Development Of Purity Reference Material Of Glimepiride And Amidopyrine

Glimepiride and Amidopyrine are two common medicines used widely in China.However,how to prepare standard compounds for their purity determination has not been reported.Therefore,the reliability of the purity check for their products,especially results from different labs,is low.In this thesis,we aim to develop standard glimepiride and amidopyrine for their purity determination.In addition,the homogeneity and stability of glimepiride and amidopyrine are also determined.The UV,IR,and Liquid chromatography–mass spectrometry(LC-MS)were used to confirm the structure of glimepiride and amidopyrine used in this study.High performance liquid chromatography(HPLC)methods with acetonitrile/water as mobile phases and C18 columns as stationary phases.Potentiometric titration methods were also used to determine the purify of these two analytes.The results showed that the linearity to determine purity of glimepiride by HPLC is0.02mg/mL~0.50 mg/mL with a correlation coefficient of 1.The inter-day,intra-day precision,and stability are 0.513%,0.014% and 0.017% respectively.For the titration method,acid-basic electrode was used with 95% of ethanol as the solvent.Sodium hydroxide(0.1 mol/L)was used as the titrant.The result of method validation suggested that this novelty titration method is accurate and reproducible.The results also showed that the linearity to determine purity of amidopyrine by HPLC is 0.02mg/mL~0.50 mg/m with a correlation coefficient of 0.99999.The inter-day,intra-day precision,and stability are 0.150%,0.060% and 0.112% respectively.For the titration method,nonaqueous titrations was used with glacial acetic acid and acetyl oxide as the solvents.The results showed that the linearity of this titration method is 70-120%with a correlation coefficient of 0.99998.The RSD of reproducibility and stability are0.17% and 0.09%,respectively.The detection limit is 15 mg.The uncertainties of glimepiride and amidopyrine are 99.70%±0.80%(k=2,P=0.95)and 99.41%±0.90%(k=2,P=0.95),respectively.The homogeneity and short term stability in 14 days of and long term stability in 12 months for glimepiride and amidopyrine are in acceptable range.Sensitive and reproducible HPLC and titration methods were established to determine the purity of glimepiride and amidopyrine.The purifies of the two analytes are in acceptable range,which can be used as standard reference in the relevant analysis.