超高效液相色谱三重四极杆质谱法测定火锅油、潲水油及地沟油中胆固醇含量

Ultra performance liquid chromatography with electrospray tandem mass spectrometry in the determination of cholesterol in hotpot oil,hogwash oil and waste oil

目的建立测定火锅油、潲水油及地沟油中胆固醇含量的超高效液相色谱-串联三重四极杆质谱(UPLC-MS/MS)方法。方法火锅油、潲水油及地沟油经皂化后用石油醚+乙醚(1+1)提取后,以2,2,3,4,4,6-d6胆固醇为内标,Waters ACQUITY UPLCBEH C18(2.1 mm×50 mm,1.7μm)色谱柱为分析柱,含0.1%甲酸的甲醇溶液为流动相,采用UPLC-MS/MS法,大气压化学电离源(APCI)正离子模式,多反应监测方式测定胆固醇浓度。胆固醇和内标检测离子对m/z分别为369.2→146.9、369.2→160.9和375.2→166.5。结果胆固醇在0.05～10μg/ml范围内线性关系良好(r=0.999),最小检出量为0.1 ng,方法回收率为105.2%。结论本方法具有良好的灵敏度、准确度及专属性,可通过检测油脂中的胆固醇含量,鉴别火锅油、潲水油或地沟油。

Objective To establish an ultraperformance liquid chromatography with electrospray tandem mass spectrometry（UPLC-MS/MS） method for the determination of cholesterol in hotpot oil,hogwash oil and waste oil.Methods Oil samples were separated on a Waters ACQUITY UPLC BEH C18 column（2.1 mm × 50 mm,1.7 μm） with a mobile phase of methanol ＋ formic acid（999＋1）.Cholesterol and internal standard（2,2,3,4,4,6-d6 cholesterol） were detected by multi-reactions monitoring（MRM） technology on the transitions of precursor to products（m/z：369.2→369.2,369.2→160.9 and 375.2→166.5）.Ion mode： APCI＋.Results The calibration curve was linear in the range of 0.05-10 μg/ml（r=0.999）,the minimum detectable amount in sample was 0.1 ng,the recovery was 105.2%.Conclusion The method is sensitive,accurate and suitable for the determination of cholesterol in hotpot oil,hogwash oil and waste oil.