Document Detail


In-line measurement of a drug substance via near infrared spectroscopy to ensure a robust crystallization process.
MedLine Citation:
PMID:  16937335     Owner:  NLM     Status:  MEDLINE    
Abstract/OtherAbstract:
The crystallization of Etoricoxib, a polymorphic compound, has been optimized and controlled by seeding with the desired polymorph at a moderate supersaturation condition. To enhance the process robustness, near infrared spectroscopy (NIRS) has been evaluated as an inline measurement method for the concentration of Etoricoxib prior to seeding in the crystallization process. In this NIRS method, a spectral discriminant analysis based on principal component analysis (PCA) was established to detect the presence of solids produced by premature crystallization, or bubbles in the path of light. Once a spectrum was qualified as that of clear solution, concentration of Etoricoxib was calculated by a NIRS calibration model built with partial least squares (PLS) regression and with offline HPLC analysis as the reference method. This model was accurate with a standard error of cross validation (SECV) less than 1.2 mg/g Etoricoxib and a standard error of prediction (SEP) less than 1.7 mg/g over the concentration range from 50 to 170 mg/g, temperature range from 49 to 65 degrees C, and different sources of materials. In addition, all aspects of the offline HPLC method, especially the sampling procedure, were optimized to provide an accurate reference for NIRS calibration models. The application of this method at a pilot plant has demonstrated its capability of accurately measuring the process concentration of Etoricoxib as well as detecting the presence of solids produced by premature crystallization before seeding.
Authors:
George X Zhou; Louis Crocker; Jing Xu; Jose Tabora; Zhihong Ge
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Publication Detail:
Type:  Journal Article    
Journal Detail:
Title:  Journal of pharmaceutical sciences     Volume:  95     ISSN:  0022-3549     ISO Abbreviation:  J Pharm Sci     Publication Date:  2006 Nov 
Date Detail:
Created Date:  2006-09-26     Completed Date:  2007-01-04     Revised Date:  -    
Medline Journal Info:
Nlm Unique ID:  2985195R     Medline TA:  J Pharm Sci     Country:  United States    
Other Details:
Languages:  eng     Pagination:  2337-47     Citation Subset:  IM    
Copyright Information:
Copyright 2006 Wiley-Liss, Inc. and the American Pharmacists Association
Affiliation:
Merck and Co., Inc., Merck Research Laboratories, Rahway, New Jersey 07065, USA. george.zhou@merck.com
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MeSH Terms
Descriptor/Qualifier:
Calibration
Chromatography, High Pressure Liquid
Crystallization
Data Interpretation, Statistical
Indicators and Reagents
Mass Spectrometry
Pharmaceutical Preparations / chemistry*
Solvents
Spectroscopy, Near-Infrared
Temperature
Chemical
Reg. No./Substance:
0/Indicators and Reagents; 0/Pharmaceutical Preparations; 0/Solvents

From MEDLINE®/PubMed®, a database of the U.S. National Library of Medicine


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