食品与发酵工业 >

2023 , Vol. 49 >Issue 3: 306 - 313

DOI: https://doi.org/10.13995/j.cnki.11-1802/ts.032719

分析与检测

湘派卤汁中10种真菌毒素液相色谱串联质谱法的建立与评价

  • 艾道迎 ,
  • 郑奕柔 ,
  • 黄展锐 ,
  • 赵良忠 ,
  • 林丽丹 ,
  • 周衡平 ,
  • 周凯 ,
  • 周劲松 ,
  • 尹世鲜
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  • 1(邵阳学院 食品与化学工程学院,豆制品加工与安全控制湖南省重点实验室,湖南 邵阳,422000)
    2(深圳市通量检测科技有限公司,广东省高特异性生物快速检测工程技术研究中心,广东 深圳,518038)
    3(平江县劲仔食品有限公司,湖南 岳阳,414000)
艾道迎硕士研究生和郑亦柔助理工程师为共同第一作者(黄展锐博士和赵良忠教授为共同通信作者,E-mail:zhangrui_huang@163.com;sys169@163.com)

收稿日期: 2022-06-22

  修回日期: 2022-07-20

  网络出版日期: 2023-03-03

基金资助

邵阳学院研究生科研创新项目(CX2021SY056);湖南省自然科学基金青年科学基金项目(2021JJ40514);湖南省教育厅科学研究优秀青年项目(20B530);湖南省科技创新计划资助目(2019TP1028,2019SK2122,2019NK4229,2022NK2039)

收起

Establishment and evaluation of LC-MS/MS method for ten mycotoxins in Xiangpai brine

  • AI Daoying ,
  • ZHENG Yirou ,
  • HUANG Zhanrui ,
  • ZHAO Liangzhong ,
  • LIN Lidan ,
  • ZHOU Hengping ,
  • ZHOU Kai ,
  • ZHOU Jinsong ,
  • YIN Shixian
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  • 1(College of Food and Chemical Engineering, Shaoyang University, Hunan Provincial Key Laboratory of Soybean Products Processing and Safety Control, Shaoyang 422000, China)
    2(Department of Industry-University-Research Collaboration, Shenzhen Total-Test Technology Co.Ltd., Guangdong Engineering Research Center of High Specificity Biological Rapid Detection, Shenzhen 518038, China)
    3(Pingjiang Jinzai Food Co.Ltd., Yueyang 414000, China)

Received date: 2022-06-22

  Revised date: 2022-07-20

  Online published: 2023-03-03

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摘要

建立基于液相色谱-串联质谱(liquid chromatography-tandem mass spectrometry,LC-MS/MS)测定湘派卤汁中10种真菌毒素的方法,并进行方法学验证及实际样品检测。样品中同步加入同位素内标经V(乙腈)∶V(水)∶V(乙酸)=84∶15∶1提取液超声波处理、离心提取后,取上清液和水稀释净化,甲醇-水溶液为流动相梯度洗脱,采用电喷雾正负离子的多反应离子监测模式,利用同位素内标定量法进行定性和定量分析。结果表明,10种真菌毒素在10~200 μg/L线性范围内线性关系良好(R2>0.998 5),检出限和定量限分别为0.1~13.0 μg/kg和0.3~40.0 μg/kg。10种真菌毒素的3个浓度水平加标回收率为78.6%~107.3%,相对标准偏差为2.2%~14.0%,符合方法学要求。该方法操作简便,回收率、灵敏度、检出限等均满足方法学要求,适用于卤汁中10种真菌毒素的测定。

关键词： 卤汁; 真菌毒素; 液相色谱-串联质谱; 同位素内标; 方法学验证

本文引用格式

艾道迎 , 郑奕柔 , 黄展锐 , 赵良忠 , 林丽丹 , 周衡平 , 周凯 , 周劲松 , 尹世鲜 . 湘派卤汁中10种真菌毒素液相色谱串联质谱法的建立与评价[J]. 食品与发酵工业, 2023 , 49(3) : 306 -313 . DOI: 10.13995/j.cnki.11-1802/ts.032719

Abstract

This study established a method for the determination of ten mycotoxins in Xiangpai brine, and carried out methodological validation and actual sample detection based on high performance liquid chromatography-tandem mass spectrometry(LC-MS/MS). The sample (added with isotope internal standard synchronously) was extracted by ultrasound and centrifugation with V(acetonitrile)∶V(water)∶V(acetic acid) =84∶15∶1, and the supernatant was diluted and purified with water. Methanol-water solution was used as mobile phase gradient elution, and electrospray positive and negative multi-reaction ion monitoring mode was adopted. Qualitative and quantitative analysis was carried out by isotope internal standard quantitative method. The results showed that the linearity of the ten mycotoxins were good in the range of 10-200 μg/L (R2>0.998 5), and the limits of detection and quantification were 0.1-13.0 μg/kg and 0.3-40.0 μg/kg, respectively. The spiked recoveries of the ten mycotoxins at the three concentration levels were 78.6%-107.3%, and the relative standard deviations were 2.2%-14.0%, which met the requirements of methodology. The method is easy to operate, and the recovery rate, sensitivity and detection limit all meet the methodological requirements. Thus, this method is suitable for the determination of ten mycotoxins in brine.

Key words： brine; mycotoxin; high performance liquid chromatography tandem mass spectrometry; isotope internal standard; methodological verification

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