Determination of desipramine in biological samples using liquid-liquid-liquid microextraction combined with in-syringe derivatization, gas chromatography, and nitrogen/phosphorus detection

作者：Saraji Mohammad^*; Mehrafza Narges; Bidgoli Ali Akbar Hajialiakbari; Jafari Mohammad Taghi

来源：Journal of Separation Science, 2012, 35(19): 2637-2644.

DOI：10.1002/jssc.201200334

• Derivatization
• Desipramine
• Hollow fiber-based liquid-liquid-liquid microextraction
• Plasma
• Urine

A method was established for the determination of desipramine in biological samples using liquidliquidliquid microextraction followed by in-syringe derivatization and gas chromatographynitrogen phosphorus detection. The extraction method was based on the use of two immiscible organic solvents. n-Dodecane was impregnated in the pores of the hollow fiber and methanol was placed inside the lumen of the fiber as the acceptor phase. Acetic anhydride was used as the reagent for the derivatization of the analyte inside the syringe barrel. Parameters that affect the extraction efficiency (composition of donor and acceptor phase, ionic strength, sample temperature, and extraction time) as well as derivatization efficiency (amount of acetic anhydride and reaction time and temperature) were investigated. The limit of detection was 0.02 mu g/L with intra and interday RSDs of 2.6 and 7.7%, respectively. The linearity of the method was in the range of 0.220 mu g/L (r2 = 0.9986). The method was successfully applied to determine desipramine in human plasma and urine.

• 出版日期2012-10