Direct Determination of Glycidyl Esters of Fatty Acids in Vegetable Oils by LC–MS

Blumhorst, Michael R.; Venkitasubramanian, Padmesh; Collison, Mark W.

doi:10.1007/s11746-011-1873-1

Cited by 25 publications

(16 citation statements)

References 7 publications

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“…The quality of indirect methodology has improved, and there are now several methods that appear to provide accurate quantitative information for these classes of contaminants (Kuhlmann 2011;Ermacora & Hrncirik 2013). As a response to the lack of reliability of the early indirect methods, direct approaches were developed for GEs (Blumhorst et al 2011;DuBois et al 2011;Firestone 2011;Haines et al 2011;Becalski et al 2012;Hori, Koriyama, et al 2012) and 3-MCPD esters (Haines et al 2011;Dubois et al 2012;Hori, Koriyama, et al 2012;Hori, Matsubara, et al 2012;Moravcova et al 2012;Yamazaki et al 2013) that do not require hydrolysis and analyse the fatty acid esters as they occur in processed oils without any structural modification. However, due to limitations with each of these direct approaches, methods were developed and validated in our laboratory at the USFDA the LC-MS/MS quantitation of intact esters of 3-MCPD and glycidol in edible oils MacMahon, Mazzola, et al 2013).…”

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confidence: 99%

Occurrence of 3-MCPD and glycidyl esters in edible oils in the United States

MacMahon

Begley

Diachenko

2013

Food Additives & Contaminants: Part A

125

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Fatty acid esters of 3-monochloropropanediol (3-MCPD) and glycidol are processing contaminants found in a wide range of edible oils. While both 3 MCPD and glycidol have toxicological properties that at present has concerns for food safety, the published occurrence data are limited. Occurrence information is presented for the concentrations of 3-MCPD and glycidyl esters in 116 retail and/or industrial edible oils and fats using LC-MS/MS analysis of intact esters. The concentrations for bound 3-MCPD ranged from below the limit of quantitation (

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confidence: 99%

Occurrence of 3-MCPD and glycidyl esters in edible oils in the United States

MacMahon

Begley

Diachenko

2013

Food Additives & Contaminants: Part A

125

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“…A similar approach to analysis by LC-MS (single stage quadrupole) using custom made internal standards of 7 GEs was also outlined by Granvogl and Schieberle [19]. Another recent paper described single stage quadrupole LC-MS analysis of GEs in vegetable oils without any purification using D31 glycidyl palmitate as an internal standard with LOQ in the range of 200-600 μg/kg [20].…”

Section: Introductionmentioning

confidence: 99%

Glycidyl fatty acid esters in food by LC-MS/MS: method development

et al. 2012

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An improved method based on liquid chromatography-tandem mass spectrometry (LC-MS/MS) for the analysis of glycidyl fatty acid esters in oils was developed. The method incorporates stable isotope dilution analysis (SIDA) for quantifying the five target analytes: glycidyl esters of palmitic (C16:0), stearic (C18:0), oleic (C18:1), linoleic (C18:2) and linolenic acid (C18:3). For the analysis, 10 mg sample of edible oil or fat is dissolved in acetone, spiked with deuterium labelled analogs of glycidyl esters and purified by a two-step chromatography on C18 and normal silica solid phase extraction (SPE) cartridges using methanol and 5% ethyl acetate in hexane, respectively. If the concentration of analytes is expected to be below 0.5 mg/kg, 0.5 g sample of oil is pre-concentrated first using a silica column. The dried final extract is re-dissolved in 250 μL of a mixture of methanol/isopropanol (1:1, v/v), 15 μL is injected on the analytical C18 LC column and analytes are eluted with 100% methanol. Detection of target glycidyl fatty acid esters is accomplished by LC-MS/MS using positive ion atmospheric pressure chemical ionization operating in Multiple Reaction Monitoring mode monitoring 2 ion transitions for each analyte. The method was tested on replicates of a virgin olive oil which was free of glycidyl esters. The method detection limit was calculated to be in the range of 70-150 μg/kg for each analyte using 10 mg sample and 1-3 μg/kg using 0.5 g sample of oil. Average recoveries of 5 glycidyl esters spiked at 10, 1 and 0.1 mg/kg were in the range 84% to 108%. The major advantage of our method is use of SIDA for all analytes using commercially available internal standards and detection limits that are lower by a factor of 5-10 from published methods when 0.5 g sample of oil is used. Additionally, MS/MS mass chromatograms offer greater specificity than liquid chromatography-mass spectrometry operated in selected ion monitoring mode. The method will be applied to the survey of glycidyl fatty acid esters in food products on the Canadian market.

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“…Therefore, methods to provide accurate quantification of GE are required. Blumhorst et al [9] reported a direct liquid chromatography-mass spectrometry (LC-MS) method which can be used as a screening method to quantify GE in processed oil samples. These researchers reported acceptable method recovery and repeatability, but Masukawa et al [6] reported a rapid decline in instrument signal/noise following injection of diluted oils without further clean-up.…”

Section: Introductionmentioning

confidence: 99%

Collaborative Study for the Analysis of Glycidyl Fatty Acid Esters in Edible Oils using LC–MS

Blumhorst

Collison

Cantrill

et al. 2012

J Americ Oil Chem Soc

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An interlaboratory study was conducted to evaluate a method for determining glycidyl fatty acid esters (GE) in edible oils. Samples were dissolved in tert‐butyl methyl ether/ethyl acetate and subjected to two solid‐phase extraction (SPE) steps. The first SPE step utilized methanol elution from a C18 cartridge, and the second SPE step utilized n‐hexane/ethyl acetate elution from a silica cartridge. The final extract was analyzed using liquid chromatography with a single quadrupole mass spectrometer in selected ion monitoring (SIM) mode. Quantification was performed using external standardization. Eighteen samples (9 oils × 2 blind duplicates) were assayed for glycidyl palmitate, glycidyl stearate, glycidyl oleate, glycidyl linoleate and glycidyl linolenate by 17 collaborating laboratories from seven countries. Sample matrices included palm, olive, corn, soybean and rapeseed oils. Repeatability (RSDr) ranged from 6.85 to 19.88 % and reproducibility (RSDR) ranged from 16.58 to 35.52 % for samples containing greater than 0.5 mg/kg of individual GE. HORRATR values ranged from 0.62 to 14.70 for determination of total GE. The method provides acceptable results for quantification of GE in edible oils.

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Direct Determination of Glycidyl Esters of Fatty Acids in Vegetable Oils by LC–MS

Cited by 25 publications

References 7 publications

Occurrence of 3-MCPD and glycidyl esters in edible oils in the United States

Occurrence of 3-MCPD and glycidyl esters in edible oils in the United States

Glycidyl fatty acid esters in food by LC-MS/MS: method development

Collaborative Study for the Analysis of Glycidyl Fatty Acid Esters in Edible Oils using LC–MS

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