Study On Quality Standards Of Furazolidone And Rosiglitazone

Study on the Quality Standard of FurazolidoneFurazolidone is a synthetic nitrofuran antibacterial drug. It is mainly used for treating intestinal infection caused by dysentery bacillus, escherichia coli, etc. In Chinese Pharmacopiea2010(ChP2010) and British Pharmacopiea2009(BP2009),5-nitro-2-furaldehyde diacetate was detected by thin layer chromatography (TLC), and related substances were not been checked. Although some literatures reported the determination of furazolidone,5-nitro-2-furaldehyde diacetate and metabolites by high performance liquid chromatography (HPLC) and liquid chromatography-mass spectroscopy (LC-MS), the determination of other purities were not found.To control the quality of furazolidone and improve its quality standard, the method for quality control of furazolidone was systematically studied. Furazolidone was identified specifically by ultraviolet (UV) spectrophotometry, infrared (IR) spectrophometry and chemical reaction. By reference to the USP32, BP2009and ChP2010, the determination method for5-nitro-2-furaldehyde diacetate was revised as HPLC, and the determination method for the related substances was added. The HPLC method is more specific, more accurate and more sensitive than the TLC method. The HPLC conditions were as follows:The separation was performed on a Alltima C18column (150mm×4.6mm,5u m) using water-acetonitrile as mobile phase with gradient elution. The linear gradient programwas0min(90%water)â†'10min (50%water)â†'20min (95%water)â†'30min (95%water)â†'35min (90%water). The flow rate of mobile phase was1.0ml·min-1. The double detection wavelengthes were set at303nm for5-nitro-2-furaldehyde diacctate. Furazolidone and its degradation products were effectively separated by validated HPLC method. There was a good linearity between the peak area and the concentration of5-nitro-2-furaldehyde diacctate over the range of0.503～7.548μg·ml-1. The average recovery of5-nitro-2-furaldehyde diacctate was100.0%(RSD=0.5%, n=9). The detection limits of furazolidone and5-nitro-2-furaldehyde diacetate were1.53ng and0.20ng, respectively. The UV method is used to assay the content of furazolidone. The linear range of the determination by UV was2.357～11.786μg·ml-1. The results demonstrated that the established standard could be used for the quality control of furazolidone.Study on the Quality Standard of RosiglitazoneRosiglitazone is an anti-diabetic drug of thiazolidinedione class. It can reduce blood glucose concentration by increasing the tissue sensitivity to insulin and improve the utilization of glucose. Its mechanism is activating the peroxisome proliferator-activated receptor-s (PPARs), reducing the resistance to insulin. Alone and combination can treat the type2diabetes, metabolic syndrome, polycystic ovarian syndrome (PCOS), etc.At present, there are multiple standards for rosiglitazone preparation. The different evaluation results of related substances and dissolution of rosiglitazone preparations were found when different standards were used, indicating that the existing methods of related substances determination and dissolution evaluation should be improved. In this paper, HPLC-UV method was used for determining the related substances of rosiglitazone preparations. The chromatographic conditions were as follows:The analysis was achieved on a Diamonsil C18column (250mm X4.6mm,5μm) using a mobile phase of0.025mol-L-’ammonium acetate-acetonitrile (50:50) as mobile phase. The flow rate of mobile phase was1.0ml·min-1and detection wavelength was at245nm. There was good resolution among the peak of rosiglitazone, the main related substances and the degradable impurities by destroying. The limit of detection was0.43ng. A paddle method with acetate buffer solution (pH4.0) as media was proposed to investigate the dissolution of rosiglitazone preparations. The details were as follows:900ml of acetate buffer solution (pH4.0), rotation speed of50r-min-1, HPLC assay was achieved on a C18column using a mobile phase of phosphate-acetonitrile (50:50), the detection wavelength was at245nm. The results showed that the exploratory dissloution measurement method has better resolution ability for different quality products.