Xiang Xiaoling, Wang Liyuan, Shen Xianghong, Li Chunsong, Shen Jianfu, Wu Pinggu
College of Biosystems Engineering and Food Science,Zhejiang University, Hangzhou 310058,China.
Wei Sheng Yan Jiu. 2017 Sep;46(5):777-782.
To establish the method of determination of 3-monochloropropane-1,2-diol( 3-MCPD) in grease food by gas chromatography-mass spectrometry( GC-MS).
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.
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.
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.
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。
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。
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）。
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。
