Simultaneous determination of impurities and degradation products by rapid RP-UPLC-MS method

[摘要] The present article describes the development and validation studies on products of testosterone (Ts) in bulk drugs. The validation parameters include system suitability, specificity, accuracy, precision, linearity, limit of detection and limit of quantification. In addition to this, the stability of main drug has also been validated. Experiments have been carried out by using Ultra high Performance Liquid Chromatography, which is highly sophisticated and of superior technology instrumentation coupled to mass detector (UPLC-MS).Unlike HPLC, the products of forced degradation and impurities in testosterone can be accurately measured by using the mass detector in UPLC. Further Rapid analysis and high sensitive method was achieved by using hybrid technology column with linear gradient elution of mobile phase. The chromatogram was analyzed at 245 nm with a run time of 6.0 minutes. Linearity graph range was 10-150 % and trueness was at three levels of 50-150% of the specification limit. The detection and quantification limit of the method for impurities was 1.6 & 5 % of the specification limit. Test drug testosterone was found degradation towards the acidic, basic, thermal and oxidative conditions and was stable for other conditions as well, confirmed by mass detector. Application of the derived method over the older and slower HPLC methods was useful for a 10 fold increase in speed analysis of the test samples in various fields like process development R & D and quality control of bulk drug manufacturing. The study was analyzed as per ICH Q1A (R2) and Q2 (R1) guidelines.

[学科分类] 药理学