Xu Xiaomin, Ren Yiping, Wu Pinggu, Han Jianlong, Shen Xianghong
Laboratory of Food Safety and Hygienic Chemistry Analysis, Zhejiang Provincial Center for Disease Prevention and Control, Hangzhou, 310009, People's Republic of China.
Food Addit Contam. 2006 Feb;23(2):110-9. doi: 10.1080/02652030500391929.
Both gas chromatography-mass spectrometry in electron ionization (GC-MS-EI) and negative chemical ionization (GC-MS-NCI) modes are reported in this paper for the simultaneous determination of 1,3-dichloropropan-2-ol (1,3-DCP), 2,3-dichloropropan-1-ol (2,3-DCP), 3-chloropropane-1,2-diol (3-MCPD) and 2-chloropropane-1,3-diol (2-MCPD) in soy sauce and other flavoring. D(5)-3-MCPD (for 3-MCPD and 2-MCPD) and d(5)-1,3-DCP (for 1,3-DCP and 2,3-DCP) were used as the deuterium isotopic labelled internal standards. The feasibility of using heptafluorobutyric anhydride modified with triethylamine (HFBA-Et(3)N) as a new derivatization reagent to replace heptafluorobutyrylimidazole (HFBI) is proposed. Liquid/liquid extraction with hexane was introduced for high lipid content samples. A small survey was carried out of soy sauces (103 samples) and instant noodles (45 samples) and the applicability of GC-MS-NCI and GC-MS-EI was assessed in these different matrices.
本文报道了采用气相色谱 - 质谱联用仪的电子电离模式（GC-MS-EI）和负化学电离模式（GC-MS-NCI）同时测定酱油及其他调味品中1,3 - 二氯丙醇（1,3-DCP）、2,3 - 二氯丙醇（2,3-DCP）、3 - 氯 - 1,2 - 丙二醇（3-MCPD）和2 - 氯 - 1,3 - 丙二醇（2-MCPD）的方法。采用D(5)-3-MCPD（用于3-MCPD和2-MCPD）和d(5)-1,3-DCP（用于1,3-DCP和2,3-DCP）作为氘同位素标记内标。提出了用三乙胺改性的七氟丁酸酐（HFBA-Et(3)N）作为新的衍生化试剂替代七氟丁酰咪唑（HFBI）的可行性。对于高脂含量样品，采用正己烷液 - 液萃取。对103份酱油样品和45份方便面样品进行了小规模调查，并评估了GC-MS-NCI和GC-MS-EI在这些不同基质中的适用性。
