Authors: Gryniewicz-Ruzicka, Connie M.; Arzhantsev, Sergey; Pelster, Lindsey N.; Westenberger, Benjamin J.; Buhse, Lucinda F.; Kauffman, John F.

Source: Applied Spectroscopy, Volume 65, Issue 3, Pages 58A-92A and 243-357 (March 2011) , pp. 334-341(8)

Publisher: Society for Applied Spectroscopy

Abstract:

The transfer of a multivariate calibration model for quantitative determination of diethylene glycol (DEG) contaminant in pharmaceutical-grade glycerin between five portable Raman spectrometers was accomplished using piecewise direct standardization (PDS). The calibration set was developed using a multi-range ternary mixture design with successively reduced impurity concentration ranges. It was found that optimal selection of calibration transfer standards using the Kennard-Stone algorithm also required application of the algorithm to multiple successively reduced impurity concentration ranges. Partial least squares (PLS) calibration models were developed using the calibration set measured independently on each of the five spectrometers. The performance of the models was evaluated based on the root mean square error of prediction (RMSEP), calculated using independent validation samples. An F-test showed that no statistical differences in the variances were observed between models developed on different instruments. Direct cross-instrument prediction without standardization was performed between a single primary instrument and each of the four secondary instruments to evaluate the robustness of the primary instrument calibration model. Significant increases in the RMSEP values for the secondary instruments were observed due to instrument variability. Application of piecewise direct standardization using the optimal calibration transfer subset resulted in the lowest values of RMSEP for the secondary instruments. Using the optimal calibration transfer subset, an optimized calibration model was developed using a subset of the original calibration set, resulting in a DEG detection limit of 0.32% across all five instruments.

Keywords: PORTABLE RAMAN SPECTROMETERS; RAPID SCREENING; PARTIAL LEAST SQUARES REGRESSION; PLS; CALIBRATION TRANSFER; PIECEWISE DIRECT STANDARDIZATION; PDS; PHARMACEUTICAL ANALYSIS; GLYCERIN

Document Type: Research article

DOI: http://dx.doi.org/10.1366/10-05976

Affiliations: 1: US Food and Drug Administration, Center for Drug Evaluation and Research, Division of Pharmaceutical Analysis, St. Louis, Missouri 63101, USA

Publication date: 2011-03-01

More about this publication?

• The Society publishes the internationally recognized, peer reviewed journal, Applied Spectroscopy, which is available both in print and online. Subscriptions are included with membership or can be purchased by institutional or corporate organizations. Abstracts may be viewed free of charge.
  
  Previously published as Bulletin (Society for Applied Spectroscopy)
• Editorial Board
• Information for Authors
• Submit a Paper
• Subscribe to this Title
• Membership Information
• Request copyrighted SAS materials
• Spectroscopic Nomenclature
• Focus Compendium
• ingentaconnect is not responsible for the content or availability of external websites

Related content

• In this: publication
• By this: publisher
• In this Subject: Analytical Chemistry
• By this author: Gryniewicz-Ruzicka, Connie M. ;  Arzhantsev, Sergey ;  Pelster, Lindsey N. ;  Westenberger, Benjamin J. ;  Buhse, Lucinda F. ;  Kauffman, John F.

Website © Publishing Technology. Article copyright remains with the publisher, society or author(s) as specified within the article.

• Terms and conditions
• Privacy policy
• Information for advertisers