GC‐MS Analysis of Various Phytoestrogens in Health Functional Foods

Abstract

This study aimed to measure phytoestrogen contents in health functional foods (HFFs) to alleviate menopausal symptoms that are commercially available in South Korea. A sensitive and selective method using gas chromatography-mass spectrometry (GC-MS) for the monitoring of 21 phytoestrogens was developed and fully validated. Phytoestrogens were extracted by liquid-liquid extraction using methyl tert-butylether as the solvent. Food samples were enzymatically hydrolyzed with β-glucuronidase/arylsulfatase. Before GC-MS, the analytes were derivatized to their trimethylsilyl derivatives by incubation with N,O-bis(trimethylsilyl)trifluoroacetamide with 1% trimethylchlorosilane for 30 min at 80 C. The calibration curves showed good linearity (r 2 > 0.99) in the range of interest for each analyte. The limits of detection and quantification of the 21 phytoestrogens were in the ranges of 0.5-20 and 1-50 ng/mL, respectively. The intra-and inter-day precisions were all below 15.7%. These multivariate procedures were efficient in determining the optimal conditions using peak heights as responses.

Detection of Phytoestrogen Metabolites in Breastfed Infants’ Urine and the Corresponding Breast Milk by Liquid Chromatography–Tandem Mass Spectrometry

“…Currently, the most popular methods are gas chromatography with mass spectrometry (GC–MS), liquid chromatography with mass spectrometry (LC–MS), and high-performance liquid chromatography (HPLC) . GC–MS was reported to be capable of detecting several PEs simultaneously in food or biological samples, but it often includes tedious sample pretreatment, especially the derivatization procedure. , LC–MS can effectively separate different PEs, with an LOD lower than that of GC–MS. Thus, the sensitive and robust LC–MS method has been extensively used in PE detection. , In this study, we optimized a method of liquid–liquid extraction coupled with ultrahigh-performance LC–MS/MS to measure 10 PE metabolites (genistein, daidzein, glycitein, enterodiol, enterolactone, equol, coumestrol, quercetin, secoisolariciresinol, and isorhamntein) simultaneously in paired infant urine–breast milk samples.…”

“…38 GC−MS was reported to be capable of detecting several PEs simultaneously in food or biological samples, but it often includes tedious sample pretreatment, especially the derivatization procedure. 39,40 LC−MS can effectively separate different PEs, with an LOD lower than that of GC−MS. Thus, the sensitive and robust LC−MS method has been extensively used in PE detection.…”

Concentration Determination of Volatile Molecular Iodine and Methyl Iodide

“…Accordingly, the use of a gas chromatograph with a detector or with a mass spectrometer may be a more suitable method than the UV–Vis spectrophotometry. Although using gas chromatography (GC) is not a new and original idea for quantitative analysis of organic species, routine use of GC for CH 3 I requires not only a reliable sampling method involving, for example, either the capture of CH 3 I in a chromatography solvent or liquid–liquid extraction (LLE) of CH 3 I from aqueous solutions but also a calibration curve established for the analyte (and an analysis system) . Establishment of a sampling method should start with the selection of a solvent because, to the best of our knowledge, optimal solvents have not been reported for CH 3 I analysis.…”