تطوير و التحقق من مصدوقية طريقة استشراب سائل ذو تداخل محب للماء للتحديد الكمي للشائبة السامة للمورثات بيريدين في المادة الدوائية الفعالة ليناغلبتين

الملخص EN

A simple and sensitive liquid chromatography - ultraviolet detector method was developed for the quantitative determination of pyridine, a reactive reagent in synthesis of linagliptin.

The pyridine sample was analyzed on a Silica column (150 mm X 4 mm, 3 ^m) and the mobile phase used was buffer- acetonitrile (15:85, v/v) containing 10.0 mM ammonium acetate, the pH of buffer was adjufted with glacial acetic acid to 3.4.

The flow rate used was 1.3 ml/min and the detection was at 258 nm in HILIC (Hydrophilic Interaction Liquid Chromatography) mode.

The calibration curve showed good linearity over the concentration range of 0.34-4.50 ^g/ml with a square correlation coefficient of 0.9991.

Detection Limit (DL) and quantification limit (QL) were found to be 0.10 and 0.34 ^g/ml, respectively.

Recovery’s values were excellent in the range 95.39-104.64 %.

RSD % values of repeatability and intermediate precision were 1.97 and 1.52 %, respectively.

The developed method was validated as per ICH guidelines in terms of DL, QL, linearity, precision, accuracy, specificity and robuftness.