A simple and reliable stir bar sorptive extraction‐liquid chromatography procedure for the determination of chlorpromazine and trifluoperazine in human serum using experimental design methodology

Abstract

A sensitive and reproducible stir bar sorptive extraction and HPLC-UV detection method was used for the therapeutic drug monitoring of chlorpromazine and trifluoperazine in human serum. The separation was achieved using a C(18) column. The mobile phase consisted of methanol/sodium acetate buffer (pH 4.1; 0.1 M) (95:5, v/v) including 0.5% triethylamine. This miniaturized method can result in faster analysis, lower solvent consumption and less workload per sample while maintaining or even improving sensitivity. In the second part, stir bar sorptive extraction/HPLC-UV method was optimized by a chemometrics approach. An experimental design was therefore used to evaluate the statistically influential and/or interacting factors, among those described in the literature, and to find the best extraction and desorption conditions. Optimal sample volume of 1 mL, extraction time of 24 min at 31°C with pH 8.1 were obtained in a screening 2(5) half fractional factorial design followed by a Box-Behnken design. For the desorption conditions, a Box-Behnken design showed that the best conditions were 150 μL mobile phase for 20 min at 50°C. The optimized method was repeatable (CV<10%, linear (LOQ-500 ng/mL)), with the LOQs equal to 0.7 and 1.5 ng/mL for chlorpromazine and trifluoperazine, respectively.

Preparation of a novel sorptive stir bar based on vinylpyrrolidone‐ethylene glycol dimethacrylate monolithic polymer for the simultaneous extraction of diazepam and nordazepam from human plasma

“…Based on previous studies , many factors including ionic strength, pH, and extraction time and temperature can influence the extraction efficiency of SBSE technique. To optimize the mentioned factors, a three‐level Box–Behnken design was utilized .…”

Parameters optimization of supercritical fluid‐CO2 extracts of frankincense using response surface methodology and its pharmacodynamics effects

“…The experimental design and statistical analysis were performed using Design Expert® software (version 8.0.5, Stat‐Ease, Minneapolis, MN, USA). A Box‐Behnken second‐order design was chosen to evaluate the combined effect of three independent variables‐extraction pressure, temperature, and time‐code as A, B, and C, respectively . The maximum and minimum extraction pressures were set at 15 and 25 MPa, extraction temperatures were 40 and 60°C, extraction times were 60 and 120 min, respectively.…”

C18-coated stir bar sorptive extraction combined with HPLC-ICP-MS for the speciation of butyltins in environmental samples

“…[18][19][20] Among these sample pretreatment techniques, SBSE has the advantages of high extraction efficiency, good reproducibility, high sensitivity, and less organic solvent consumption and has been successfully applied to the extraction of trace organic compounds, inorganic elements, and their species in environmental, food, and biological samples. [21][22][23][24][25][26] The methods that involve the use of SBSE for OT analysis are usually combined with derivatization-GC-ICP-MS 26 or GC-MS. 25 In these methods, the OTs adsorbed on the stir bar are thermally desorbed and introduced to the GC system. To date, the direct coupling of SBSE with HPLC-ICP-MS for OT analysis without derivatization has not been reported.…”