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Development and validation of two methods based on high‐performance liquid chromatography‐tandem mass spectrometry for determining 1,2‐benzopyrone, dihydrocoumarin, o ‐coumaric acid, syringaldehyde and kaurenoic acid in guaco extracts and pharmaceutical preparations
Author(s) -
Gasparetto João C.,
Guimarães de Francisco Thais M.,
Campos Francinete R.,
Pontarolo Roberto
Publication year - 2011
Publication title -
journal of separation science
Language(s) - English
Resource type - Journals
SCImago Journal Rank - 0.72
H-Index - 102
eISSN - 1615-9314
pISSN - 1615-9306
DOI - 10.1002/jssc.201000792
Subject(s) - chemistry , chromatography , derivatization , syringaldehyde , formic acid , ammonium formate , high performance liquid chromatography , trifluoroacetic acid , tandem mass spectrometry , mass spectrometry , vanillin , organic chemistry
In this study, two HPLC‐ESI‐MS/MS methods were developed and validated for the determination of 1,2‐benzopyrone (COU), o ‐coumaric acid (OCA), kaurenoic acid (KAU), syringaldehyde (SYR), and dihydrocoumarin (DIH) in guaco extracts and pharmaceutical preparations (syrup and oral solution). The chromatographic separation was achieved using a C18 XBridge 150×2.1‐mm (5‐μm particle size) column maintained at 25°C. The mobile phases consisted of a gradient of water and acetonitrile containing 0.05% formic acid or 5 mM ammonium formate for the positive and negative ion modes, respectively. All of the calibration curves showed excellent coefficients of correlation ( r ≥0.9970) over the ranges of 1.25–400 ng/mL for coumarin, 10–600 ng/mL for dihydrocoumarin, 5–250 ng/mL for KAU, and 25–500 ng/mL for o ‐coumaric acid and syringaldehyde. The range of recovery was 96.3–103% with an RSD% of <4.85% for intraday and interday precision. The results indicate that the developed methods are fast, efficient, and sensitive for the quantification of the guaco metabolites in extracts and pharmaceutical forms while avoiding purification and derivatization steps.