Rapid, Solid Phase Extraction Technique for the High-Throughput Assay of Darifenacin in Human Plasma

Abstract

A novel method has been developed for the rapid solid phase extraction of drugs and metabolites from biological fluids, prior to further analysis. The newly designed, 96-tube micropreparation block facilitates high throughput by enabling the extraction of 96 samples simultaneously. The system is described, linked to HPLC/APCI-MS/MS, for the determination of darifenacin in human plasma. The resulting procedure, using deuterated darifenacin as internal standard, is validated over the concentration range 25-2000 pg/mliter; accuracy (0.6-4.6%) and precision (3.6-18.8%) are considered acceptable and overall recovery was determined to be approximately 50%.

Method Development and Validation of Darifenacin in Rat Plasma by Liquid Chromatography-Tandem Mass Spectrometry: Application to a Pharmacokinetic Study

“…Literature survey reveals that there are few methods reported for quantitation and identification of darifenacin in pharmaceutical formulations [6][7][8][9][10][11][12][13][14][15] and biological matrices [16][17][18][19][20]. These methods are developed with different analytical instruments like UV [7,8], spectroflurimetric [9], HPTLC [10], HPLC [11][12][13][14], LC-MS [15,19,20], and positron emission tomography [16].…”

“…These methods are developed with different analytical instruments like UV [7,8], spectroflurimetric [9], HPTLC [10], HPLC [11][12][13][14], LC-MS [15,19,20], and positron emission tomography [16]. Among all the reported methods quantification in rats [16], mice [18], and human plasma [19,20] methods are helpful for clinical pharmacokinetics. The reported methods [16,[18][19][20] do not show the accurate and rugged method.…”

“…Among all the reported methods quantification in rats [16], mice [18], and human plasma [19,20] methods are helpful for clinical pharmacokinetics. The reported methods [16,[18][19][20] do not show the accurate and rugged method. It is required to develop and validate the most economical, simple, rugged, and reproducible bioanalytical method for quantification of darifenacin in biological matrices for its clinical pharmacokinetics.…”

Fully automated determination of eserineN-oxide in human plasma using on-line solid-phase extraction with liquid chromatography coupled with electrospray ionization tandem mass spectrometry

“…Since the late 1980s, the introduction of atmospheric pressure ionization (API) sources coupled with mass spectrometers has broadened the use of mass spectrometry (MS) in drug analysis. 10,11 They have been used to develop very specific and sensitive assays of drugs in biological samples using triple-quadrupole 12,13 or quadrupole ion traps 14 as the analyzer, and are now the method of choice as the bioanalytical tool for pharmacokinetic and metabolism studies. The use of miniaturized HPLC (i.e.…”

Automated sample preparation using membrane microtiter extraction for bioanalytical mass spectrometry

“…This development was first described and utilized for sample preparation by B. Kaye et al 8 and has since been adopted by other laboratories. 9 Although the throughput of sample extraction using these packed particle beds has at least been doubled by their incorporation into the microtiter plate format, the technology retains the same disadvantages of single packed bed cartridges, specifically, large volumes of solvent needed for processing and elution, and an additional evaporation step is usually required.…”