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目的:建立测定植物油料(油菜籽、花生、黄豆、玉米、芝麻)中胆固醇含量的超高液相-串联四极杆质谱(UPLC-MS/MS)方法。方法:样品经皂化后用石油醚-乙醚(1∶1)提取,以2,2,3,4,4,6-d6胆固醇为内标,Waters ACQUITYUPLCBEH 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,大气压化学电离源(APCI)正离子模式,多反应检测方式测定。胆固醇和内标离子检测对m/z分别为369.2→146.9,369.2→160.9和375.2→166.5。结果:胆固醇在0.05μg.ml-1～10μg.ml-1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106%。结论:本方法具有良好的灵敏度、准确度及专属性,可用于植物油料中胆固醇含量测定。
Objective: To establish a high performance liquid chromatography-tandem quadrupole mass spectrometry (UPLC-MS / MS) method for the determination of cholesterol in plant oilseeds (rapeseed, peanut, soybean, corn and sesame). Methods: The samples were saponified and extracted with petroleum ether-diethyl ether (1: 1). The internal standard was 2,2,3,4,4,6-d6 cholesterol. Waters ACQUITY UPLCBEH C18 (2.1 mm × 50 mm, 1.7 μm) column as analytical column, methanol solution containing 0.1% formic acid as mobile phase, atmospheric pressure chemical ionization source (APCI) as positive ion mode and multi-reaction detection method. Cholesterol and internal standard ion detection pairs m / z 369.2 → 146.9, 369.2 → 160.9 and 375.2 → 166.5, respectively. Results: Cholesterol had good linearity (r = 0.999) in the range of 0.05μg.ml-1 ~ 10μg.ml-1 with the detection limit of 0.1 ng. The recovery rate was 106%. Conclusion: The method has good sensitivity, accuracy and specificity, can be used for determination of cholesterol content in vegetable oils.