high sensitivity,and they are suitable for quantitative analysis and rapid screening of foodborne poisoning caused by poisonous cortinarius.
文章编号:202602020     中图分类号:    文献标志码:
基金项目:贵州省科学技术基金项目(黔科合支撑[2021]一般023);安顺市科技计划项目(安市科社〔2021〕16 号);安顺市科技创新平台建设项目(安市科平[2022]1号)
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