气相色谱与串联质谱联用检测血清中脱氢表雄酮  

Determination of Ddehydroepiandrosterone in Emasculated Rat′s Serum by Gas Chromatography-Tandem Mass Spectrometry

作　　者：陈君[1] 梁琼麟[1] 罗国安[1] 王义明[1] 段雪艳[1] 章弘扬[1] 

机构地区：[1]清华大学分析中心,北京100084

出　　处：《分析化学》2008年第2期172-176,共5页Chinese Journal of Analytical Chemistry

基　　金：国家973项目资助(Nos.2005CB23503;2001CB510305)

摘　　要：在晚期前列腺癌雄激素全阻断治疗最终导致前列腺癌雄激素非依赖性的转变过程中，肾上腺分泌脱氢表雄酮（DHEA）被认为是重要的诱因。本研究主要利用睾丸摘除（去势）大鼠模型，对血清中DHEA浓度进行测定。采用了气相色谱与串联质谱联用（GC-MS／MS）技术，建立了高灵敏度的测定大鼠血清中脱氢表雄酮（DHEA）的方法。样品经过甲醇沉蛋白，而后固相萃取提取血清中微量的DHEA，通过七氟丁酸酐（HFBA）衍生。采用GC-MS／MS测定。对固相萃取条件、衍生化条件以及质谱测定条件进行优化。DHEA在0．1～100μg／L范围内线性良好，相关系数r为0．9996；在2～50μg／L浓度范围内，加标回收率在99％～106％之间；相对标准偏差小于5％。本方法灵敏度高，选择性好，可满足临床对于血清样品中DHEA的测定要求。对去势大鼠血清中DHEA测定结果表明，去势后DHEA明显上升。Dehydroepiandrosterone （DHEA）, which is mostly secreted from adrenal in prostate cancer patients with anti-androgen therapy, is considered as the very inducer who should take responsibility for the androgen-independent transition. DHEA serum concentration in Rat with orchiectomy for different time was detected by a gas chromatography/electron impact ionization tandem mass spectrometric method, which had been developed for the determination of DHEA in serum samples. Methanol was used to deproteinize the serum sample, then DHEA was analyzed by GC-MS/MS after SPE process and derivatization by heptafluorobutyric anhydride （HFBA）. Sample pretreatment and GC-MS/MS analytical condition were optimized. The linear range was 0. 1 - 100 μg/L. The correlation coefficient （r） was 0. 9996. The average recovery of DHEA in serum sample （from 2 μg/L to 50 μg/L） ranged from 99% to 106%, and the relative standard deviation was less than 5 %. The result indicats that the method developed is more sensitive and selective. It also demonstrated that this analysis method could meet the requirement for the clinical determination of DHEA in serum sampies. The result shows that there really exists a raise of DHEA in rat＇s serum after orchiectomy.

关 键 词：脱氢表雄酮 气相色谱-串联质谱 肾上腺源雄性激素 临床分析 

分 类 号：R446.1[医药卫生—诊断学]