UPLC-MS/MS法测定蘑菇、科研用人血清和尿液中5种鹅膏肽类毒素的方法研究  

Determination of 5 Amanita Peptide Toxins in Mushrooms、Human Serum and Urine for Scientific Research by UPLC-MS/MS

作　　者：曾豪威 戚平 林子豪 彭名军 陈婷 毛新武 ZENG Haowei;QI Ping;LIN Zihao;PENG Mingjun;CHEN Ting;MAO Xinwu(Guangzhou Institute for Food Inspection,Guangzhou 511400,China)

机构地区：[1]广州市食品检验所,广州511400

出　　处：《食品与发酵科技》2024年第3期117-123,共7页Food and Fermentation Science & Technology

基　　金：国家市场监督管理总局科技计划项目(2020MK129);广州市市场监督管理局科技项目(2022kj41)。

摘　　要：本文建立了适用于蘑菇、科研用人血清和尿液样本中5种鹅膏肽类毒素的超高效液相色谱-串联质谱分析方法。样品经乙腈提取和水稀释后,采用XSelect HSS T3(3mm×150mm,2.5μm)进行色谱分离,以0.01%甲酸-乙腈和水为流动相进行梯度洗脱,串联质谱-电喷雾离子源(ESI)正离子模式检测。5种鹅膏肽类毒素在1~50ng/mL范围内呈现良好线性关系,相关系数均大于0.99,蘑菇样品方法检出限为0.06 mg/kg,定量限为0.2 mg/kg,在3个加标水平下平均回收率为92.6%~124.0%,相对标准偏差为3.2%~14.8%(n=6);科研用人血清样品方法检出限为0.01 mg/L,定量限为0.03 mg/L,在3个加标水平下平均回收率为85.5%~123.5%,相对标准偏差为0.9%~16.4%(n=6);科研用人尿液样品方法检出限为0.005 mg/L,定量限为0.015 mg/L,在3个加标水平下平均回收率为84.8%~119.3%,相对标准偏差为0.9%~16.1%(n=6)。本方法简单快速,高效准确,适用于蘑菇、科研用人血清和尿液中5种鹅膏肽类毒素的快速检测,为突发事件应急检验提供参考依据。An ultra-performance liquid chromatography-tandem mass spectrometry(UPLC-MS/MS)method was developed for the determination of five Amanita peptide toxins in mushrooms,human serum and urine samples used for scientific research.The samples were extracted with acetonitrile and diluted with water,and then separated by XSelect HSS T3(3 mm×150 mm,2.5μm)with 0.01%formic acid-acetonitrile and water as mobile phase for gradient elution,and detected by tandem mass spectrometry electro-spray ionization(ESI)in positive ion mode.The five Amanita peptide toxins showed a good linear relationship in the range of 1~50 ng/mL,and the correlation coefficients were all greater than 0.99.The detection limit of the mushroom samples method was 0.06 mg/kg,the limit of quantitation was 0.2 mg/kg,the average recoveries for three spiked levels were 92.6%~124.0%,and the relative standard deviations were 3.2%~14.8%(n=6).The detection limit of the human serum samples used in scientific research was 0.01 mg/L,the limit of quantitation was 0.03 mg/L,the average recoveries for three spiked levels were 85.5%~123.5%,and the relative standard deviations were 0.9%~16.4%(n=6).The detection limit of the human urine samples used in scientific research was 0.005 mg/L,the limit of quantitation was 0.015 mg/L.the average recoveries for three spiked levels were 84.8%~119.3%,and the relative standard deviations were 0.9%~16.1%(n=6).This method is simple,rapid,efficient and accurate,and is suitable for the rapid detection of five Amanita peptide toxins in mushrooms,serum and urine for scientific research,and has a function of providing reference for the emergency test of emergencies.

关 键 词：鹅膏肽类毒素 蘑菇 血清 尿液 超高效液相色谱-串联质谱 

分 类 号：TS207.3[轻工技术与工程—食品科学]