气相色谱-同位素稀释串联质谱法同时测定17β-雌二醇、17α-雌二醇和雌酮
Simultaneous Measurement of 17β-Estradiol, 17α-Estradiol and Estrone by GC-Isotope Dilution MS/MS.
作者信息
Prokai-Tatrai Katalin, Bonds Darius, Prokai Laszlo
机构信息
Department of Molecular Biology and Immunology, University of North Texas Health Science Center, 3500 Camp Bowie Boulevard, Fort Worth, TX 76107, USA;
出版信息
Chromatographia. 2010 Feb;71(3-4):311-315. doi: 10.1365/s10337-009-1441-0.
A convenient GC-MS/MS-based method was developed for the simultaneous measurement of 17β-estradiol, 17α-estradiol and estrone using liquid-liquid extraction, a single-step derivatization with N-(trimethylsilyl)imidazole and the corresponding deuterated estrogens as internal standards. Separation of these estrogens was achieved on a 50% phenyl polysilphenylene-siloxane bonded phase column. MS/MS response factors for the derivatized analytes and their corresponding internal standards were found to be practically identical. Therefore, analyte concentrations could be determined by multiplying the measured analyte to internal standard ion-current ratio with known molar concentration of the corresponding deuterated internal standards. Assay accuracies, determined from the analyses of quality control samples obtained by spiking known concentrations of analytes into charcoal-stripped human serum, were in the -11% to +14% range. Limits of quantitations were between 13 pg/mL and 21 pg/mL from this biological medium.
开发了一种基于气相色谱-串联质谱（GC-MS/MS）的便捷方法，用于同时测定17β-雌二醇、17α-雌二醇和雌酮，该方法采用液-液萃取、用N-（三甲基硅基）咪唑进行一步衍生化，并以相应的氘代雌激素作为内标。这些雌激素在50%苯基聚硅苯撑硅氧烷键合相柱上实现分离。发现衍生化分析物及其相应内标的串联质谱响应因子几乎相同。因此，通过将测得的分析物与内标离子流比乘以相应氘代内标的已知摩尔浓度，可以确定分析物浓度。通过将已知浓度的分析物加标到经活性炭处理的人血清中获得质量控制样品进行分析，测定的分析准确度在-11%至+14%范围内。该生物介质的定量限在13 pg/mL至21 pg/mL之间。
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