Abstract—3-Chloro-1,2-propanediol (3-chloropropanediol) is a well-known food processing contaminant found in a wide range of foods and ingredients and there has been recent concern about the levels of carcinogenic 3-chloropropanediol (3-MCPD) in some soy sauces. This paper reports on the development of an analytical method for the fast determination of 3-MCPD at trace level in commercial soy sauce using novel liquid phase extraction (LPE)/cleanup coupled with microwave-assisted derivatization (MAD) method followed by high performance liquid chromatography-ultraviolet (HPLC-UV) detection. In this method, 3-MCPD was first isolated from soy sauce sample matrix by LPE/cleanup with Extrude NT3 column cartridges and the isolated (eluent) solution was subjected to MAD with acetophenone to form 2-methyl-2-phenyl-4-(chloromethyl)-1,3-dioxolane under microwave irradiation using a specially modified domestic microwave oven, then the derivatizeddioxolane was directly analyzed with a HPLC-UV system. The optimum conditions for MAD such as the ratio of reagents, acidic catalyst, microwave irradiation power and time, as well as the chromatographic conditions were thoroughly investigated. Experimental results indicated that maximum derivatization can be achieved in 10 min under microwave irradiation at 362 watts when compared to 18 hours by conventional refluxing reaction. The proposed method provided a simple and rapid analytical procedure for 3-MCPD analysis in soy sauce with the detection limit of 80 ng mL-1. The relative standard deviations were all below 3.0 % (n = 7). Application was illustrated by the analysis of commercial sauce sample obtained from a local traditional store in central Taiwan.
Keywords—3-Chloropropanediol,liquid phase extraction,microwave-assisted derivatization,sample preparation, soy sauce.
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