固相萃取-衍生化-气相色谱-质谱法测定油脂类食品中3-氯-1,2-丙二醇
[Determination of 3-monochloropropane-1,2-diol in grease food by solid phase extraction-derivatization-gas chromatography-mass spectrometry].
作者信息
Xiang Xiaoling, Wang Liyuan, Shen Xianghong, Li Chunsong, Shen Jianfu, Wu Pinggu
机构信息
College of Biosystems Engineering and Food Science,Zhejiang University, Hangzhou 310058,China.
出版信息
Wei Sheng Yan Jiu. 2017 Sep;46(5):777-782.
OBJECTIVE
To establish the method of determination of 3-monochloropropane-1,2-diol( 3-MCPD) in grease food by gas chromatography-mass spectrometry( GC-MS).
METHODS
3-MCPD in grease food represented by bean paste was extracted by ultrasound,purified by alkaline earth solid phase extraction column,derivatived using phenylboronic acid( PBA) and detected by GC-MS.
RESULTS
The linearity of 3-MCPD ranged from 1-100 ng/mL,with correlation coefficient at 0. 9993.The limits of quantitation( LOQ) in soy sauce,bean paste,pepper oil were 0. 6,0. 5 and7. 0 μg/kg and limits of detection( LOD) were 1. 9,1. 6 and 18. 8 μg/kg,respectively.Average recovery rate and relative standard deviation was 78. 3%-106. 7% and 1. 9%-11. 6%( n = 6), when 3-MCPD was added in grease food at 2. 5-1000 μg/kg.
CONCLUSION
The method has good purification effect and the detection sensitivity and accuracy,and can be used for the determination of 3-MCPD in grease food.
目的
建立气相色谱 - 质谱联用法（GC - MS）测定油脂类食品中3 - 氯 - 1,2 - 丙二醇（3 - MCPD）的方法。
方法
以豆瓣酱为代表的油脂类食品中的3 - MCPD经超声提取，用碱土固相萃取柱净化，苯硼酸（PBA）衍生化后用GC - MS检测。
结果
3 - MCPD在1 - 100 ng/mL范围内线性良好，相关系数为0.9993。酱油、豆瓣酱、辣椒油中的定量限（LOQ）分别为0.6、0.5和7.0 μg/kg，检测限（LOD）分别为1.9、1.6和18.8 μg/kg。在油脂类食品中添加2.5 - 1000 μg/kg的3 - MCPD时，平均回收率和相对标准偏差分别为78.3% - 106.7%和1.9% - 11.6%（n = 6）。
结论
该方法净化效果好，检测灵敏度和准确度高，可用于油脂类食品中3 - MCPD的测定。
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