Separation and identification of glucosinolates from Brassica vegetables using high-performance capillary gas chromatography (GC)-positive-ion chemical ionization mass spectrometry (PICIMS) and GC-PICIMS/MS

Abstract

LITERATURE CITED Aldrich Library of Infrared Spectra, 3rd ed. Pouchent, C. J., Ed.; Aldrich: Milwaukee, WI, 1981; p 1242D. Alpert, N. L.; Keiser, W. E.; Szymanski, H. A. IR-Theory and Practice of Infrared Spectroscopy; Plenum: New York, 1973; Bourne, S.; Reedy, G. T.; Coffey, P. J.; Mattson, D. Matrix Isolation GC/FTIR. Am. Lab. 1984, 16, 90-95. Christensen, B. W.; Kjaer, A.; Madsen, J. 0.; Olsen, C. E.; Olsen, 0.; Sorensen, H. Mass Spectrometric Characteristics of Some Pertrimethylsilyl Desulfoglucosinolates. Tetrahedron 1982, 38, 353-357. Ettlinger, M. A,; Lundeen, A. J. First Synthesis of a Mustard Oil Glucoside; The Enzymatic Lossen Rearrangement.A new, general-purpose analytical procedure for identification of desulfoglucosinolates from Brassica vegetables has been developed by combining high-performance capillary gas chromatography (HPCGC) with positive-ion chemical ionization mass spectrometry (PICIMS) and PICIMS/MS. HPCGC on a 25 m X 0.2 mm Ultra 1 WCOT fused silica column gave highly reproducible base-line separation of alkyl, alkenyl, hydroxyalkenyl, aryl, and indole desulfoglucosinolates as their per(trimethylsily1)desulfoglucosinolate analogues. PICIMS and PICIMS/MS of these compounds using methane as the reagent gas gave conventional and daughter ion mass spectra in which the major ions were highly diagnostic of the glucosinolate structure.

Plant Metabolites and Nutritional Quality of Vegetables

“…Chemical derivatization (for example, trimethylsilylation) can often be employed to increase the volatility of compounds containing polar functional groups (for example, –OH, –COOH, –NH 2 ), thereby extending the range of potential analytes to such compounds as steroids, organic acids, amino acids, and small peptides (Adams and others 1999; Lehotay and Hajšlová 2001). Gas chromatography was applied to analyze flavonols (Bilyk and others 1984), glucosinolates (Shaw and others 1989), sterols (Normén and others 1999), phenolic acids (Robbins 2003), polysaccharides (Villanueva‐Suárez and others 2003), and aroma compounds (Jeleń and others 2000) in vegetables and their products.…”

High‐performance liquid chromatographic separation of natural and synthetic desulphoglucosinolates and their chemical validation by UV, NMR and chemical ionisation‐MS methods

“…Sulphate-release assay Schnug (1987Schnug ( , 1988 Arguello et al (1999) iv. Capillary GC-MS, GC-MS, GC-MS-MS Shaw et al (1987Shaw et al ( , 1989 sinolates are commonly separated using end-capped C 18 reverse phase columns eluted with water:acetonitrile gradients, whilst isocratic elution with water:methanol phases has also been reported for the separation of both desulphoglucosinolates and intact glucosinolates (Table 1). In this paper we report details of species and tissues that are good sources of glucosinolate standards, details of macro-and micro-glucosinolate extraction methods, and optimised desulphation conditions for subsequent analysis by reverse-phase HPLC.…”

Determination of two intact glucosinolates in vegetables and Chinese herbs

“…Derivatization of glucosinolates has allowed the use of gas chromatography (GC) [17,18] and gas chromatographymass spectrometry (GC-MS) [13] for the determination of their parent compounds in vegetables. GC and GC-MS have also been used for separating and detecting trimethylsilylated derivatives of desulfoglucosinolates that are products after the sulfate group has been removed by a sulfohydrolase [19,20]. High-performance liquid chromatography (HPLC) analysis of the desulfoglucosinolates has also been developed [21,22,23] and established as the official reference method of the European Community [24].…”