title: Optimization of an Indirect Enzymatic Method for the Simultaneous Analysis of 3-MCPD, 2-MCPD, and Glycidyl Esters in Edible Oils.
abstract: We developed a novel, indirect enzymatic method for the analysis of fatty acid esters of 3-monochloro-1,2-propanediol (3-MCPD), 2-monochloro-1,3-propanediol (2-MCPD), and glycidol (Gly) in edible oils and fats. Using this method, the ester analytes were rapidly cleavaged by Candida rugosa lipase at room temperature for 0.5 h. As a result of the simultaneous hydrolysis and bromination steps, 3-MCPD esters, 2-MCPD esters, and glycidyl esters were converted to free 3-MCPD, 2-MCPD, and 3-monobromo-1,2-propanediol (3-MBPD), respectively. After the addition of internal standards, the mixtures were washed with hexane, derivatized with phenylboronic acid, and analyzed by gas chromatography-mass spectrometer (GC-MS). The analytical method was evaluated in preliminary and feasibility studies performed by 13 laboratories. The preliminary study from 4 laboratories showed the reproducibility (RSD R ) of < 10% and recoveries in the range of 102-111% for the spiked 3-MCPD and 2-MCPD in extra virgin olive (EVO) oil, semi-solid palm oil, and solid palm oil. However, the RSDR and recoveries of Gly in the palm oil samples were not satisfactory. The Gly content of refrigerated palm oil samples decreased whereas the samples at room temperature were stable for three months, and this may be due to the depletion of Gly during cold storage. The feasibility studies performed by all 13 laboratories were conducted based on modifications of the shaking conditions for ester cleavage, the conditions of Gly bromination, and the removal of gel formed by residual lipase. Satisfactory RSDR were obtained for EVO oil samples spiked with standard esters (4.4% for 3-MCPD, 11.2% for 2-MCPD, and 6.6% for Gly).
authors.affiliation: Central Research & Development Institute, House Foods Group Inc.
authors.forename: Kazuo
authors.initials: K
authors.lastname: Koyama
authors.forename: Kinuko
authors.initials: K
authors.lastname: Miyazaki
authors.forename: Kousuke
authors.initials: K
authors.lastname: Abe
authors.forename: Keiich
authors.initials: K
authors.lastname: Ikuta
authors.forename: Yoshitsugu
authors.initials: Y
authors.lastname: Egawa
authors.forename: Tadashi
authors.initials: T
authors.lastname: Kitta
authors.forename: Hirotsugu
authors.initials: H
authors.lastname: Kido
authors.forename: Takashi
authors.initials: T
authors.lastname: Sano
authors.forename: Yukinari
authors.initials: Y
authors.lastname: Takahashi
authors.forename: Toru
authors.initials: T
authors.lastname: Nezu
authors.forename: Hidenori
authors.initials: H
authors.lastname: Nohara
authors.forename: Takashi
authors.initials: T
authors.lastname: Miyashita
authors.forename: Hiroshi
authors.initials: H
authors.lastname: Yada
authors.forename: Kumiko
authors.initials: K
authors.lastname: Yamazaki
authors.forename: Yomi
authors.initials: Y
authors.lastname: Watanabe
mesh_terms: D002175:Candida / Q000201:enzymology; D057075:Enzyme Assays / Q000379:methods*; D004852:Epoxy Compounds / Q000032:analysis*; D004952:Esters; D005240:Feasibility Studies; D008401:Gas Chromatography-Mass Spectrometry; D005990:Glycerol / Q000031:analogs & derivatives* / Q000032:analysis; D054879:Halogenation; D008049:Lipase; D000069463:Olive Oil / Q000737:chemistry*; D000073878:Palm Oil; D010938:Plant Oils / Q000737:chemistry*; D020005:Propanols / Q000032:analysis*; D013696:Temperature; D000517:alpha-Chlorohydrin / Q000032:analysis*; D011409:Propylene Glycols
chemical_list: D004852:Epoxy Compounds; D004952:Esters; D005990:Glycerol; D008049:Lipase; D000069463:Olive Oil; D000073878:Palm Oil; D010938:Plant Oils; D020005:Propanols; D000517:alpha-Chlorohydrin; C585004:monochloropropanediol; D011409:Propylene Glycols; C004312:glycidol