MEASUREMENT OF PLASMA TESTOSTERONE BY GAS-CHROMATOGRAPHY NEGATIVE-ION MASS-SPECTROMETRY USING PENTAFLUOROPROPIONIC DERIVATIVES
MEASUREMENT OF PLASMA TESTOSTERONE BY GAS-CHROMATOGRAPHY NEGATIVE-ION MASS-SPECTROMETRY USING PENTAFLUOROPROPIONIC DERIVATIVES
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DOI：
10.1016/0378-4347(94)00461-d
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发表时间：
1995-01-20
期刊：
影响因子：
--
通讯作者：
NABET, P
中科院分区：
文献类型：
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作者：
LEGRAND, C;DOUSSET, B;NABET, P
采用气相色谱-负离子化学电离质谱法（GC-MS）测定血浆睾酮。采用自制Extremut柱和乙醚洗脱法从血浆中提取睾酮。通过m/z 560（睾酮）和563（d（3）-睾酮）的选择离子监测，将其定量为五氟丙酸酯（PFP）衍生物，约占总离子的34%。该方法的特点是：萃取回收率为95%，线性范围为1.7- 71.5nmol·l ~（-1），线性回归方程为y = 1.41x + 0.0217，r = 0.999，进样检测限为3.5fmol，信噪比为7.4，日内变异系数GC-MS为3%，全过程变异系数为5.8%。日间变异系数为6.6- 11%，取决于浓度。GC-MS测定结果与RIA测定结果具有良好的相关性（r = 0.994），但GC-MS测定值显著低于RIA测定值（p < 0.05）。
Plasma testosterone was measured by gas chromatography-negative-ion chemical ionisation mass spectrometry (GC-MS). The testosterone was extracted from plasma using home-made Extrelut columns and diethyl ether elution. It was quantified as the pentafluoropropionate (PFP) derivative by selected-ion monitoring at m/z 560 (testosterone) and 563 (d(3)-testosterone), accounting for about 34% of the total ion. The characteristics of the method were: extraction recovery about 95%; linearity over the range 1.7-71.5 nmol l(-1) with linear regression equation y = 1.41x + 0.0217, r = 0.999; detection limit 3.5 fmol injected with a signal-to-noise ratio of 7.4; within-day variation, 3% for GC-MS, and 5.8% for the whole process; day-to-day coefficient of variation, 6.6-11%, depending on the concentrations. There was a good correlation between the results obtained by GC-MS and RIA (r = 0.994), but the GC-MS values were significantly lower (p < 0.05) than those obtained by RIA.