Abstract

Dipeptidyl peptidase-4 inhibitors, so-called gliptins, constitute a fairly novel class of oral hypoglycemic agents. The development and validation of an automated online SPE-LC-UV method to determine intact sitagliptin, saxagliptin, vildagliptin and metformin simultaneously in human urine samples were performed. For the two-dimensional chromatographic separation, a Gemini C18 (250.0 × 4.6 mm i.d., 110 A⁰, 5.0 μ) analytical column and a gradient elution with 10.0 mM o-phosphoric acid and methanol and for the online SPE analysis of urine samples, a LiChrospher® ADS SPE-column (20.0 mm × 2.0 mm i.d., 25.0 μm) were used through the study. The fractionation, transfer, elution and separation of the spiked urine samples were achieved in just 9.57 min runtime with 12.0 mL of solvent consumption which was green and economical compared to other sample preparation methods. The calibration curves were determined to be linear in a wide range of 0.10–100.00 μg/mL with satisfactory regression coefficients. Method developed for two-dimensional determination of gliptins would be useful as a reference in therapeutic drug monitoring and screening for forensic medical cases which involve the abuse, unintentional or misuse of multiple gliptins in terms of its practical use, easy detection and reliable results.

中文翻译：

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交叉参考二维液相色谱法测定尿液中完整的脂肪素。

摘要

二肽基肽酶-4抑制剂，所谓的脂肪素，构成一类相当新颖的口服降糖药。进行了自动在线SPE-LC-UV方法的开发和验证，该方法可以同时测定人尿液样品中的完整西他列汀，沙格列汀，维达列汀和二甲双胍。对于二维色谱分离，一个双子C18（250.0×4.6毫米内径，110中的⁰，5.0μ）分析柱，并用10.0mM的梯度洗脱邻通过这项研究，使用磷酸和甲醇以及尿液样品的在线SPE分析，使用了LiChrospher®ADS SPE色谱柱（内径20.0 mm×2.0 mm，25.0μm）。加标尿液样品的分离，转移，洗脱和分离仅需9.57分钟即可完成，消耗的溶剂量为12.0 mL，与其他样品制备方法相比，绿色环保且经济。确定的校准曲线在0.10–100.00μg/ mL的宽范围内呈线性，并且回归系数令人满意。开发用于脂蛋白二维测定的方法将可作为法医案件的治疗药物监测和筛查的参考，这些法医在实际使用，易于检测和可靠结果方面涉及滥用，无意或滥用多种脂蛋白。