同位素稀释液相色谱串联质谱法测定血清总甘油  

Determination of serum total glycerol by isotope dilution liquid chromatography tandem mass spectrometry

作　　者：周伟燕[1] 刘蕾[2] 张传宝[4] 孙春华[2] 胡欣[2] 李红霞[3] 董军[3] 王抒[3] 申子瑜[4] 陈文祥[4] 

机构地区：[1]中国医学科学院中国协和医科大学,北京100730 [2]卫生部北京医院药学部 [3]卫生部北京医院老年医学研究所 [4]卫生部临床检验中心

出　　处：《中华检验医学杂志》2008年第3期254-257,共4页Chinese Journal of Laboratory Medicine

基　　金：国家科技支撑计划资助项目（2007BA105B09）;国家高技术研究发展计划（863计划）资助项目（2006AA020909）

摘　　要：目的建立同位素稀释液相色谱串联质谱测定血清总甘油的方法。方法以[^13C3]-甘油作内标，用氢氧化钾异丙醇溶液水解血清甘油酯为游离甘油，将游离甘油转化为苯甲酸酯，用同位素稀释液相色谱串联质谱（LC／MS／MS）分离检测，用标准曲线法定量。结果甘油／内标峰面积比与甘油浓度（0．565～4．517mmol／L）线性相关系数大于0．9999；测定不同浓度血清总甘油批内变异系数（CV）平均为0．52％（范围0．21％～2．62％），总CV平均为1．15％（范围0．62％～2．00％）；分析国际和国家标准物质，测定值与认证值的偏倚小于1％（-0．20％～1．06％）。结论建立同位素稀释液相色谱串联质谱测定血清总甘油方法，方法特异、精密、准确，可望用作血清总甘油测定参考方法。Objective To develop a method for measuring serum total glycerol by isotope dilution （ID） liquid chromatography tandem mass spectrometry （LC/MS/MS）. Methods Serum samples were mixed with [ ^13C3 ]-glycerol （internal standard） and treated with alcoholic potassium hydroxide to hydrolyze serum glycerides to glycerol. The natural glycerol and the internal standard were benzoylated with the Sehotten-Baumann reaction and the benzoates were analyzed by LC/MS/MS. Results The correlation coefficients between the peak area ratios and glycerol concentrations were 0. 999 9 and higher. The withinrun coefficients of variation （CV） for serum total glycerol analysis averaged 0. 94% （ ranged 0. 21% - 2. 62% ） and the total CV 1.15% （0. 62% - 2. 00% ）. Results on certified reference materials （ SRM 909b Level Ⅰ and Level Ⅱ ; GBW 09146 and GBW 09147） showed an averaged bias of 0. 20% （ - 0. 20% - 1.06% ）. Conclusions An ID-LC/MS/MS method for serum total glycerol has been developed. The method is highly specific and precise and may be used as a candidate reference method for serum total glycerol measurements.

关 键 词：甘油 甘油三酯 色谱法 液相 光谱分析 质量 同位素标记 碳同位素 

分 类 号：R686[医药卫生—骨科学]