超高效液相色谱-串联质谱法测定食用植物油中胆固醇含量

提出了食用植物油中胆固醇的超高效液相色谱-串联质谱测定方法。食用植物油经皂化后用石油醚-乙醚(1+1)溶液提取,以Waters ACQUITY UPLC BEH C18色谱柱(50mm×2.1mm,5μm)为分离柱,以甲酸-甲醇(0.1+99.9)溶液为流动相,以2,2,3,4,4,6-d6胆固醇为内标,采用大气压化学电离源在多反应监测负离子模式下进行测定,胆固醇和内标的定量离子对分别为m/z369.2/146.9,369.2/160.9和375.2/166.5。胆固醇在0.1～5mg·L-1范围内呈线性,测定下限(10S/N)为0.02ng。在3个浓度水平上对方法做回收试验,测得回收率在102%～110%之间。

UHPLC-MS/MS Determination of Cholesterol in Edible Vegetable Oil

A method for the determination of cholesterol in edible vegetable oil by ultra-high-performance liquid chromatography hyphenated with tandem mass spectrometry(HPLC-MS/MS) was proposed.Cholesterol in samples was extracted with a mixture of petroleum ether and ethyl ether(1+1).The eluate was used for UHPLC-MS/MS determination,in which the ACQUITY UPLC BEH C18 column(50 mm×2.1 mm,5 μm) was used as separation column,a mixture of formic acid and methanol(0.1+99.9) was used as mobile phase,and 2,2,3,4,4,6-d6-cholesterol was used as internal standard.Atmospheric pressure chemical electrospray ionization under the mode of multiple reaction monitoring was used in the detection.Ion pairs used for the quantitative analysis were m/z 369.2/146.9,369.2/160.9 for cholesterol and m/z 375.2/166.5 for internal standard.Linearity range was found between 0.1-5 mg·L-1,and lower limit of determination(10S/N) found was 0.02 ng.Recovery was tested at 3 concentration levels,giving results of recovery ranged from 102% to 110%.