Abstract：
:This paper describes a new liquid chromatography-tandem mass spectrometric (LC-MS/MS) method for the analysis of three stanozolol metabolites (16β-hydroxystanozolol, 3'-hydroxystanozolol, and 4β-hydroxystanozolol) in urines of animal origins. The solid-phase extraction (SPE) clean-up procedure was optimized to reduce the matrix effects in the LC-MS/MS analysis and to enhance recovery. Four different approaches were tested to prepare the sample, which include anion, and cation mixed-mode ion exchange, reversed-phase and normal-phase SPE cartridges. Mixed-mode anion exchange Strata-XL-A SPE column with diethyl ether elution yielded the best values. The separation of metabolites was optimized on Kinetex XB column using isocratic elution. The best mobile phase composition was achieved at the acidic pH with 0.1% (v/v) formic acid in water and methanol composition. The main advantages of the approach applied in the present study over other known methods include the single step SPE clean-up, relatively fast separation on HPLC column packed with core-shell particles, and lowering the limit of detection of target metabolites to the range between 0.05 and 0.15μg/l. Additionally, the developed method was successfully validated for the first time for three species in accordance with the European Union (EU) 2002/657/EC decision. Finally, the efficiency of method was demonstrated by analyzing incurred samples.
journal_name
J Pharm Biomed Analjournal_title
Journal of pharmaceutical and biomedical analysisauthors
Tölgyesi Á,Sharma VK,Fekete Jdoi
10.1016/j.jpba.2013.08.019subject
Has Abstractpub_date
2014-01-01 00:00:00pages
45-52eissn
0731-7085issn
1873-264Xpii
S0731-7085(13)00374-9journal_volume
88pub_type
杂志文章abstract：:The Mahuang-Xingren herb-pair (MX), the combination of Herba Ephedrae (Mahuang in Chinese) and Semen Armeniacae Amarum (Xingren in Chinese), is a classical combination used in traditional Chinese Medicine to treat asthma and bronchitis. A simple and reliable ultra-performance liquid chromatography-tandem mass spectrom...
journal_title：Journal of pharmaceutical and biomedical analysis
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journal_title：Journal of pharmaceutical and biomedical analysis
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abstract：:A novel stability-indicating high-performance liquid chromatographic assay method was developed and validated for docetaxel in the presence of degradation products generated from forced decomposition studies. A gradient HPLC method was developed to separate the drug from the degradation products, using a Hichrom RPB H...
journal_title：Journal of pharmaceutical and biomedical analysis
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doi：10.1016/j.jpba.2006.01.011
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journal_title：Journal of pharmaceutical and biomedical analysis
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journal_title：Journal of pharmaceutical and biomedical analysis
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journal_title：Journal of pharmaceutical and biomedical analysis
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doi：10.1016/j.jpba.2004.01.023
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journal_title：Journal of pharmaceutical and biomedical analysis
pub_type： 杂志文章
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journal_title：Journal of pharmaceutical and biomedical analysis
pub_type： 杂志文章
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journal_title：Journal of pharmaceutical and biomedical analysis
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journal_title：Journal of pharmaceutical and biomedical analysis
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journal_title：Journal of pharmaceutical and biomedical analysis
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doi：10.1016/j.jpba.2008.07.017
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journal_title：Journal of pharmaceutical and biomedical analysis
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pub_type： 杂志文章
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journal_title：Journal of pharmaceutical and biomedical analysis
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journal_title：Journal of pharmaceutical and biomedical analysis
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