Određivanje razgradnih produkata diazepama spektrometrijom masa visoke razlučivosti

Each drug or pharmaceutical contains various organic or inorganic contaminants and degradable products that typically lag behind in drug during the manufacturing process, preparation of a medicated form or by storage of the drug. The degradable products can be generated under the influence of light, temperature, water or pH change, and may also occur during the preparation or storage of the pharmaceutical dosage form. Even in very small quantities, the presence of contamination can affect the efficacy and safety of drug use. In this study, a quick and efficient method for analysis of contaminants and degradation products of diazepam was developed. High efficiency liquid chromatography (UHPLC) coupled with mass spectrometry (LC-MS/MS) was used for determination and quantification of diazepam and his degradation products. Degradation products generated by forced degradation of diazepam in acid, alkaline solution, hydrogen peroxide, untreated sample, and under the influence of temperature and light, were determinated by the developed UHPLC method. Also, based on the developed method, their structures and possible pathways of fragmentation were assumed. Drylab software was used to determine the optimal conditions of chromatographic separation method (column temperature, composition of mobile phase, time gradient, pH).