کد مقاله کد نشریه سال انتشار مقاله انگلیسی نسخه تمام متن
1222274 967859 2010 6 صفحه PDF دانلود رایگان
عنوان انگلیسی مقاله ISI
Determination of nutlin-3a in murine plasma by liquid chromatography electrospray ionization tandem mass spectrometry (LC–ESI-MS/MS)
موضوعات مرتبط
مهندسی و علوم پایه شیمی شیمی آنالیزی یا شیمی تجزیه
پیش نمایش صفحه اول مقاله
Determination of nutlin-3a in murine plasma by liquid chromatography electrospray ionization tandem mass spectrometry (LC–ESI-MS/MS)
چکیده انگلیسی

A sensitive and precise LC–ESI-MS/MS method for determination of nutlin-3a in murine plasma using ketoconazole as an internal standard was developed and validated. Plasma nutlin-3a samples were prepared by either a simple protein precipitation (PP) for the high concentration range (10–20,000 ng/mL) or by liquid–liquid extraction (LLE) for the low concentration range (0.25–300 ng/mL). Nutlin-3a and ketoconazole were separated on a modified C18 analytical column (4 μm, 75 mm × 2 mm) with an isocratic mobile phase (acetonitrile/5 mM HCOONH4 = 70/30, v/v). The retention times of nutlin-3a and ketoconazole were 1.14 and 1.45 min. Detection was achieved by a tandem MS system, monitoring m/z 582/99 and m/z 532/82 for nutlin-3a and ketoconazole, respectively. The PP method was linear in a range of 10–20,000 ng/mL (R2 ≥ 0.993) and the LLE method was linear in a range of 0.25–300 ng/mL (R2 ≥ 0.992). The mean recoveries for PP and LLE were 24% and 78%, respectively. Within-day and between-day precisions were ≤4.5% for PP and were ≤4.9% for LLE. Within-day and between-day accuracies (% error) ranged from 4.8 to −7.9 for PP, and from −0.2 to −8.4 for LLE. The two extraction methods produced equivalent results, allowing use of both within the same study. This method has been applied to the measurement of nutlin-3a concentrations in murine plasma samples obtained from a preclinical pharmacokinetic study.

ناشر
Database: Elsevier - ScienceDirect (ساینس دایرکت)
Journal: Journal of Pharmaceutical and Biomedical Analysis - Volume 51, Issue 4, 11 March 2010, Pages 915–920
نویسندگان
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