Extraction and determination of trace amounts of chlorpromazine in biological fluids using magnetic solid phase extraction followed by HPLC

A simple, rapid and sensitive method termed as magnetic solid phase extraction （MSPE） combined with high-performance liquid chromatography-ultraviolet detector （HPLC-UV） has been proposed for the determination of trace amounts of chlorpromazine （CPZ） in water, urine and plasma samples. The separation and determination was performed on a C18 column under the optimal chromatographic conditions. Several factors influencing the extraction efficiency of CPZ, such as pH, surfactant and adsorbent amounts, ionic strength, extraction time, sample volume and desorption conditions, were studied and optimized. Under the optimal MSPE conditions, the extraction percentage of CPZ was 74%, 27% and 16% in water, urine and plasma samples, respectively. The limits of detection （LODs） of the proposed approach were 0.1, 5.0 and 10ng/mL in water, urine and plasma samples, respectively. The relative standard deviations （RSDs） based on five replicate determinations at 10 ng/mL level of CPZ was 1.2%. Good linear behaviors over the investigated concentration ranges （0.25-300 ng/mL） with good coefficient of determination, R2 〉 0.9998, were obtained. Good spike recoveries with relative errors less than 9.0% were obtained when applying the proposed method to water, urine and plasma samples.

LC-MS/MS assay for olanzapine in human plasma and its application to a bioequivalence study

This paper describes a selective and sensitive assay for the determination of olanzapine(OLZ)in human plasma based on liquid chromatography-tandem mass spectrometry(LC-MS/MS).The analyte and quetiapine as internal standard(IS)were extracted from 200μL plasma via solid phase extraction on Waters Oasis HLB cartridges.Chromatographic separation was achieved on an ACE 5C18-300 column(100 mm × 4.6 mm,5μm)under isocratic conditions in a run time of 3.5 min.Mass spectrometric detection involved electrospray ionization in the positive ion mode followed by multiple reaction monitoring(MRM)of the transitions at m/z 313/256 for OLZ and m/z 384/253 for the IS.The assay was linear in the range 0.10-40.0 ng/mL with a lower limit of quantitation and limit of detection of 0.10 and 0.012 ng/mL,respectively.Intra-and inter-day precision(as coefficient of variation)and relative recovery were<5.0% and>90%,respectively.The method was succesfully applied to a bioequivalence study of 5 and 10 mg OLZ disintegrating tablets in 40 healthy Indian males with reproducibility by incurred sample reanalysis in the range-7.43 to 8.07%.