Rapid measurement of estrogens and their metabolites in human serum by liquid chromatography-tandem mass spectrometry without derivatization
Rapid measurement of estrogens and their metabolites in human serum by liquid chromatography-tandem mass spectrometry without derivatization
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DOI：
10.1016/j.clinbiochem.2008.02.009
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发表时间：
2008-06-01
影响因子：
2.8
通讯作者：
Soldin, Steven J.
中科院分区：
文献类型：
--
作者：
Guo, Tiedong;Gu, Jianghong;Soldin, Steven J.
目的：雌激素主要有雌二醇（E2）、雌酮（E1）和雌三醇（D）。E1/E2及其代谢产物16-羟基雌酮（16-OHE 1，已知具有致癌性）可能参与包括人类乳腺癌在内的许多癌症的发展。本研究的目的是建立一种快速、简便的高效液相色谱-串联质谱法本发明涉及一种用于同时测量人血清中的E1、E2、E3和16-OHE 1的高效液相色谱-串联质谱（HPLC-MS/MS）测定法，而不需要固相萃取或衍生化。API-5000三重四极杆质谱仪与电喷雾电离（EST）耦合使用Source和Shimadzu HPLC系统，对每种分析物采用氘标记的内标（IS）进行同位素稀释。结果：E1和16-OHE 1的检测限为1.0 pg/mL，E2和E3的检测限为2.0 pg/mL。所有检测分析物的日内CV均< 6.5%，日间CV范围为4.5%至9.5%。结论：该方法可在8 min内同时测定人血清中4种雌激素，具有样品处理简单、样品量少、高通量等优点，可用于临床。(c)2008年加拿大临床化学家协会。爱思唯尔公司出版All rights reserved.
Objectives: The steroids estradiol (E2), estrone (E1), and estriol (D) are the major estrogens. E1/E2 and their metabolite 16-hydroxyestrone (16-OHE1, known to be carcinogenic) could be involved in the development of many cancers including human breast cancer. The aim of the current study was to develop a rapid and simple high performance liquid chromatography-tandem mass spectrometry (HPLC-MS/MS) assay to simultaneously measure El, E2, E3 and 16-OHE1 in human serum without the need for solid phase extraction or derivatization.Methods: An API-5000 triple-quadrupole mass spectrometer coupled with electrospray ionization (EST) source and Shimadzu HPLC system was used employing isotope dilution with deuterium-labeled internal standard (IS) for each analyte. Quantitation by multiple reaction monitoring (MRM) analysis was performed in negative ion mode.Results: The limits of detection were 1.0 pg/mL for El and 16-OHE1 and 2.0 pg/rnL for E2 and E3. Within-day CVs were < 6.5% for all analytes tested and between-day CVs ranged from 4.5% to 9.5%. Recovery ranged from 88% to 108%.Conclusion: This method allows for the simultaneous measurement of four estrogens in human serum within 8 min. It can be routinely employed in a clinical environment and is attractive because of its simplicity in sample processing, micro sample requirement, and high throughput. (c) 2008 The Canadian Society of Clinical Chemists. Published by Elsevier Inc. All rights reserved.