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目的建立测定蛋黄卵磷脂中胆固醇含量的超高液相色谱-串联四极杆质谱(UPLC-MS/MS)方法。方法蛋黄卵磷脂经三氯甲烷-乙醇(5∶45)溶解后,以2,2,3,4,4,6-d6胆固醇为内标,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,多反应检测方式测定胆固醇的浓度。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0.25～10μg.mL-1范围内的线性关系良好(r=0.999),定量限为0.02 ng,方法回收率为102%。结论所建方法具有良好的灵敏度、准确度及专属性,可用于蛋黄卵磷脂中胆固醇的含量测定。
Objective To establish a method for the determination of cholesterol in egg lecithin by ultra performance liquid chromatography-tandem quadrupole mass spectrometry (UPLC-MS / MS). Methods Egg lecithin was dissolved in chloroform-ethanol (5:45), and the mobile phase consisted of 2,2,3,4,4,6-d6 cholesterol and 0.1% formic acid in methanol. MS / MS method, atmospheric pressure chemical ionization source (APCI) positive ion mode, multi-reaction detection method to determine the concentration of cholesterol. 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 a good linearity (r = 0.999) in the range of 0.25-10μg.mL-1 with a limit of quantification of 0.02 ng and a recovery of 102%. Conclusion The proposed method has good sensitivity, accuracy and specificity and can be used for the determination of cholesterol in egg lecithin.