血清胆汁酸LC-MS/MS测定及在老年人血清检测中的应用

目的：建立稳定、有效的血清中所有胆汁酸的液相色谱-串联质谱（LC-MS／MS）测定方法，分析老年人血清胆汁酸谱的特征。方法：建立血清胆汁酸LC-MS／MS定量检测方法，并对方法的灵敏度、精密度、回收率、线性范围等性能指标进行评价；利用该检测方法对10例老年人和15例儿童的空腹血清中所有胆汁酸进行定量检测，分析老年组血清胆汁酸组成特征。结果：该检测体系中，血清中15种胆汁酸和内标在10分钟内完成定量检测，最低检测极限为2～4ng／ml，浓度在3．9～3000ng／ml范围内线性良好，相对回收率为91．95～108．25％，偏移系数为1．71％～10．83％，日内变异度为0．68％～7．05％，日间变异度为2．04％～11．05％；与儿童组相比，老年组血清中胆汁酸总量、疏水性胆汁酸的含量百分较高。结论：所建立的胆汁酸LC-MS／MS检测方法稳定可靠，能满足临床定量检测要求；老年人体内血清胆汁酸谱可能促进胆石症的发生。

Simultaneous Determination of Free and Conjugated Bile Acids in the Serum by LC-MS/MS and the Clinical Use in the Old

Objective:Intended to developed effective and quantitative methods for the analysis of all the free and conjugated bile acids in the serum, and then to determine the characteristic of bile acids in the old. Methods: A sensitive method was founded based on high performance liquid chromatography separation coupled to an electrospray triple-quadrupole mass spectrome-try (LC-MS/MS). Samely the linearity, analytical sensitivity, detection limit, precision and recovery were also evaluated. 10 serum samples of the old and 15 of the child were analyzed by LC-MS/MS. Results: In a single chromatographic run within 10 minutes, bile acids including all free, glycine and taurine-conjugated isomeric forms of bile acids were determined simultaneously. A linear correlation over a wide range of bile acid concentrations (3.9-3000ng/ml) was observed. The recovery period for all of the analyzed bile acids was 91.95%-108.25% ,Intra-day and inter-day precision were 0.68%-7. 05%and 1. 71 %-10. 83%, respectively. The detection limit was about 2-4ng/ml. The mean of total bile acids in child was lower statistically than that in the old. On the contrary, The portion of hydrophobic bile acids such as DCA and CDCA increased notably. Conclusion; The provided method was effective and simple and can be used in clinic research in the future. The profile of the bile acids in the serum of the old may contribute to the development of the cholelithisas.