Salting-Out Induced Liquid-Liquid Microextraction for Alogliptin Benzoate Determination in Human Plasma by HPLC/UV

Abstract

Salting-out induced liquid-liquid microextraction method has been developed for plasma sample treatment before determination of alogliptin by high performance liquid chromatography with UV detection. Several parameters were optimized to achieve maximum enrichment including type of extractant, volume of extractant, type of anion, type of cation, salt amount and pH. The optimum conditions were achieved using 500 µL of acetonitrile, added to 1 mL of aqueous sample containing 250 mg of sodium chloride at pH 12. An RP-HPLC method was developed and validated according to the International Conference on Harmonization guidelines Q2 (R1). The method was linear in the concentration range of 0.1 to 50 µg/mL (correlation coefficient= 0.997). The limit of detection was 19 ng/mL and limit of quantitation was 60 ng /mL. The method was accurate and precise with a % recovery of 99.7% and a % relative standard deviation ranging between 1.5 and 2.5. These results showed that the salting-out induced liquid-liquid microextraction methods could be better than other sample preparation protocols in terms of sensitivity, easiness, solvent consumption and waste reduction.

Sugaring‐out induced homogeneous liquid‐liquid microextraction as an alternative mode for biological sample preparation: A comparative study

“…LLME F I G U R E 1 Chemical structures of the studied antivirals, antidiabetics, and β-blockers can be classified into homogeneous and heterogeneous types depending, on the extractant miscibility in water. Homogeneous liquid-liquid microextraction [5,6] involves using a water miscible organic solvent, such as acetonitrile, ethanol, or acetone, that can be separated from the aqueous sample using salts (in salting-out induced LLME; SALLME) [7][8][9] or sugars (in sugaringout induced LLME; SULLME) [10][11][12][13]. Heterogeneous LLME is similar to conventional LLE in using a water immiscible organic solvent, but the amount employed is very small (30-200 µL instead of 3-10 mL).…”