液-液萃取-液相色谱-串联质谱法测定“地沟油”中辣椒碱类化合物及丁香酚

Determination of capsaicinoids and eugenol in waste-edible-oil by liquid-liquid extraction and liquid chromatographytandem mass spectrometry

建立了"地沟油"中辣椒碱类化合物(包括辣椒素、二氢辣椒素、合成辣椒素)及丁香酚的液-液萃取及液相色谱-串联质谱(LC-MS/MS)检测方法。"地沟油"中辣椒碱类化合物及丁香酚用甲醇萃取,采用SUPEL COSIL ABZ+Plus dC18色谱柱(150 mm×4.6 mm,5μm)分离,电喷雾离子源在正、负离子模式下电离,多反应监测(MRM)模式扫描。对辣椒素、二氢辣椒素、合成辣椒素及丁香酚的检出限分别为0.02、0.03、0.03和0.6μg/L,且在一定的质量浓度范围内线性良好。同一操作人员与不同操作人员间测定的精密度低于5%。该方法专属性强、灵敏、准确,可以作为"地沟油"的判定标准之一。

A method was developed for the determination of capsaicinoids（capsaicin,dihydrocapsaicin and synthetic capsaicin） and eugenol in waste-edible-oil extracted by liquid-liquid extraction and liquid chromatography-tandem mass spectrometry（LC-MS/MS）.The capsaicinoids and eugenol in waste-edible-oil were extracted by methanol,and then separated by a SUPEL COSIL ABZ＋Plus dC18 column（150 mm×4.6 mm,5μm）.The analysis was performed by MS/MS with electrospray ionization in positive and negative ion modes with multiple reaction monitoring（MRM）.The limits of detection for capsaicin,dihydrocapsaicin,synthetic capsaicin and eugenol were 0.02,0.03,0.03 and 0.6μg/L,respectively.The good linear relationships were obtained in certain concentration ranges of capsaicinoids and eugenol.The relative standard deviations（RSDs,n=5） of same-worker and different-worker were less than 5%.The method is exclusive,sensitive and accurate,and can be used in waste-edible-oil determination.