Near Infrared Spectroscopy In Analysis Of Finished Pharmaceutical Products And Active Pharmaceutical Ingredients

Near infrared spectroscopy(NIRS),combined with chemometric techniques,is becoming a popular analytical method for the drug quality control because it is sample-nondestructive,real-time and available for process analysis.In this paper,the feasibility of detection of microbial contamination in tazarotene gel,determination of ultra low-content active pharmaceutical ingredient(API)in tazarotene gel and identification of glimepiride cis-trans-isomer was evaluated by using NIRS.OBJECTIVES:1.To establish NIRS for the detection of microbial contamination in tazarotene gel.2.To establish NIRS for the determination of ultra low-content API in tazarotene gel.3.To establish NIRS for the identification of glimepiride cis-trans-isomer.METHODS:1.Detection of microbial contamination in tazarotene gel by NIRS.The near infrared transflectance spectra(NIRTFS)of 61 tazarotene gel samples were measured within the range of 10000 – 4000 cm-1 using the resolution of 8 cm-1,64 co-averaged scans,and the specimen holder thickness of 1 mm.Based on the NIRTFS,the discriminant analysis(DA)and counter propagation artificial neural network(CP-ANN)models were used to detect microbial contamination in tazarotene gel samples.2.Determination of ultra low-content API in tazarotene gel by NIRS.The NIRTFS of 61 tazarotene gel samples were measured within the range of 10000 – 4000 cm-1 using the resolution of 8 cm-1,64 co-averaged scans,and the specimen holder thickness of 1 mm.Based on the NIRTFS,the partial least squares(PLS)model was built to determine ultra low-content API in tazarotene gel samples.3.Identification of glimepiride cis-trans-isomer by NIRS.Each near infrared diffuse reflectance spectrum(NIRDRS)of 12 glimepiride samples was the 64 co-averaged scans at 4 cm-1 resolution within the range of 10000 – 4000 cm-1.The DA and CP-ANN models were used to identify glimepiride cis-trans-isomer based on the NIRDRS.RESULTS:1.Detection of microbial contamination in tazarotene gel by NIRS.The established DA model reaches the classification accuracy of calibration(CAC)100.0% and the classification accuracy of validation(CAV)100.0%.The established CP-ANN model owns the CAC 100.0%,the classification accuracy of cross validation(CACV)100.0%,and the CAV 100.0%.2.Determination of ultra low-content API in tazarotene gel by NIRS.The established PLS model has the correlation coefficient of calibration(Rc)0.9780,the correlation coefficient of cross validation(Rcv)0.9491,the correlation coefficient of validation(Rv)0.9656,the root mean square error of calibration(RMSEC)0.0154 mg/g,the root mean square error of cross validation(RMSECV)0.0232 mg/g,the root mean square error of validation(RMSEV)0.0215 mg/g,and the bias 0 mg/g.3.Identification of glimepiride cis-trans-isomer by NIRS.The established DA model possesses the CAC 100.0% and the CAV 100.0%.The established CP-ANN model reaches the CAC 100.0%,the CACV 100.0%,and the CAV 100.0%.CONCLUSIONS:1.The microbial contamination in tazarotene gel can be detected accurately using the established NIRS.2.The ultra low-content API in tazarotene gel can be determined accurately using the established NIRS.3.The glimepiride cis-trans-isomer can be identified accurately using the established NIRS.