Citation: YI Qing, MIAO Hong, WU Yong-Ning. Derivatization-free Method for Chloropropanols Determination in Food by Online Gel Permeation Chromatography-Gas Chromatography-Triple Quadrupole Mass Spectrometry[J]. Chinese Journal of Analytical Chemistry, ;2016, 44(5): 678-684. doi: 10.11895/j.issn.0253-3820.150789 shu

Derivatization-free Method for Chloropropanols Determination in Food by Online Gel Permeation Chromatography-Gas Chromatography-Triple Quadrupole Mass Spectrometry

YI Qing ^1, ,
MIAO Hong ² ,
WU Yong-Ning ^1,2

1.
School of Food Science and Engineering, Wuhan Polytechnic University, Hubei Collaborative Innovation Center for Processing of Agricultural Products, Wuhan 430000, China;
2.
Key Laboratory of Food Safety Risk Assessment, Ministry of Health, China National Center for Food Safety Risk Assessment, Beijing, 100021, China

Received Date: 10 October 2015
Revised Date: 22 December 2015

Fund Project: This work was supported by the State Key Development Program for Basic Research of China (No. 2012CB720840)

A derivatization-free method for chloropropanols determination in food using online gel permeation chromatography-gas chromatography-triple quadrupole mass spectrometry (Online GPC-GC-MS/MS) with free of derivatization was established. The target compounds were 3-monochloropropane-1,2-diol (3-MCPD), 2-monochloro-propane-1,3-diol (2-MCPD), 1,3-dichloropropan-2-ol (1,3-DCP) and 2,3-dichloropropan-1-ol (2,3-DCP). Samples were spiked with isotope internal standards, and extracted by matrix solid-supported liquid-liquid extraction on the ExtrelutTM NT absorbent. Hexane was added to wash away the apolar matrix interferences and then ethyl acetate was used to extract the target compounds. The concentrated extracts were directly injected into Online GPC-GC-MS/MS. The good linear relationships for the four types of analytes were obtained in the concentration range of 0.005-1.000 mg/L with correlation coefficients not less than 0.999. The limits of detection and quantitation for chloropropanols in the food samples were in the ranges of 0.002-0.005 mg/kg, and 0.005-0.01 mg/kg respectively. The recoveries and the relative standard deviations (RSD, n=6) for the spiked blank samples at the levels of 0.02, 0.1, 0.5 mg/kg were in the ranges of 94.8%-106.3% (2.2%-10.3%), 91.8%-108.8% (2.1%-10.6%) and 83.1%-109.4% (1.3%-9.4%), respectively. The established method was applied to the samples of soy sauce, hydrolyzed vegetables protein solution and powder, cooking wine, chicken powder, bread and cake, and satisfactory results were acquired.
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