摘要
目的建立月饼中8种真菌毒素的液相色谱-串联质谱确证方法。方法样品用pH=7.4的磷酸盐缓冲液(PBS)和甲醇提取后,过IAC-ADOZ 204免疫亲和柱净化,氮气吹干后用乙腈、甲醇与水溶液(15∶15∶70,V/V)定容,液相色谱-串联质谱法测定,电喷雾正、负离子(ESI+、ESI-)多反应模式监测。结果各种真菌毒素的质量浓度为0.06 ng/ml^15.0 ng/ml时,线性关系良好,相关系数(r)均>0.999,检出限为0.2μg/kg^2.0μg/kg,定量限为0.3μg/kg^5.0μg/kg。3种加标水平下的平均回收率为75.8%~98.4%,相对标准偏差(RSD)为2.4%~9.7%。结论该方法检测准确、可靠,定量限可适用于月饼中8种真菌毒素的同时测定。
Objective To establish a method for the determination and verification of 8 mycotoxins in mooncake by liquid chromatography-tendem mass spectrometry（ LC-MS / MS）. Methods Samples were sequentially extracted with PBS solution（ p H = 7. 4） and methanol,and then the extracts were cleaned-up with IAC-ADOZ 204 immunoaffinity column,and dried-up under nitrogen gas stream. The residue was quantified with acetonitrile / methanol / water mixture before the determination by LC-MS / MS. The monitoring was conducted in the negative（ ESI＋） and positive（ ESI-） electrospray ionization mode.Results When the concentration of the 8 mycotoxins was within 0. 06 ng / ml-15. 0 ng / ml,good linearity was obtained,with the correlation cofficient（ r） greater than 0. 999,the limits of detection（ LOD） within 0. 2 μg / kg-2. 0 μg / kg,and the limit of quantitation（ LOQ） within 0. 3 μg / kg-5. 0 μg / kg. The average recovery rates were within 75. 8%-98. 4%,and the relative standard deviation（ RSD） among 2. 4%-9. 7%. Conclusion This analytical method is simple,rapid,accurate,and it can be applied for the simultaneous determination of 8 mycotoxins in mooncake.
出处
《中国卫生检验杂志》
CAS
2016年第11期1524-1528,共5页
Chinese Journal of Health Laboratory Technology
基金
广东省省级科技计划项目(2014A040401011)
国家质检总局科技项目(2015IK260)
中山市社会公益重大专项(2015B2295)
关键词
免疫亲和柱
液相色谱-串联质谱法
真菌毒素
月饼
Immunoaffinity column
Liquid chromatography-tendem mass spectrometry
Mycotoxins
Mooncake
