摘要
目的：建立气相色谱-负化学离子源-质谱法（gas chromatography-negative chemical ionization-mass spectrometry, GC-NCI-MS）测定植物油中3-氯丙醇酯（3-MCPDE）含量的方法。方法植物油样品经甲醇钠-甲醇水解,硅藻土固相萃取小柱净化,七氟丁酰咪唑衍生化后采用 GC-NCI-MS 在离子监测模式下对植物油中3-MCPDE的含量进行测定和分析,测定结果均以游离态的3-MCPD计,内标法定量。结果3-MCPD在0.5~50μg/L质量浓度范围内线性良好（r=0.9999）,定量限为0.01 mg/kg,在0.10、0.50和1.0 mg/kg 3个加标水平下的平均回收率为79.5%~81.7%,相对标准偏差为6.0%~9.2%。结论该方法准确度和精密度良好,灵敏度高,可用于食用植物油中3-MCPDE的含量测定。
Objective To establish a method for the content determination of 3-chloro-1,2-propylene glycol ester （3-MCPDE） in vegetable oils by gas chromatography-negative chemical ionization-mass spectrometry （GC-NCI-MS）. Methods The vegetable oils samples were hydrolyzed by sodium methoxide-methanol, purified by solid phase extraction （SPE） using diatomaceous earth as the sorbent, and derivatized with heptafluorobutyrylimidazole （HFBI）. The content of 3-MCPDE in vegetable oils was determined and analyzed by GC-NCI-MS in selected ion monitoring （SIM） mode. The results were calculated with internal standard method according to the content of free state 3-MCPD. Results There was a good linearity when the mass concentration of 3-MCPD ranged from 0.5 μg/L to 50 μg/L （r=0.9999） and the limit of quantitation （LOQ） of method was 0.01 mg/kg. The average recoveries of 3-MCPD were 79.5%~81.7%at 3 spiked levels of 0.10, 0.50 and 1.0 mg/kg, with RSDs between 6.0%and 9.2%. Conclusion The established method is accurate, precise and sensitive, which can be used for the content determination of 3-MCPDE＆nbsp;in vegetable oils.
作者
沈伟健
魏雪缘
蔡理胜
张睿
吴斌
沈崇钰
赵增运
柳菡
SHEN Wei-Jian WEI Xue-Yuan CAI Li-Sheng ZHANG Rui WU Bin SHEN Chong-Yu ZHAO Zeng-Yun LIU Han(Animal, Plant and Food Inspection Center, Jiangsu Entry-Exit Inspection and Quarantine Bureau, Nanjing 210001, China)
出处
《食品安全质量检测学报》
CAS
2016年第11期4484-4489,共6页
Journal of Food Safety and Quality
基金
国家质检总局科技计划项目(2015IK141)
江苏省"333工程"项目(BRA2014330)
上海长三角科技合作项目(15395810100)~~
关键词
气相色谱-质谱法
负化学离子源
食用植物油
3-氯丙醇酯
gas chromatography-mass spectrometry
negative chemical ionization
edible vegetable oils
3-chloro-1,2-propylene glycol ester
