Stereospecific determination of amisulpride,a new benzamide derivative,in human plasma and urine by automated solid-phase extraction and liquid chromatography on a chiral column application to pharmacokinetics |
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| Affiliation: | 1. School of Mechano-Electronic Engineering, Xidian University, Xi''an 710071, China;2. School of Economics and Management, Xidian University, Xi''an 710071, China;3. Center for Polymer Studies and Department of Physics, Boston University, Boston, MA 02215, USA;1. Department of Chemistry, School of Chemical Sciences, Central University of Karnataka, Kalaburagi, 585367, Karnataka, India;2. IAS-INSA-NASI Summer Research Fellow, Department of Chemistry, School of Chemical Sciences, Central University of Karnataka, Kalaburagi, 585367, Karnataka, India;1. Key Laboratory of Tropical & Subtropical Fishery Resource Application & Cultivation, Ministry of Agriculture, Pearl River Fisheries Research Institute, Chinese Academy of Fishery Sciences, Guangzhou, 510380, China;2. College of Animal Science and Technology, Henan University of Science and Technology, Luoyang, 471003, China;1. University of Marmara, Faculty of Science and Letters, Department of Biology, 34722 İstanbul, Turkey;2. University of Sinop, Faculty of Arts and Sciences, Department of Biology, 57000 Sinop, Turkey;3. International Center for Agricultural Research in the Dry Areas (ICARDA), Giza, Egypt;4. University of Jordan, Faculty of Agriculture, Department of Horticulture and Crop Science, 11942 Amman, Jordan;5. International Center for Agricultural Research in the Dry Areas (ICARDA), Av. Mohamed Belarbi Alaoui, PO Box 6299, Al Irfane, Rabat, Morocco;1. Department of Neonatology, First People''s Hospital of Jining, Jining, Shandong 272011, PR China;2. Department of Neonatology, Maternal and Child Health Hospital of Sishui, Jining, Shandong 273200, PR China;3. Department of Obstetrics, First People’s Hospital of Jining, Jining, Shandong 272011, PR China;4. Department of Internal Medicine, Traditional Chinese Medicine Hospital of Yanzhou, Jining, Shandong 272000, PR China |
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| Abstract: | Amisulpride, a drug belonging to the benzamide series, demonstrates antischizophrenic and antidepressant (antidysthymic) properties in man. For the pharmacokinetic studies of the racemic drug in man, a method of determination based on solid-phase extraction (SPE) from plasma and HPLC on a stereoselective column was developed. For this aim, one millilitre of plasma, after the addition of the internal standard, tiapride or metoclopramide, is diluted with a borate buffer at pH 9, then automatically loaded onto a SPE C18 100-mg column. The column is washed with different solvents, then eluted with 0.5 ml of methanol. After evaporation of the eluted fraction, the residue is reconstituted in 0.25 ml of eluent mixture. An aliquot is injected onto the HPLC column, a Chiralpak AS, equilibrated with an eluent mixture constituted by n-hexane-ethanol, (67:33, v/v) containing 0.2% (v/v) of diethylamine (DEA) or n-heptane-ethanol, (70:29.8, v/v) containing 0.2% of DEA and connected to a UV detector set at 280 nm or to a fluorimetric detector set at λex = 280 nm and λem = 370 nm. The limit of quantitation (LOQ) in human plasma is 2.5 ng ml−1 for both S-(−)- and R-(+)-amisulpride isomers with both detection methods. The method has been demonstrated to be linear in the range 2.5–320 ng ml−1 for both R-(+)- and S-(−)-amisulpride in human plasma with both UV and luorescence detection. Absolute recovery of S(−)- and R-(+)-amisulpride enantimers from human plasma, as well as selectivity, precision and accuracy have been demonstrated to be satisfactory for pharmacokinetics in man and equivalent for both the proposed methods that have been cross-validated on real dosed human plasma samples. The methods have been used for clinical pharmacokinetic studies allowing pharmacokinetic parameters for amisulpride enantiomers in agreement with those obtained for the racemate to be obtained. After dilution with water, urinary samples from subjects treated with amisulpride racemate can be analysed according to the method used for plasma. |
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