免疫亲和柱净化-超高效液相色谱串联质谱法同时测定火锅底料中的5种真菌毒素
Simultaneous Determination of 5 Mycotoxins in Hot Pot Seasoning by Ultra Performance Liquid Chromatography-Tandem Mass Spectrometry with Immunoaffinity Column Clean-Up
孟春杨 1吴玉田 1邹璐 1钟雪 1杨绍群 1刘文政 1周贻兵1
作者信息
- 1. 贵州省疾病预防控制中心,贵州贵阳 550004
- 折叠
摘要
目的:建立复合免疫亲和柱净化、超高效液相色谱串联质谱检测火锅底料中的黄曲霉毒素B1(Aflatoxins B1,AFB1)、黄曲霉毒素B2(Aflatoxins B2,AFB2)、黄曲霉毒素G1(Aflatoxins G1,AFG1)、黄曲霉毒素G2(Aflatoxins G2,AFG2)、赭曲霉毒素A(Ochratoxin A,OTA)的方法.方法:样品提取后,经复合免疫亲和柱净化,以0.1％甲酸水和甲醇为流动相梯度洗脱,用Agilent EclipsePlus C18 RRHD色谱柱分离,ESI+进行多反应监测,内标法定量.结果:5种真菌毒素的线性范围在0.1～10.0 ng/mL,相关系数(r)＞0.999,检出限0.1 μg/kg,定量限0.3 μg/kg.3个加标水平下(0.2、5.0、10.0μg/kg)的回收率在81.38％～97.87％之间,相对标准偏差为0.79％～6.18％.结论:该方法快速准确,可用于火锅底料中5种真菌毒素的定性、定量检测.
Abstract
Objective:A method for the determination of aflatoxins B1(AFB1),aflatoxins B2(AFB2),aflatoxins G1(AFG1),aflatoxins G2(AFG2)and ochratoxin A in hot pot seasoning by ultra performance liquid chromatography-tandem mass spectrometry with immunoaffinity column clean-up was established.Methods:After extraction,the samples were purified by immunoaffinity column,eluted with 0.1％formic acid water and methanol as mobile phase gradient,separated by Agilent EclipsePlus C18 RRHD chromatographic column,ESI+was used for multiple reaction monitoring,and internal standard method was used for quantification.Results:Good linearity was obtained for 5 mycotoxins within the concentration range of 0.10-10.0 ng/mL,with the correlation coefficients(r)higher than 0.999,the limit of detection and the limit of quantification of the 5 mycotoxins were 0.1 μg/kg and 0.3 μg/kg.The average recovery rates at three concentrations of 0.20,5.0,10.0 μg/kg was in the range of 81.51％-97.87％,with relative standard deviations of 0.79％-6.18％.Conclusion:The results showed that this method could be used to determine the quality and quantity of 5 mycotoxins rapidly and accurately.
关键词
免疫亲和柱/超高效液相色谱串联质谱/火锅底料/真菌毒素Key words
immunoaffinity column/ultra performance liquid chromatography-tandem mass spectrometry/hot pot seasoning/mycotoxins引用本文复制引用
基金项目
贵州省卫生健康委科学技术基金(gzwkj2022-268)
贵州省科学(青年)技术基金(2021-E1-2青)
出版年
2024
NETL
NSTL
万方数据