基于自建数据库的超高效液相色谱-四极杆-飞行时间质谱法定量测定玉米中5种真菌毒素  

Determination of 5 kinds of mycotoxins in Zea mays by ultra performance liquid chromatography-quadrupole-time-of-flight mass spectrometry based on self-established database

作　　者：梁艳婷[1] 杨奉筠 贾艳丰 张鑫宇 刘蓉 柳明[1] LIANG Yan-Ting;YANG Feng-Jun;JIA Yan-Feng;ZHANG Xin-Yu;LIU Rong;LIU Ming(Chifeng Center for Disease Control and Prevention,Inner Mongolia,Chifeng 024000,China;SCIEX Corporation,Beijing 100000,China)

机构地区：[1]内蒙古赤峰市疾病预防控制中心,赤峰024000 [2]中国SCIEX公司,北京100000

出　　处：《食品安全质量检测学报》2024年第20期279-287,共9页Journal of Food Safety and Quality

基　　金：赤峰市科协自然科学科研课题项目(20230130)。

摘　　要：目的基于自建数据库建立超高效液相色谱-四极杆-飞行时间质谱法(ultra performance liquid chromatography-quadrupole-time-of-flight mass spectrometry,UPLC-Q-TOF/MS)测定玉米中玉米赤霉烯酮(zearalenone,ZEN)、交链孢酚(alternariol,AOH)、交链孢酚单甲醚(alternariol monomethyl ether,AME)、细交链孢菌酮酸(tenuazonic acid,TeA)、腾毒素(tentoxin,TEN)5种负离子真菌毒素的方法。方法样品经提取、净化、复溶后,采用Waters UPLC BEH C18色谱柱进行分离后在信息依赖型的扫描(information-dependent scanning,IDA)负离子模式采集。SCIEX OS Explorer条件下确定5种负离子真菌毒素精确数据录入数据库。在玉米基质中以筛查检出限作为主要参数验证方法。结果高分辨模式下采用加内标来改善基质干扰系数校正,在玉米基体中对真菌毒素类的基质效应θ进行计算,θ在0.84~1.10之间。基质匹配内标校准定量,5种负离子真菌毒素在范围内具有较好的线性关系,相关系数(r)为0.9972~0.9993。5种负离子真菌毒素的检出限为0.2~5.0μg/kg。玉米基质在低、中、高3个加标水平下的平均回收率为83.9%~119.4%,相对标准偏差为2.39%~11.37%(n=6)。用此方法检测内蒙地区120份玉米中5种负离子真菌毒素都有检出,TeA和TEN检出率高达98.1%和95.6%。有3份玉米中ZEN超过100μg/kg限量标准,应引起相关监管部门重视。结论本方法具有高通量、精准、快速等优点,可以在无标准物质情况下对玉米中ZEN、AOH、AME、TeA、TEN的定性筛查,为玉米中这5种真菌毒素污染监测提供技术支持。Objective To establish a method for determining 5 kinds of negative ion mycotoxins in Zea mays,namely zearalenone(ZEN),alternariol(AOH),alternariol monomethyl ether(AME),tenuazonic acid(TeA),and tentoxin(TEN),by ultra performance liquid chromatography-quadrupole-time-of-flight mass spectrometry(UPLC-Q-TOF/MS)based on a self-established database.Methods After extraction,purification and redissolution of the sample,separation was carried out using Waters UPLC BEH C18 chromatographic column and then collection was performed in negative ion mode of information-dependent scanning(IDA).Under the conditions of SCIEX OS Explorer,the accurate data of 5 kinds of negative ion mycotoxins were determined and entered into the database.The limit of detection for screening in corn matrix was used as the main parameter to verify the method.Results In high-resolution mode,internal standard addition was used to improve the correction of matrix interference coefficient.The matrix effectθof mycotoxins was calculated in corn matrix,andθwas between 0.84 and 1.10.Matrix-matched internal standard calibration was used for quantification.The 5 kinds of negative ion mycotoxins had a good linear relationship within the range,and the correlation coefficient(r)was between 0.9972 and 0.9993.The limits of detection of 5 kinds of negative ion mycotoxins were 0.2–5.0μg/kg.The average recoveries of corn matrix at low,medium and high spiked levels were 83.9%–119.4%,and the relative standard deviations were 2.39%–11.37%(n=6).Using this method,all 5 kinds of negative ion mycotoxins were detected in 120 corn samples from Inner Mongolia.The detection rates of TeA and TEN were as high as 98.1%and 95.6%.In 3 corn samples,ZEN exceeded the limit standard of 100μg/kg,which should attract the attention of relevant regulatory departments.Conclusion This method has the advantages of high throughput,accuracy and speed.It can qualitatively screen ZEN,AOH,AME,TeA and TEN in corn without standard substances and provide technical support for the monitoring

关 键 词：超高效液相色谱-四极杆-飞行时间质谱法 自建数据库 玉米 负离子 真菌毒素 

分 类 号：O657.63[理学—分析化学] TS213.4[理学—化学]