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Ultrasound-assisted dispersive liquid-liquid microextraction for determination of three gliflozins in human plasma by HPLC/DAD.
Journal of Chromatography B ( IF 3 ) Pub Date : 2019-12-09 , DOI: 10.1016/j.jchromb.2019.121932
Mokhtar M Mabrouk 1 , Suzan M Soliman 2 , Heba M El-Agizy 2 , Fotouh R Mansour 1
Affiliation  

A novel, highly sensitive ultrasound-assisted dispersive liquid-liquid microextraction (UA-DLLME) high performance liquid chromatography with diode-array detection (HPLC/DAD) method was developed for the determination of empagliflozin, dapagliflozin and canagliflozin in human plasma using methanol as protein precipitating agent/disperser and 1-dodecanol as extracting solvent. The analytes were eluted with an isocratic mobile phase consisting of acetonitrile:aqueous 0.1% trifluoroacetic acid pH 2.5, (40:60, v/v), at a flow rate of 1 mL/min and UV detection at 210 nm. The microextraction conditions were optimized regarding type and volume of extractant, type of disperser, sample pH, extraction time and centrifugation time. Under the optimal conditions, the enrichment factors were 19 for empagliflozin, 27 for dapagliflozin and 50 for canagliflozin. Linearity ranges were 2-2500 ng/mL, 3.5-2500 ng/mL and 1.1-2500 ng/mL for empagliflozin, dapagliflozin and canagliflozin, respectively. The developed method employs very small volumes of organic solvents in sample extraction and allows determination of small concetrations of gliflozins in human plasma.

中文翻译:

超声辅助分散液-液微萃取,用于通过HPLC / DAD测定人血浆中的三种格列净。

开发了一种新型的高灵敏度超声辅助分散液-液微萃取(UA-DLLME)高效液相色谱-二极管阵列检测(HPLC / DAD)方法,以甲醇为标准品测定人血浆中的恩帕格列净,达格列净和坎格列净蛋白质沉淀剂/分散剂和1-十二烷醇作为提取溶剂。将分析物用等度流动相洗脱,该流动相由乙腈:0.1%三氟乙酸水溶液pH 2.5(40:60,v / v)组成,流速为1 mL / min,并在210 nm处进行UV检测。针对萃取剂的类型和体积,分散器的类型,样品的pH值,萃取时间和离心时间对微萃取条件进行了优化。在最佳条件下,依帕列净的富集因子为19,达帕列净的富集因子为27,而卡那列净的富集因子为50。依格列净,达格列净和canagliflozin的线性范围分别为2-2500 ng / mL,3.5-2500 ng / mL和1.1-2500 ng / mL。所开发的方法在样品提取中使用非常少量的有机溶剂,并可以测定人血浆中小浓度的格列净。
更新日期:2019-12-09
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