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.

中文翻译：

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盐析诱导液液微萃取用于人血浆中HPLC / UV测定阿格列汀苯甲酸酯

已经开发了盐析诱导液-液微萃取方法，用于血浆样品处理，然后通过高效液相色谱和紫外检测器测定阿格列汀。优化了几个参数以实现最大富集，包括萃取剂的类型，萃取剂的体积，阴离子的类型，阳离子的类型，盐量和pH。使用500 µL乙腈，将其添加到1 mL含有250 mg氯化钠的pH值为12的含水样品中，可获得最佳条件。根据国际协调会议M10的要求，开发并验证了RP-HPLC方法。该方法在0.1至50 µg / mL的浓度范围内呈线性（相关系数= 0.997）。检测限为0.019 µg / mL，定量限为0.06 µg / mL。该方法准确准确，平均回收率达99.7％，相对标准偏差％在1.5至2.5之间。这些结果表明，在敏感性，易用性，溶剂消耗和废物减少方面，盐析诱导的液-液微萃取方法可能比其他样品制备方案更好。