应用超高压液相-质谱联用技术同时测定花生及其制品中的6种黄曲霉毒素  

Simultaneous determination of six aflatoxins contaminants in peanut and their derivative products by ultra-performance liquid chromatography tandem mass spectrometry

作　　者：蔡增轩[1] 潘红锋[2] 王丽丽[2] 韩铮[3] 任一平[1] 

机构地区：[1]浙江省疾病预防控制中心,杭州310009 [2]浙江工业大学药学院,杭州310014 [3]浙江大学药学院,杭州310000

出　　处：《中国卫生检验杂志》2009年第5期970-974,共5页Chinese Journal of Health Laboratory Technology

基　　金："浙江省分析测试"科技计划(2008F81G1360019)

摘　　要：目的：建立首次同时对花生及其制品中的6种黄曲霉毒素进行定性定量分析的超高效液相色谱三重四极杆质谱确证方法。方法：样品用84/16的乙腈/水混合液匀浆提取3 min,经一种创新型的自制混合固相萃取柱纯化后,进样,经Acquity UPLC HSS T3柱（100 mm×2.1 mm,1.7μm particle size;Waters,Milford,MA,USA）分离,在6 min内6种黄曲霉毒素即可得到完全分离。结果：标准曲线的线性范围分别是：AFTB1：0.08-10μg/kg,AFT B2：0.4-20μg/kg,AFTG1：1-20μg/kg,AFTG2：0.4-20μg/kg,AFTM1：0.4-20μg/kg,AFT M2：1-20μg/kg。加样平均回收率为：75.0%-86.9%,RSD为1.8%-9.4%,然后运用所建立的方法对20份不同产地不同批次的花生及其制品进行分析。结论：所建立的超高压液相质谱联用的方法能够显著的提高样品通量,减少溶剂的损耗,定量限LOQ能够满足欧盟相关的黄曲霉素的最低限量标准,首次在花生及其制品中发现黄曲霉毒素M1,M2的存在。此方法是一种快速、灵敏、准确、可靠的检测方法。Objective： A new separation and quantification method utilizing liquid chromatography under ultra - high - pressure in combination with tandem mass spectrometry （MS/MS） has been developed for simultaneous determination of the six aflatoxins （B1, B2, G1, G2 ,M1 ,M2） in peanuts and their derivative products. Methods：Homogenized samples were sequentially extracted by 84% % （v/v） of acetonitrile aqueous solution, cleaned up with self- made SPE columns, centrifuge, evaporate, re - dissolve and filtration. After injection, the analysis was performed on acquity UPLC HSS T3 column（ 100 mm × 2. 1 mm, 1. 8 μm particle size; Waters, Milford, MA, USA）using a mobile phase consisting of（A） water containing 0. 1% formic acid and （B） acetate/ methanol（50/50） with gradient elution. Results：The calibration curves were linear over the range of 0. 08 - 10. 0 μg/kg for aflatoxin B1, 0. 4 - 20. 0 μg/kg for aflatoxin B2, 1.0 - 20.0 μg/kg for aflatoxin G1, 0.4 - 20.0 μg/kg for aflatoxin G2, 0.4 20. 0μg/kg for aflatoxin M1, 1.0 - 20. 0 μg/kg for aflatoxin M2, respectively. The average recoveries ranged from 75.0% 86. 9% with RSD≤9.4%. Conclusion：The twenty peanuts and their derivative products samples from different batches and different areas are analyzed by the established method. The results indicated that the established method is sensitive enough to meet the European regulations concerning aflatoxins, it can be applied as a rapid and reliable method for the authentication and quality evaluation of the aflatoxins in the peanuts and their derivative products. At the same time, aflatoxin M1 and M2 are detected in the peanuts and their derivative products for the first time.

关 键 词：超高压液相-质谱联用 黄曲霉毒素 多反应离子监测 

分 类 号：O657.63[理学—分析化学]