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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 determination of 3-MCPDE in vegetable oil by gas chromatography-negative chemical ionization-mass spectrometry (GC-NCI-MS). Methods The vegetable oil samples were purified by sodium methylate-methanolysis and diatomite solid-phase extraction cartridges. After derivatization with heptafluorobutyryl imidazole, the content of 3-MCPDE in vegetable oil was determined by GC-NCI-MS in ionic monitoring mode. Analysis, determination of the results are free 3-MCPD, internal standard method. Results The linearity was good (r = 0.9999) and the limit of quantification was 0.01 mg / kg. The average recoveries of 3-MCPD at the three spiked levels of 0.10, 0.50 and 1.0 mg / kg were 79.5% ~ 81.7%, the relative standard deviation was 6.0% ~ 9.2%. Conclusion The method has good accuracy and precision, high sensitivity and can be used for the determination of 3-MCPDE in edible vegetable oil.