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目的:建立同时测定人唾液中4种溶血磷脂酸(LPA)的方法。方法:采用液-质联用(LC-MS)法,以LPA17:0为内标,唾液样品以盐酸酸化的正丁醇提取后进行测定。色谱柱为Nucleodur100-5C8,流动相为甲醇:2.5mmo·lL-1甲酸铵缓冲液(甲酸调pH3.0)(85:15),流速为0.5mL·min-1,LPA16:0、18:0、18:1、20:4、17:0定量分析的离子反应分别为m/z409.0→153.0、437.0→153.0、435.0→153.0、457.0→153.0、423.0→153.0。结果:LPA各组分在5～2000μg·L-1范围内线性关系良好,平均提取回收率在79.91%～90.01%之间,平均方法回收率在92.16%～106.37%之间,日内和日间RSD均<15%。结论:本方法灵敏度高,操作简便、快速,适用于人唾液中LPAs的浓度测定。
Objective: To establish a method for simultaneous determination of 4 lysophosphatidic acid (LPA) in human saliva. Methods: Liquid-liquid chromatography-mass spectrometry (LC-MS) method with LPA 17: 0 as internal standard, saliva samples were extracted with hydrochloric acid-acidified n-butanol. The column was Nucleodur 100-5C8 and the mobile phase consisted of methanol: 2.5 mmol·L-1 ammonium formate buffer (pH 3.0 for formic acid) (85:15), the flow rate was 0.5 mL · min -1, LPA 16: 0, 18: 0, 18: 1, 20: 4, 17: 0. The ion reactions for quantitative analysis were m / z 409.0 → 153.0, 437.0 → 153.0, 435.0 → 153.0, 457.0 → 153.0, 423.0 → 153.0, respectively. Results: The linear relationship between the components of LPA in the range of 5 ~ 2000μg · L-1 was good. The average recovery was between 79.91% and 90.01%. The average recoveries were between 92.16% and 106.37% RSD <15%. Conclusion: The method is sensitive, simple, rapid and suitable for the determination of LPAs in human saliva.