Measurement of Estradiol in Human Serum by LC-MS/MS Using a Novel Estrogen-Specific Derivatization Reagent
| Autor: | Reena Desai, Pekka Keski-Rahkonen, Mark Jimenez, D. Tim Harwood, David J. Handelsman |
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| Rok vydání: | 2015 |
| Předmět: |
Chromatography
Estradiol Molecular Structure medicine.drug_class Estrogens Sulfinic Acids Tandem mass spectrometry Serum samples Mass spectrometry Analytical Chemistry Triple quadrupole mass spectrometer chemistry.chemical_compound chemistry Tandem Mass Spectrometry Estrogen Reagent Lc ms ms medicine Humans Indicators and Reagents Derivatization Chromatography High Pressure Liquid |
| Zdroj: | Analytical Chemistry. 87:7180-7186 |
| ISSN: | 1520-6882 0003-2700 |
| DOI: | 10.1021/acs.analchem.5b01042 |
| Popis: | A liquid chromatography-tandem mass spectrometry (LC-MS/MS) method is described that employs a novel derivatization reagent for the measurement of serum estradiol (E2), with simultaneous analysis of underivatized testosterone (T) and dihydrotestosterone (DHT). The main advantage of the new derivatization reagent 1,2-dimethylimidazole-5-sulfonyl chloride is its analyte-specific fragmentation that enables monitoring of confirmatory mass transitions with high sensitivity. The reaction mixture can be analyzed without additional purification steps using a 9.5 min gradient run, and sensitive detection is achieved with a triple quadrupole mass spectrometer using atmospheric pressure photoionization. Method validation was performed with human serum samples, including a comparison with a standard LC-MS/MS method using 120 samples from a clinical study, and analysis of certified E2 serum reference materials BCR-576, BCR-577, and BCR-578. The lower limits of quantification for E2, T, and DHT were 0.5 pg/mL, 25 pg/mL, and 0.10 ng/mL, respectively, from a 200-μL sample. Validation results indicated good accuracy and agreement with established, conventional LC-MS/MS assays, demonstrating suitability for analysis of samples containing E2 in the low pg/mL range, such as serum from men, children, and postmenopausal women. |
| Databáze: | OpenAIRE |
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