Analytical Sciences

Abstract − Analytical Sciences, 21(11), 1343 (2005).

Determination of 3-Chloropropane-1,2-diol in Liquid Hydrolyzed Vegetable Proteins and Soy Sauce by Solid-Phase Microextraction and Gas Chromatography/Mass Spectrometry
Minjia HUANG,* Guibin JIANG,* Bin HE,* Jingfu LIU,* Qingxiang ZHOU,* Wusheng FU,** and Yongning WU**
*Key Laboratory of Environmental Chemistry and Ecotoxicology, Research Center for Eco-Environmental Sciences, Chinese Academy of Sciences, P. O. Box 2871, Beijing 100085, China
**Chinese Disease Control Center, Beijing, 100050, China
Headspace solid-phase microextraction (HS-SPME) coupled with gas chromatography/mass spectrometry (GC/MS) method was developed to determine 3-chloropropane-1,2-diol (3-MCPD) in hydrolyzed vegetable protein and Chinese soy sauce. The 3-MCPD was firstly derivativized with phenylboronic acid in aqueous solution at 90°C for 10 min, then extracted by HS-SPME and finally detected with GC/MS, parameters related to both the derivative reaction and the HS-SPME process were optimized. The proposed method has a linear range of 0.0194 - 394 µg g-1, a detection limit of 3.87 ng g-1 (S/N = 3), and a precision of RSD = 7.5% (n = 5). Seventeen real samples, including four HVPs and thirteen soy sauce samples, were analyzed to examine the feasibility of the proposed procedure; with a concentration of 3-MCPD and acceptable recoveries at 0.71 µg g-1 spiked levels were obtained. Being simpler, faster and more environmentally benign than the existing methods, this method is accurate and suitable for routine analysis.