同位素稀释液相色谱串联质谱法测定血清睾酮  

Determination of serum testosterone by isotope dilution liquid chromatography tandem mass spectrometry

作　　者：张天娇[1] 王玉飞[1] 曾洁[1] 张江涛[1] 周伟燕[1] 闫颖[1] 赵海舰[1] 汪静[1] 王冬环[1] 马嵘[1] 胡翠华[1] 张传宝[1] 

机构地区：[1]北京医院国家老年医学中心卫生部临床检验中心,北京100730

出　　处：《临床检验杂志》2016年第12期892-896,共5页Chinese Journal of Clinical Laboratory Science

基　　金：国家自然科学基金(81301488);国家科技基础性工作专项(2013FY113800);北京生物医药产业跨越发展工程项目(G20工程;Z161100001816043)

摘　　要：目的建立一种用同位素稀释液相色谱串联质谱法(ID-LC/MS/MS)测定血清睾酮的候选参考方法。方法以[16,17,17-d3]睾酮为内标,用重量法准确地与血清混合,用乙酸乙酯-正己烷混合溶剂提取,以羟丙基-β-环糊精水溶液对提取液作净化处理,用液相色谱串联质谱分析,质谱选择离子监测模式检测睾酮与内标的特定碎片离子,用包括法定量。结果血清睾酮测定的批内、批间和总变异系数(CV)的均值(范围)为0.84%(0.22%~2.00%)、1.01%(0.48%~2.37%)和1.37%(0.53%~3.09%)。参考物质ERM DA-345a和NIST SRM 971测定结果与认定值的平均偏差范围为-2.0%^+1.8%。结论用ID-LC/MS/MS建立了血清睾酮的测定方法,方法准确、精密、简便,有望作为血清睾酮测定的参考方法。Objective To establish a candidate reference method of isotope dilution liquid chromatography tandem mass spectrometry（ ID-LC/MS/MS） for the determination of human serum testosterone. Methods The [16,17,17-d3] testosterone was selected as the internal standard,and added into serum samples exactly. Then,the testosterone in the serum samples was extracted with mixed solvent of acetic ether and N-hexane,and purified by an aqueous solution of 2-hydroxypropyl-β-cyclodextrin. Last,the testosterone level was analyzed by the liquid chromatography tandem mass spectrometry system under the multiple reaction monitoring（ MRM） mode,and the concentration of serum testosterone was calculated by the theory of bracketing method. Results The within-run,between-run and total coefficients of variation（ mean and range） for the determination of serum testosterone concentration were 0. 84%（ 0. 22%-2. 00%）,1. 01%（ 0. 48%-2. 37%） and 1. 37%（ 0. 53%-3. 09%）,respectively. The average deviation for the certified reference materials ERM DA-345 a and NIST SRM 971 ranged from-2. 0% to ＋ 1. 8%. Conclusion The established ID-LC / MS / MS method for the determination of serum testosterone is simple,precise and accurate,and may be used as a candidate reference method.

关 键 词：睾酮 同位素稀释 质谱法 

分 类 号：O629.23[理学—有机化学]