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A more desirable method was developed for the determination of fatty acid esters of 3-chloropropane-1,2-diol (3-MCPD esters) and 2-chloropropane-1,3-diol (2-MCPD esters) in vegetable oils. The conditions of hydrolysis, derivatization and extraction of the vegetable oil were optimized. The oil sample added with the isotopic labelled d(5)-3-MCPD ester and d(5)-2-MCPD ester was hydrolyzed with 0.50 mL of sodium methoxide (0.50 mol/L) for 1 min. And then the solution was derivatized with 0.25 mL of phenylbroronic acid solution, then the solution was neutralized with 3.0 mL acetic acid and cleaned up with 3.0 mL of hexane 2 times. The derivatized solution was extracted with 2.0 mL of ethyl acetate 3 times. The extract was dried at nitrogen flow and the residue was dissolved with 0.5 mL of isooctane, and then detected by gas chromatography-mass spectrometry. Under the optimized conditions, the response of MCPD esters was 15-33 times of that of DGF method and the relative percentage of isooctane's impurities removal was as high as 99.1% compared with that of ethyl acetate. The method performance was fully validated. Limit of detection (S/N = 3) and quantitation of MCPD ester were 65.0-76.0 mu g/kg and 210-250 mu g/kg, respectively. There was an excellent linear correlation between the ratio of the MCPD and its internal standard and the mass (r>0.9990) in the range of 25-500 ng of MCPD esters (shown by MCPD). When peanut oils was spiked with MCPD esters at levels of 250-1000 mu g/kg (n = 6), average recoveries were 81.1%-92.3% and 103%-120%, and relative standard deviation (RSD) was 6.3%-12.4% and 5.0%-9.5%, respectively. An excellent result was obtained with -0.5 of Z scope when the method was used for 3-MCPD ester proficiency test sponsored by Food Analysis Performance Assessment Scheme. It was concluded that the developed method was much better than DGF method (Deutsche Gesellschaft fur Fettwissenschaft Standard Method(III 186(2009)), especially in sensitivity, accuracy and preventing the contamination of GC-MS systems.
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CHINESE JOURNAL OF ANALYTICAL CHEMISTRY
ISSN: 0253-3820
CN: 22-1125/O6
Year: 2012
Issue: 9
Volume: 40
Page: 1329-1335
0 . 7 6 9
JCR@2012
1 . 2 0 0
JCR@2023
ESI Discipline: CHEMISTRY;
JCR Journal Grade:4
CAS Journal Grade:4
Cited Count:
WoS CC Cited Count: 8
SCOPUS Cited Count:
ESI Highly Cited Papers on the List: 0 Unfold All
WanFang Cited Count:
Chinese Cited Count:
30 Days PV: 10
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