Determination of ticlopidine in human plasma by capillary gas chromatography with ion trap detection

Abstract

A gas chromatographic method for determination of ticlopidine in human plasma using mass spectrometric detection was developed. A Perkin Elmer model 8500 gas chromatograph coupled to an ion trap detector (ITD) in electron impact mode (EI) was used. The gas chromatograph was fitted with a 30 m )/0.32 mm i.d., DB-17 capillary column with a film thickness of 0.25 mm. The compounds were isolated from plasma by Extrelut-1 solid-phase extraction using hexane as the solvent of elution. The detection and quantification limits for this method were 0.005 and 0.01 mg/ml, respectively. The calibration curves were linear from 0.01 and 2.5 mg/ml. Recoveries from human plasma spiked at 0.01 and 2.0 mg/ml ranged from 84.4 and 87.3%. The coefficient of variation (CV) was between 5.1 and 6.9%. The results show that the sensitivity, accuracy and precision of the method are adequate for the determination of ticlopidine in human plasma samples. The ITD in SIM mode allows the unequivocal identification of ticlopidine. The suitability of this method was evaluated in the determination of ticlopidine in plasma from healthy volunteers following oral administration of a dose of 500 mg/day. #

A review of current trends and advances in modern bio-analytical methods: Chromatography and sample preparation

“…Extrelut liquid-liquid extraction was commonly used in bioanalytical laboratories as sample preparation, e.g., in the analysis of acetylgestagens in plasma, followed by SPE and by HPLC-MS analysis (elution by 13 mL of ethyl acetate) [131]; in the analysis of ticlopidine in plasma, followed by capillary GC-MS (elution by 6.5 mL of hexane) [132]; in the analysis of synthetic corticosteroids in urine samples, followed by HPLC-MS (elution by 12 mL of toluene/diethyl ether) [133]; in the analysis of rifabutin in plasma, followed by HPLC-PDA (elution 2× by 3 mL of hexane/ethyl acetate) [134] or in the analysis of lornoxicam and its metabolite in plasma and synovial fluid, followed by HPLC-PDA (elution 2× by 5 mL dichloromethane) [135].…”

Understanding cloacal anomalies

“…This surgical manoeuvre has reduced operative time and simplified the procedure. In this modification, the rectum is separated from the vagina via the posterior sagittal approach and then the entire urogenital sinus is dissected and mobilised en bloc 21. In some cases a combined abdominal and posterior sagittal approach with a total urogenital approach may be necessary.…”

Determination of Ticlopidine in Pharmaceutical Tablets by Flow Injection Analysis Using UV-Detection

“…[9,10] A limited number of analytical techniques have been used for the determination of TP in drugs and biological samples. TP concentrations were determined by liquid chromatography [11][12][13][14][15][16][17][18] and gas chromatography [19][20][21] coupled with different types of detectors in these studies. The proposed method in the European Pharmacopoeia [22] is also a gas chromatographic method with flame-ionization detection.…”