Mowaka S, Ayoub B M
Pharmazie. 2017 Feb 1;72(2):67-72. doi: 10.1691/ph.2017.6151.
A new UPLC-MS/MS method (method A), for simultaneous determination of alogliptin (ALN) and metformin (MET) in their recently approved pharmaceutical combination Kazano® tablets, was developed and compared to a new UHPLC-UV method (method B). Concerning method A, separation was achieved on Hypersil gold 50 mm × 2.1 mm (1.9 μm) column, using acetonitrile and 0.2 % formic acid aqueous solution as the mobile phase with a gradient elution. Electrospray ionization (ESI) source was operated in positive ion mode. Selected reaction monitoring (SRM) mode on a triple quadropole mass spectrometer was used to quantify the drugs utilizing the transitions of 340.33 → 116.32 (m/z) and 130.12 → 71.32 (m/z) for ALN and MET, respectively. Concerning chromatographic separation using UV detection in method B, it was achieved on a Symmetry® C18 column 100 mm × 2.1 mm (2.2 μm) applying an isocratic elution based on methanol - water (10:90, v/v) at pH 3 as a mobile phase. The photodiode array detector was operated at 210 nm. Method A showed good linearity over the concentration ranges of 5-400 ng mL-1 and 25-2000 ng mL-1 for ALN and MET, respectively, while method B showed satisfactory results using ranges of 0.25-8 μg mL-1 and 5-50 μg mL-1 for ALN and MET, respectively. The optimized validated methods are suitable for QC labs but the UPLC-MS/MS method offered the advantage of shorter analytical times and higher sensitivity and selectivity.
开发了一种用于同时测定最近获批的复方药物Kazano®片剂中阿格列汀（ALN）和二甲双胍（MET）的超高效液相色谱-串联质谱新方法（方法A），并与一种超高效液相色谱-紫外新方法（方法B）进行了比较。关于方法A，在Hypersil gold 50 mm×2.1 mm（1.9μm）色谱柱上进行分离，使用乙腈和0.2%甲酸水溶液作为流动相进行梯度洗脱。电喷雾电离（ESI）源在正离子模式下运行。在三重四极杆质谱仪上采用选择反应监测（SRM）模式，分别利用340.33→116.32（m/z）和130.12→71.32（m/z）的离子跃迁对ALN和MET进行定量。关于方法B中使用紫外检测的色谱分离，在Symmetry® C18 100 mm×2.1 mm（2.2μm）色谱柱上进行，以甲醇-水（10:90，v/v）在pH 3下作为流动相进行等度洗脱。光电二极管阵列检测器在210 nm波长下运行。方法A在ALN和MET的浓度范围分别为5 - 400 ng mL-1和25 - 2000 ng mL-1时显示出良好的线性，而方法B在ALN和MET的浓度范围分别为0.25 - 8 μg mL-1和5 - 50 μg mL-1时显示出满意的结果。优化验证后的方法适用于质量控制实验室，但超高效液相色谱-串联质谱方法具有分析时间短、灵敏度和选择性更高的优势。
