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10~200μg/L线性范围内线性关系良好(R^(2)>0.9985),检出限和定量限分别为0.1~13.0μg/kg和0.3~40.0μg/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。
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 10-200μg/L(R^(2)>0.9985),and the limits of detection and quantification were 0.1-13.0μg/kg and 0.3-40.0μg/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.
作者
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
AI Daoying;ZHENG Yirou;HUANG Zhanrui;ZHAO Liangzhong;LIN Lidan;ZHOU Hengping;ZHOU Kai;ZHOU Jinsong;YIN Shixian(College of Food and Chemical Engineering,Shaoyang University,Hunan Provincial Key Laboratory of Soybean Products Processing and Safety Control,Shaoyang 422000,China;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;Pingjiang Jinzai Food Co.Ltd.,Yueyang 414000,China)
出处
《食品与发酵工业》
CAS
CSCD
北大核心
2023年第3期306-313,共8页
Food and Fermentation Industries
基金
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)。
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
brine
mycotoxin
high performance liquid chromatography tandem mass spectrometry
isotope internal standard
methodological verification
作者简介
第一作者:艾道迎,硕士研究生;共同第一作者:郑奕柔,助理工程师;共同通信作者:黄展锐,博士,E-mail:zhangrui_huang@163.com;共同通信作者:赵良忠,教授,sys169@163.com。
