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Study on Synthesis of 13C, 15N3-Semicarbazide Hydrochloride |
WANG Wei;DU Xiao-ning;LIU Zhan-feng;LI Liang-jun;SONG Ming-ming;LI Jie |
Shanghai Research Institute of Chemical Industry, Shanghai 200062, China |
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Abstract The 13C,15N2 doubly labeled Urea and 15N2 labeled Hydrazine hydrate were used as raw materials, and 13C,15N3-SEM·HCl was synthesized by a direct one-step synthesis which based on the reflux reacting. The reaction conditions of 13C,15N3 labeled semicarbazide hydrochloride were mainly investigated by the experiment designs, like singlefactor design and orthogonal design. The following optimized conditions were obtained as follow: the mole ratio 15N2-N2H4 to 13C,15N2-urea was 1.4∶1, the reaction temperature was 135 ℃, the reaction time was 4.5 h, and the yield of 13C,15N3 labeled semicarbazide hydrochloride was above 90%, the purity ≥98%, the abundance of 13C ≥97%, the abundance of 15N ≥99%. This technology had many advantages, like short production cycle, high yield and sample later-processing.
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Received: 01 January 1900
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[1] |
刘德炎.动物性食品中兽药残留的现状、问题及对策[J]. 养殖与饲料,2009, 34(2):14-15.
|
[2] |
Off J Europ Communities,Commission Regulation (EC)1442/95 [J/OL]. Official Journal of the Europeen Union, 1995, 143: 26-30. [2010-08-30] http://eur-lex.europa.eu/pri/en/oj/dat/2003/1071.pdf.
|
[3] |
World Health Organization. Evaluation of certain veterinary drug residues in foods: report of the 40th meeting of the JECFA[R]. Geneva:WHO,1993, 85:85-90.
|
[4] |
Commission Decision 2003/181/EC, March 13, 2003, amending decision 2002/657/EC as regards the setting of minimum required performance limits (MRPLs) for certain residues in food of animal origin [J/OL]. Official Journal of the European Union, 2003, 71:17-18.[2010-08-30] http://eur-lex.europa.eu/pri/en/oj/dat/2003/l_071/l_07120030315en00170018.pdf.
|
[5] |
Effkemann S, Feldhussen F. Triple-quadrupole LC-MS-MS for quantitative determination of nitrofuran metabolites in complex food matrixes[J]. Analytical and Bioanalytical Chemistry, 2004, 378(4): 842-844.
|
[6] |
Becalski A, Lau BPY, Lewis D, et al. semicarbazide formation in azodicarbonamidetreated flour: a model study[J]. Jagric Food Chem, 2004, 52 (18): 5 730-5 734
|
[7] |
李述文,范如霖. 实用有机化学手册[M]. 上海:上海科学技术出版社,1981: 315.
|
[8] |
潘丽军,陈锦权. 试验设计与数据处理[M]. 南京:东南大学出版社,2008: 100-140.
|
[9] |
马正飞,殷翔. 数学计算方法与软件的工程应用[M]. 北京:化学工业出版社,2002: 215-223.
|
|
|
|