Abstract

目的 建立同位素稀释液相色谱串联质谱(LC/MS/MS)测定血清总胆固醇的方法.方法 血清样品中加入[3,4-13C2]-胆固醇作内标,用氢氧化钠水解血清胆固醇酯为胆固醇,用三氧化铬-硫酸氧化胆固醇为胆甾-4-烯-3,6-二酮,用LC/MS/MS分析胆固醇氧化产物,采用大气压化学电离源,用多反应监测(MRM)模式和选择离子监测(SIR)模式检测,用修正标准曲线法对血清样品进行定量.结果 两种检测模式的峰面积比与胆固醇浓度的线性相关系数均大于0.999 9.MRM模式测定血清总胆固醇的平均批内变异系数(CV)为0.95%(范围0.92%~0.99%),平均总CV为0.86%(0.82%~0.89%);SIR模式平均批内CV为0.64%(0.54%~0.77%),平均总CV为0.69%(0.62%~0.81%).测定国际或国家标准物质结果与靶值的平均偏差在MRM模式下为0.23%(0.14%~1.00%),SIR模式为0.24%(0.07%~1.27%).结论 成功建立了LC/MS/MS测定血清总胆固醇的方法,方法特异、精密、简便,可望用作血清胆固醇测定的参考方法。

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