HPLC/MS/MS同时测定血浆肾上腺素、去甲肾上腺素、可的松和氢化可的松的方法建立  

Simultaneous Determination of Adrenaline,Noradrenaline,Cortisone and Cortisol in Plasma with HPLC/MS/MS

作　　者：雍莉[1] 王宇[2] 邹晓莉[2] 朱岚[1] 谢蟪旭[3] 李龙江[3] 

机构地区：[1]四川省疾病预防控制中心,成都610041 [2]四川大学华西公共卫生学院卫生检验学教研室,成都610041 [3]四川大学口腔疾病研究国家重点实验室,成都610041

出　　处：《四川大学学报（医学版）》2014年第1期142-146,共5页Journal of Sichuan University(Medical Sciences)

基　　金：国家自然科学基金项目(No.81172578)资助

摘　　要：目的建立高效液相色谱-质谱-质谱联用（HPLC／MS／MS）同时测定血浆中的肾上腺素、去甲。肾上腺素、可的松和氢化可的松的方法。方法样品经乙腈沉淀蛋白和萃取后，15000r／min离心5min，取上清液进样分析。电喷雾离子源（ESI），正离子检测，多反应监测（MRM）方式定量分析。结果肾上腺素、去甲肾上腺素、可的松和氢化可的松在0．02～200．00ng／mL浓度范围内线性良好（相关系数均≥0．999），检出限分别为4．13pg／mL、4．64pg／mL、4．29pg／mL和4．52pg／mL，日内和日间精密度分别为1．19％～5．42％和2．16％～6．04％；将所建立的方法用于空白人血浆样品分析，加标回收率为80．0％～109．0％，样品测定精密度为3．93％～7．57％。结论本研究所建立的方法快速灵敏，适合血浆样品的批量分析。Objective To develop a method for simultaneous determination of adrenaline, noradrenaline, cortisone and eortisol in plasma using HPLC/MS/MS. Methods Sample proteins were precipitated with acetonitrile and the sample solution was inieeted into HPLC/MS/MS after centrifugation at 15 000 r/min for 5 min. Electrospray ionization （ESI） and the positive ion detection were applied with a multiple reaction monitoring （MRM） mode for quantitative analyses. Results Under the optimal conditions, good linearity （r〉0. 999） was observed in the range of 0. 02-200. 00 ng/mL of target compounds. The detection limit reached 4.13 pg/mL, 4.64 pg/mL, 4.29 pg/mL and 4.52 pg/mL for adrenaline, noradrenaline, cortisone and cortisol respectively. The inter-day and intra-day precisions ranged from 1.19%-5.42% and 2.16%-6.04% respectively. Satisfied results were achieved using human plasma samples, with a spiked recovery in the range of 80.0%-109.0% and a relative standard deviation of 3.93%-7.57N. Conclusion The proposed method is quick, sensitive and suitable for batch analyses of plasma samples.

关 键 词：HPLC MS MS 肾上腺素 去甲肾上腺素 可的松 氢化可的松 血浆 

分 类 号：R446.11[医药卫生—诊断学] O657.63[医药卫生—临床医学]