کد مقاله کد نشریه سال انتشار مقاله انگلیسی نسخه تمام متن
1217444 1494193 2006 8 صفحه PDF دانلود رایگان
عنوان انگلیسی مقاله ISI
Selective and sensitive determination of amisulpride in human plasma by liquid chromatography–tandem mass spectrometry with positive electrospray ionisation and multiple reaction monitoring
موضوعات مرتبط
مهندسی و علوم پایه شیمی شیمی آنالیزی یا شیمی تجزیه
پیش نمایش صفحه اول مقاله
Selective and sensitive determination of amisulpride in human plasma by liquid chromatography–tandem mass spectrometry with positive electrospray ionisation and multiple reaction monitoring
چکیده انگلیسی

The development of a validated liquid chromatography–tandem mass spectrometry (LC-MS/MS) method with positive electrospray ionisation (ESI(+)) and multiple reaction monitoring (MRM) for the selective and sensitive bioanalytical determination of amisulpride, a substituted benzamide derivative, in human plasma is described. Plasma was cleaned up using a liquid–liquid extraction (diisopropylether:dichloromethane = 1:1 (v/v)) procedure. The chemically related drug sulpiride was used as internal standard (ISTD) and a primary calibration function was established in the concentration range of 0.50–500.52 ng/ml for amisulpride in plasma by triple analysis of the corresponding calibration standards. A linear relationship between concentration and signal intensity (given as peak area ratio analyte/ISTD) was obtained (linear regression: r = 0.9999). A lower limit of quantification (LLQ) of 0.50 ng/ml was used during measurement of study plasma samples. Satisfying results of within-day precision (CV = 0.79 to 1.98%) and accuracy (mean relative deviation: −1.68 to 3.58%) and between-day precision (CV = 1.34 to 4.62%) and accuracy (mean relative deviation: −1.73 to −3.77%) as well as of recovery (amisulpride: 81.74 to 84.83%; sulpiride: 58.65%) and selectivity investigations confirmed the high reliability of this established LC-MS/MS method. Sufficient stability of amisulpride in plasma was achieved during freeze–thaw-cycles, for storage periods of 24 h at room temperature and 20 days at <−20 °C as well as in extracts (storage conditions: <−20 °C, 6 days and 7 °C, 6 days) with mean relative deviations between − 2.83 and 2.91%. An example of a pharmacokinetic profile determined after administration of an amisulpride 200 mg dose in a pilot study is given in this paper. A peak plasma concentration (Cmax) of 522.58 ng/ml was achieved after 3.55 h (tmax). Corresponding values of areas under the plasma concentration–time curve (AUC) of 3405.35 ng h/ml (AUC0−∞) and 3306.54 ng h/ml (AUC0−tlast) were obtained. The terminal plasma elimination half-life (t1/2) was 10.36 h.

ناشر
Database: Elsevier - ScienceDirect (ساینس دایرکت)
Journal: Journal of Chromatography B - Volume 831, Issues 1–2, 2 February 2006, Pages 132–139
نویسندگان
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