Validated LC–MS-MS Method for Simultaneous Analysis of 17 Barbiturates in Horse Plasma for Doping Control
| Autor: | Xiaoqing Li, Lawrence R. Soma, Cornelius E Uboh, Fuyu Guan, Fengchang Zhu, Youwen You, George A Maylin, Ying Liu |
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| Rok vydání: | 2017 |
| Předmět: |
Methyl Ethers
Analyte Accuracy and precision Health Toxicology and Mutagenesis Electrospray ionization Liquid-Liquid Extraction Analytical chemistry Toxicology Mass spectrometry 01 natural sciences Analytical Chemistry Plasma 03 medical and health sciences 0302 clinical medicine Liquid–liquid extraction Animals Environmental Chemistry Horses 030216 legal & forensic medicine Doping in Sports Detection limit Chemical Health and Safety Chromatography Chemistry 010401 analytical chemistry Extraction (chemistry) Horse 0104 chemical sciences Substance Abuse Detection Barbiturates |
| Zdroj: | Journal of Analytical Toxicology. 41:431-440 |
| ISSN: | 1945-2403 0146-4760 |
| DOI: | 10.1093/jat/bkx025 |
| Popis: | A rapid and sensitive method for simultaneous screening, quantification and confirmation of 17 barbiturates in horse plasma using liquid chromatography-tandem mass spectrometry is described. Analytes were recovered from plasma by liquid-liquid extraction using methyl tert-butyl ether, separated on a C18 column, and analyzed in negative electrospray ionization mode. Multiple-reaction monitoring was employed for screening and quantification. Confirmation for the presence of the analytes was achieved by comparing ion intensity ratio. The ranges for limits of detection, quantification and confirmation were 0.003-1 ng/mL (S/N ≥ 3), 0.01-2.5 ng/mL and 0.02-5 ng/mL, respectively. The linear dynamic range of the method was 0.1-100 ng/mL. The precision and accuracy at 0.5, 5 and 50 ng/mL of all 17 barbiturates during intra-day assay were 1.6-8.6% and 96-106%, respectively. For inter-day assay, precision and accuracy at the same three concentrations were 2.6-8.9% and 96-106%, respectively. Analysis of all 17 analytes was completed within 7 min. Thus, the present method is fast, simple, sensitive and reproducibly reliable. |
| Databáze: | OpenAIRE |
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