摘要
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 UPLCBEH 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.
出处
《中国食品卫生杂志》
北大核心
2011年第5期429-432,共4页
Chinese Journal of Food Hygiene
关键词
胆固醇
火锅油
潲水油
地沟油
超高效液相色谱-串联质谱
鉴别
食品安全
Cholesterol
hotpot oil
hogwash oil
waste oil
ultra performance liquid chromatography with electrospray tandem mass spectrometry
distinguish
food safety