Development and validation of a liquid chromatography-tandem mass spectrometry method to determine intact glucosinolates in bee pollen
| Autor: | Ana María Ares Sacristán, José Luis Bernal Yagüe, JOSÉ BERNAL DEL NOZAL, María Jesús Nozal |
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| Rok vydání: | 2015 |
| Předmět: |
Formic acid
Electrospray ionization Glucosinolates Clinical Biochemistry Analytical chemistry Tandem mass spectrometry Biochemistry Analytical Chemistry chemistry.chemical_compound Limit of Detection Tandem Mass Spectrometry Liquid chromatography–mass spectrometry Animals Solid phase extraction Detection limit Chromatography Reproducibility of Results Glucotropaeolin Cell Biology General Medicine Bees chemistry Bee pollen Linear Models Pollen Chromatography Liquid |
| Zdroj: | Journal of Chromatography B. 1000:49-56 |
| ISSN: | 1570-0232 |
| Popis: | A new method was developed to determine twelve intact-glucosinolates (GLSs) (glucoiberin, GIB; glucoraphanin, GRA; glucoerucin GER; gluconapin, GNA; glucotropaeolin, GTL; glucobrassicin, GBC; gluconasturtiin, NAS; glucoalyssin, ALY; 4-hydroxyglucobrassicin, 4OH; 4-methoxyglucobrassicin, 4ME; neoglucobrassicin, NEO; sinigrin, SIN) in bee pollen, by means of liquid chromatography tandem mass spectrometry (LC-MS/MS) with electrospray ionization (ESI). An efficient extraction procedure was proposed (average analyte recoveries were between 85% and 96%); this involved a solid-liquid extraction (SLE) with heated water, followed by a solid phase extraction (SPE) with a weak anion exchange (NH2) sorbent. Chromatography was performed on a Gemini(®) C18 analytical column with a mobile phase of formic acid in water (0.5%,v/v) and formic acid in acetonitrile (0.5%,v/v), in gradient elution mode at 1mL/min, resulted in baseline-separated peaks and a run time of 30min. The method was fully validated in terms of selectivity, limits of detection (LOD) and quantification (LOQ), linearity, carry-over effect, reinjection reproducibility, precision and accuracy. A good selectivity, low LODs and LOQs, ranging from 1 to 16μg/kg, wide linear ranges from LOQ to 1000μg/kg, and satisfactory reinjection reproducibility, precision and accuracy with relative standard deviation and relative error values lower than or equal to 9%; meanwhile, results indicates a negligible carry-over effect. The proposed method was applied to analyze intact-GLSs in bee pollen. Nine of the GLSs studied were identified in certain samples analyzed over a wide concentration range (LOQ-2226μg/kg), and significant differences in GLS content were observed among the samples. |
| Databáze: | OpenAIRE |
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