Determination of 7 Mycotoxin Contaminants in Spices by Ultra-high Performance Liquid Chromatography-tandem Mass Spectrometry
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摘要: 建立了同时测定香辛料中7种真菌毒素的超高效液相色谱-串联质谱分析方法(UPLC-MS/MS)。选用香辛料中的辣椒、花椒和八角为研究对象,粉碎后的样品用70%甲醇水溶液提取,6合1免疫亲和柱净化,ACQUITY UPLC HSS T3色谱柱分离,超高效液相色谱-串联质谱测定,电喷雾正离子(ESI+)多反应离子监测方式监测,外标法定量。结果表明,7种真菌毒素在各自的线性响应范围内线性关系良好,相关系数均不低于0.995,7种真菌毒素的定量限为0.5~20 μg/kg。低、中、高3个加标水平平均回收率(n=6)为67.25%~113.47%,相对标准偏差(RSD)为1.07%~10.20%。该方法具有前处理简单、净化效果好、灵敏度高和高通量检测的优点,适用于香辛料中多组分真菌毒素残留的分离和检测。
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关键词:
- 香辛料 /
- 真菌毒素 /
- 高通量检测 /
- 超高效液相色谱-串联质谱
Abstract: A method was developed for the determination of 7 mycotoxins in spices by ultra-high performance liquid chromatography-tendem mass spectrometry (UPLC-MS/MS). Selection of spices in chili, pepper and star anise for the study, smashed samples were extracted with 70% methanol water solution, purified by multifunction immunological affinity column, isolated by ACQUITY UPLC HSS T3 chromatographic column, determined by ultra-efficient liquid chromatography-mass spectrometry. The mass spectrometry was conducted by using positive (ESI+) electrospray ionization and multi-reactions monitoring (MRM) models, with external standard method. The results indicated that 7 mycotoxins had good linear relationship, correlation coefficient were not less than 0.995, and the limit of quantitation (LOQ) for the range from 0.5 to 20 μg/kg. The average recovery rates at three levels of adding external standard were from 67.25% to 113.47%, with a relative standard deviation (RSD) varying from 1.07% to 10.20%. The method had simple process, good purification effect and the advantages of high sensitivity and high throughput detection, suitable for spices in multicomponent separation and detection of mycotoxin residues. -
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1. 刘妍妍，陈文璐，孙志刚，郑莹莹，李亚霖，郝婷婷. 乳清蛋白酶解物对酸奶品质及抗氧化活性的影响. 中国乳业. 2024(10): 84-92 . 
百度学术
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