IMBP - Institute for Biomedical and Pharmaceutical Research, Paul-Ehrlich-Straße 19, D-90562, Nürnberg-Heroldsberg, Germany.
University of Cologne, Faculty of Medicine and University Hospital Cologne, Center for Pharmacology, Department I of Pharmacology, Gleueler Str. 24, D-50931, Cologne, Germany.
J Pharm Biomed Anal. 2019 Oct 25;175:112754. doi: 10.1016/j.jpba.2019.07.002. Epub 2019 Jul 3.
This article describes the development and validation of a HILIC-MS/MS method for the simultaneous quantification of metformin and sitagliptin from human plasma and urine. The presented method uses quick sample preparation and fast chromatography allowing for high sample throughput. The quantification is performed using multi-reaction monitoring and ESI positive mode with stable isotope labelled internal standards for both metformin and sitagliptin. Excellent linearity in the selected calibrations ranges, low inter-day variability (CV% <6.7%), and high accuracy (95.5-104.1%) were obtained. Adequate retention was attained for both analytes by hydrophilic interaction liquid chromatography using a plain silica column in combination with a mobile phase composed of ammonium formate, acetonitrile, formic acid and water in gradient separation mode.
本文描述了一种用于同时定量测定人血浆和尿液中二甲双胍和西他列汀的亲水相互作用色谱-串联质谱（HILIC-MS/MS）方法的开发和验证。所提出的方法采用快速样品制备和快速色谱，允许高样品通量。通过多反应监测和电喷雾正离子模式进行定量分析，同时使用稳定同位素标记的内标物对二甲双胍和西他列汀进行定量分析。在选定的校准范围内，获得了良好的线性（<6.7%的日内变异系数）和高准确度（95.5-104.1%）。通过在梯度分离模式下使用含有甲酸铵、乙腈、甲酸和水的流动相在普通硅胶柱上进行亲水相互作用液相色谱，实现了两种分析物的充分保留。
