气相色谱-负化学离子源-质谱测定食用植物油中 3-氯丙醇酯的含量

Determination of 3-chloro-1,2-propylene glycol ester in edible vegetable oils by gas chromatography-negative chemical ionization-mass spectrometry

中文关键词:  气相色谱-质谱法  负化学离子源  食用植物油  3-氯丙醇酯

英文关键词:gas chromatography-mass spectrometry  negative chemical ionization  edible vegetable oils  3-chloro-1,2-propylene glycol ester

中文摘要:

      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0.5~50 μg/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。

英文摘要:

      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 in vegetable oils.