title: Quantitative analysis of binary polymorphs mixtures of fusidic acid by diffuse reflectance FTIR spectroscopy, diffuse reflectance FT-NIR spectroscopy, Raman spectroscopy and multivariate calibration.
abstract: Vibrational spectroscopic techniques such as infrared, near-infrared and Raman spectroscopy have become popular in detecting and quantifying polymorphism of pharmaceutics since they are fast and non-destructive. This study assessed the ability of three vibrational spectroscopy combined with multivariate analysis to quantify a low-content undesired polymorph within a binary polymorphic mixture. Partial least squares (PLS) regression and support vector machine (SVM) regression were employed to build quantitative models. Fusidic acid, a steroidal antibiotic, was used as the model compound. It was found that PLS regression performed slightly better than SVM regression in all the three spectroscopic techniques. Root mean square errors of prediction (RMSEP) were ranging from 0.48% to 1.17% for diffuse reflectance FTIR spectroscopy and 1.60-1.93% for diffuse reflectance FT-NIR spectroscopy and 1.62-2.31% for Raman spectroscopy. The results indicate that diffuse reflectance FTIR spectroscopy offers significant advantages in providing accurate measurement of polymorphic content in the fusidic acid binary mixtures, while Raman spectroscopy is the least accurate technique for quantitative analysis of polymorphs.
authors.affiliation: School of Pharmacy, China Pharmaceutical University, Nanjing 211198, China.
authors.forename: Canyong
authors.initials: C
authors.lastname: Guo
authors.affiliation: Center for Pharmaceutical Quality Research, School of Science, China Pharmaceutical University, Nanjing 210038, China; Key Laboratory of Drug Quality Control and Pharmacovigilance (China Pharmaceutical University), Ministry of Education, Nanjing 210009, China. Electronic address: liuluo21998@126.com.
authors.forename: Xuefang
authors.initials: X
authors.lastname: Luo
authors.affiliation: Jiangsu Institute for Food and Drug Control, Nanjing 210008, China.
authors.forename: Xiaohua
authors.initials: X
authors.lastname: Zhou
authors.affiliation: Jiangsu Institute for Food and Drug Control, Nanjing 210008, China.
authors.forename: Beijia
authors.initials: B
authors.lastname: Shi
authors.affiliation: Shimadzu (China) Co., Ltd., Block E, No. 570 West Huaihai Road, Shanghai 200052, China.
authors.forename: Juanjuan
authors.initials: J
authors.lastname: Wang
authors.affiliation: World (Jiangsu) Industry Co., Ltd., No. 56 Renmin Middle Road, Yancheng 224001, China.
authors.forename: Jinqi
authors.initials: J
authors.lastname: Zhao
authors.affiliation: School of Science, China Pharmaceutical University, Nanjing 211198, China.
authors.forename: Xiaoxia
authors.initials: X
authors.lastname: Zhang
mesh_terms: D002138:Calibration; D005672:Fusidic Acid; D016018:Least-Squares Analysis; D017550:Spectroscopy, Fourier Transform Infrared; D019265:Spectroscopy, Near-Infrared; D013059:Spectrum Analysis, Raman
chemical_list: D005672:Fusidic Acid
keywords: Diffuse reflectance FT-NIR; Diffuse reflectance FTIR; Fusidic acid; Partial least square; Polymorphism; Raman