Chemical Identification of Botanical Components Using Liquid Chromatography/Mass Spectrometry
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Drug Information Journal, Vol. 32, pp. 4 7 1 4 8 5 , 1998 Printed in the USA. All rights reserved.
CHEMICAL IDENTIFICATION OF BOTANICAL COMPONENTS USING LIQUID CHROMATOGRAPHY/ MASS SPECTROMETRY EDWARD H. KERNS, KEVIN J. VOLK, JEFFREYL. WHITNEY, ROBYNA. ROURICK,AND MIKE S. LEE Bristol-Myers Squibb Pharmaceutical Research Institute, New Brunswick and Princeton, New Jersey, and Wallingford, Connecticut
The chemical identification of botanical products can be accomplished by obtaining a “profile” of the mixture components. Changes in this profile are powerjkl indicators of variations due to such factors as process differences, raw material source, or storage stability. Such a profile may be obtained using an analytical protocol based on liquid chromatography/mass spectrometry (LC/MS)techniques. This paper describes an analytical strategy using L U M S which can be used to rapidly characterize the components in complex materials and to support their research, development, and manufacturing. This strategy utilizes standard method approaches, a rapid “template ” approach for structure identification, and the application of databases of compounds to facilitate identification and consistency throughout the product lifetime. This analytical strategy is illustrated with the LUMS characterization of mixtures of taxanes from Taxus Brevifolia extracts and development of a tarane database. This LC/MS-based strategy provides effective information for the accelerating medicinal field. Key Words: Botanical; Identification; LCIMS; TAXOL’; Database
INTRODUCTION BOTANICAL EXTRACTS CONTAIN A complex mixture of natural compounds. The content of this mixture can change as a result of many factors, such as the specific identity of the botanical material, the growing and seasonal conditions, the environment of botanical material storage, the method of extraction, and the conditions of extract stor-
Presented at the DIA Workshop “Botanical Quality: Workshop on Identification and Characterization,” April 9-10, 1996, Washington, District of Columbia. Reprint address: Edward H. Kerns, Bristol-Myers Squibb Pharmaceutical Research Institute, 1 Squibb Drive, New Brunswick. NJ 08903-0191.
age. Achieving consistent content suggests the need for a detailed knowledge of the mixture components and reproducible strategies for monitoring consistency. A number of advanced techniques are available for the qualitative and quantitative analysis of complex mixtures. The analysis of natural extracts is, in many ways, more complex than the analysis of single component synthetic products. Typically, analysis of natural compounds has relied on a protocol involving: 1. Sample scale-up, 2. Extraction, 3. Solvent partitioning, 4. Column fractionation,
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E. H . Kerns, K. J. Volk, J. L. Whitney, R. A. Rourick, and M. S. h e
5. Profiling with an ultra violet (UV) detector and 6. Individual component spectroscopic analysis using nuclear magnetic resonance spectroscopy (NM
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