Development of a solid phase extraction method for simultaneous determination of corticoids and tranquilizers in serum samples

Abstract

A simple and fast solid phase extraction (SPE) method allowing the preconcentration, clean-up, and subsequent separate elution of phenothiazines (chlorpromazine hydrochloride, acetopromazine, and propionylpromazine hydrochloride) and glucocorticoids (dexamethasone, betamethasone acetate, and phenylbutazone) from serum samples has been developed. Both fractions were separately collected and analyzed without any additional treatment by high performance liquid chromatography with UV-Vis. The performance of the complete procedure was satisfactory irrespective of the spiking level with recoveries in the range 64-85% for all analytes investigated but for phenylbutazone (20%). Repeatability, evaluated as the relative standard deviation, was globally better than 12%. LC-MS was used for final confirmation of the results.

Determination of selected phenothiazines in human plasma by solid-phase extraction and liquid chromatography with coulometric detection

“…Several papers can be found in the literature regarding the determination of some phenothiazines as a single analyte or together with other drugs in biological fluids or tissues [9][10][11][12][13][14][15][16][17][18][19][20][21][22][23][24][25]. Usually, the drugs are analysed by means of highperformance liquid chromatography (HPLC) coupled with UV detection [9,11,24,25], fluorescence detection [13], mass spec-trometry [13] or electrochemical (both amperometric and coulometric) detection [18][19][20][21][22][23]. One paper concerns the use of capillary electrophoresis (CE) for forensic purposes [10].…”

Analytical strategy for the confirmatory analysis of the non-steroidal anti-inflammatory drugs firocoxib, propyphenazone, ramifenazone and piroxicam in bovine plasma by liquid chromatography tandem mass spectrometry

“…The majority of methods that have been cited to date have been developed in equine plasma or serum alone or in combination with other matrices [17][18][19][20]22,[25][26][27][30][31][32] with limits of detection ranging from 0.1 ng ml −1 to 5 g ml −1 . Other methods exist for the determination of NSAIDs in bovine plasma or serum but the limits of detection range from 20 ng to 3.4 g ml −1 [15,21,22,24,29,30] or in rat serum [23]. Only two methods are available in equine plasma to date capable of meeting the requirement to monitor at 5 ng ml −1 in plasma.…”

“…The advantages of using plasma as a target matrix in regulatory control are that it is an easy matrix for analysis, can identify the presence of drugs in live animals prior to slaughter and residues can be found in this matrix for a long time (personal communication with the CRL). Methods have been reported for the analysis of NSAIDs in plasma in the literature by LC-UV [15,16,[18][19][20][21][22][23][24], GC-MS [19,[25][26][27][28], LC-MS [17,23,25,[29][30][31] and capillary electrophoresis [32]. The majority of methods that have been cited to date have been developed in equine plasma or serum alone or in combination with other matrices [17][18][19][20]22,[25][26][27][30][31][32] with limits of detection ranging from 0.1 ng ml −1 to 5 g ml −1 .…”

Separation and pre‐concentration of glucocorticoids in water samples by ionic liquid supported vortex‐assisted synergic microextraction and HPLC determination

“…However, as glucocorticoids are normally present in low concentrations, their direct detection may not be feasible due to the inadequate sensitivity of detection procedures . Hence, pre‐concentration of water samples is performed using a number of methods prior to chemical analysis, such as pressurized liquid extraction, SPE , and solid‐phase microextraction (SPME) . Unfortunately, all of these methods require a large sample volume and are time consuming.…”