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 attained 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 M10. The method was linear in the concentration range of 0.1 to 50 µg/mL (correlation coefficient = 0.997). The limit of detection was 0.019 µg/mL and limit of quantitation was 0.06 µg/mL. The method was accurate and precise with an average % 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.

Menthol-assisted homogenous liquid-liquid microextraction for HPLC/UV determination of favipiravir as an antiviral for COVID-19 in human plasma

“…The extractant volume is one of the most important experimental variables that could affect the enrichment in HLLE. Generally, the analyte pre-concentration is inversely proportional to the volume of extractant [25] , and thus small volumes of THF were tested in the range of 100–900 μL. The results ( Fig.…”

Construction and application of highly sensitive spinel nanocrystalline zinc chromite decorated multiwalled carbon nanotube modified carbon paste electrode (ZnCr2O4@MWCNTs/CPE) for electrochemical determination of alogliptin benzoate in bulk and its dosage form: green chemistry assessment

“…7 While ALG as benzoate salt is more soluble in water than alogliptin free base. 8 ALG has been determined spectrophotometric, [9][10][11] spectro-uorometric, 12,13 chromatographic, [14][15][16][17][18][19][20] and HPTLC. 21 While the literature review revealed no electrochemical method.…”

“…ALG has been determined spectrophotometric, 9–11 spectrofluorometric, 12,13 chromatographic, 14–20 and HPTLC. 21 While the literature review revealed no electrochemical method.…”

Hantzsch condensation reaction as a spectrofluorometric method for determination of alogliptin, an antidiabetic drug, in pure form, tablet form, and human and rat plasma

“…[ 1–3 ] ALO’s scientific name is 2‐[[6‐[(3R)‐3‐aminopiperidin‐1‐yl]‐3‐methyl‐2,4‐dioxopyrimidin‐1‐yl][2]methyl]benzonitrile (Figure 1) with empirical formula C 18 H 21 N 5 O 2. [ 4 ] Some attempts have been made to estimate ALO either alone or in conjunction with other medications, including using capillary electrophoresis, [ 5 ] conductometry, [ 6 ] high performance liquid chromatography (HPLC), [ 7–30 ] spectrophotometry, [ 7,17,31–36 ] spectrofluorometry, [ 37,38 ] and thin‐layer chromatography [ 27,39–41 ] methods. The use of costly reagents (e.g.…”