同位素稀释气相色谱质谱法测定血清孕酮  被引量:7

Determination of serum progesterone by isotope dilution gas chromatography mass spectrometry

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作  者:张天娇[1] 徐锐锋[2] 王卫华[2] 戴新华[2] 张传宝[3] 陈文祥[3] 

机构地区:[1]中国医学科学院 中国协和医科大学,北京100730 [2]中国计量科学研究院化学计量与分析研究所 [3]卫生部北京医院卫生部临床检验中心

出  处:《中华检验医学杂志》2007年第3期255-259,共5页Chinese Journal of Laboratory Medicine

基  金:科学技术部新技术新方法研究专项项目资助(2005JG200200);国家科技基础条件平台专项项目资助(2005DKA1080)

摘  要:目的建立一种血清孕酮测定候选参考方法。方法以[3,4-^(13)C_2]孕酮为内标,用正己烷提取血清,以羟丙基-β-环糊精水溶液对提取液作净化处理,用七氟丁酸酐对孕酮进行衍生化。用气相色谱分离衍生产物,质谱选择离子监测模式检测孕酮与内标的特定碎片离子,用包括法定量。结果血清孕酮测定的总变异系数为0.69%~2.12%,平均分析回收率为98.3%~100.1%。分析血清孕酮标准物质,测定结果与靶值的偏差小于1.5%。结论建立的同位素稀释气相色谱质谱测定血清孕酮的方法,准确、精密,可望作为测定血清孕酮的参考方法。Objective To develop a candidate reference method for the measurement of progesterone in human serum. Methods The serum sample is mixed with the internal standard [ 3, 4-^13 C2 ] progesterone. After extraction with n-hexane and purified by a aqueous solution of 2-Hydroxypropyl-β- cyelodextrin (HP-β-CD), the serum progesterone and labeled progesterone are converted to the 3-enol beptafluorobutyrate and analyzed by gas chromatography mass spectrometry (GC/MS) with selected ion monitoring. The concentration of serum progesterone is calculated by bracketing method. Results The results gave coefficients of variation (CVs) of 0. 69% to 2. 12%. The analytical recoveries ranged from 98. 3% to 100. 1%. The results of measuring certified reference materials of serum progesterone are agree with the target value. Conclusion The procedure for measuring progesterone in serum is a highly accurate and precise method and may be used as a candidate reference method for serum progesterone assays.

关 键 词:孕酮 同位素稀释质谱 羟丙基-Β-环糊精 气相色谱 

分 类 号:R817.4[医药卫生—影像医学与核医学]

 

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