以D4-甲醇为原料,通过酯化、N-甲基化、缩合等过程合成得到稳定同位素标记D6-结晶紫,利用均匀设计法,研究了投料比、三氯氧磷用量、反应温度和反应时间对合成结晶紫的影响.实验数据通过多元回归分析,得出了优化的工艺条件.目标产物的结构经质谱(MS)、核磁(NMR)和高效液相色谱(HPLC)等表征,化学纯度高于98.0％,同位素丰度高于99.5％(atom D),可作为食品安全领域检测用同位素内标试剂.
参考文献
| [1] | REN Xiulian,WEI Qifeng,QU Jing,et al.Determination of Malachite Green,Crystal violet and Its Metabolites in Aquatic Products by RP-HPLC[J].Chem Anal Meter,2006,15(4):32-34(in Chinese).任秀莲,魏琦峰,曲径,等.反相高效液相色谱法测定水产品中孔雀石绿、结晶紫及其代谢物[J].化学分析计量,2006,15(4):32-34. |
| [2] | GU Fu,LI Xuezhe,GONG Yaozhong,et al.Determination of Crystal Violet and Its Ramifications in Aquatic Products by HPLC[J].Mod Instrum,2006,12(4):35-37(in Chinese).谷福,李学哲,弓耀忠,等.高效液相色谱法测定水产品中结晶紫及其衍生物的残留[J].现代仪器,2006,12:35-37. |
| [3] | ZHANG Zhigang,SHI Bing,CHEN Luping,et al.Simultaneous Determination and Confirmation of Malachite Green,Crystal Violet and Their Leuco Metabolites Residues in Aquatic Product by Liquid Chromatography-Visible Detection and Tandem Mass Spectrometric Detection[J].Chinese J Anal Chem,2006,34(5):663-667(in Chinese).张志刚,施冰,陈鹭平,等.液相色谱法同时测定水产品中孔雀石绿和结晶紫残留[J].分析化学,2006,34(5):663-667. |
| [4] | SHAO Shengwen,WEN Sheng,WANG Yan,et al.Alalysis of Malachite Green and Crystal Violet Residues in Freshwater Fishes in Hubei Province[J].J Public Health Prev Med,2011,22(2):49-50(in Chinese).邵生文,闻胜,王艳,等.湖北省淡水鱼中孔雀石绿、结晶紫监测结果分析[J].公共卫生与预防医学,2011,22(2):49-50. |
| [5] | WU Shihui,ZHU Xinping,ZHENG Guangming,et al.Determination of Malachite Green and Gentian Violet Residues in Fishery Products by High Performance Liquid Chromatography (HPLC) with Fluorescence Detector[J].J Guangdong Ocean Univ,2009,29(1):54-57(in Chinese).吴仕辉,朱新平,郑光明,等.高效液相色谱法检测水产品中的孔雀石绿和结晶紫[J].广东海洋大学学报,2009,29(1):54-57. |
| [6] | LIN Hong,FU Xiaoting,QIU Xujian,et al.Determination of Residues of Malachite Green,Gentian Violet and Their Metabolites in Fish Tissues by High-Performance Liquid Chromatography[J].Period Ocean Univ China,2006,36(6):919-922(in Chinese).林洪,付晓婷,邱绪建,等.液相色谱法测定鱼肌肉中孔雀石绿、结晶紫及其代谢物[J].中国海洋大学学报(自然科学版),2006,36(6):919-922. |
| [7] | Mitrowska K,Posyniak A.Determination of Malachite Green and Leucomalachite Green in Carp Muscle by Liquid Chromatography with Visible and Fluorescence Detection[J].J Chromatogr A,2005,1089 (1/2):187-192. |
| [8] | XIE Wen,DING Huiying,XI Junyang,et al.Determination of the Malachite Green,Crystal Violet and Their Metabolites Residues in Aquatic Animals[J].Chinese J Chromatogr,2006,24(5):529-530(in Chinese).谢文,丁慧瑛,奚君阳,等.水产品中孔雀石绿、结晶紫及其代谢产物残留量的检测[J].色谱,2006,24(5):529-530. |
| [9] | Wu X L,Zhang G,Wu Y N,et al.Simultaneous Determination of Malachite Green,Gentian Violet and Their Leucometabolites in Aquatic Products by High-performance Liquid Chromatography linear Ion Trap Mass Spectrometry[J].J Chromatogr A,2007,1172(2):121-126. |
| [10] | ZHU Kuanzheng,WANG Peng,LIN Yanfei,et al.Simultaneous Determination of Residues of Malachite Green,Crystal Violet and Their Leuco Metabolites in Aquatic Products by Liquid Chromatography-Tandem Mass Spectrometry[J].Chinese J Chromatogr,2007,25(1):66-69(in Chinese).朱宽正,王鹏,林雁飞,等.液相色谱-串联质谱法同时测定水产品中孔雀石绿、结晶紫以及它们的隐色代谢物残留[J].色谱,2007,25(1):66-69. |
| [11] | WANG Peng,ZHU Kuanzheng,LIN Yanfei,et al.Rapid Determination of Residues of Crystal Violet and Its Metabolite Leucocrystal Violet in Aquatic Products by Liquid Chromatography Tandem Mass Spectrometry[J].J Anal Sci,2006,22 (3):283-286(in Chinese).王鹏,朱宽正,林雁飞,等.液相色谱-串联质谱法快速测定水产品中结晶紫及其隐色代谢物残留[J].分析科学学报,2006,22(3):283-286. |
| [12] | George B,John F,Edward W.Isotope Dilution Mass Spectrometry and the National Reference System[J].Anal Chem,1993,65(12):475-479. |
| [13] | LUO Yong,YANG Weicheng,LIU Weixia.Syntheses of Labeled 13C6-Crystal Violet and 13C6-Leucocrystal Violet[J].Fine Chem,2011,28(10):950-953(in Chinese).罗勇,杨维成,刘卫霞.稳定同位素标记13C6-结晶紫和13 C6-隐色结晶紫的合成[J].精细化工,2011,28(10):950-953. |
| [14] | Yang W C,Luo Y,Liu W X,et al.An Efficient Synthesis of[D6]-Leucocrystal Violet[J].J Label Comp Radio,2011,54(4):211-213. |
| [15] | YANG Weicheng,QI Qingrui,LIU Weixia,et al.Synthesis of Isotope-Labeled 15 N-N,N-Dimethylaniline[J].Chinese J Org Chem,2012,32(1):145-148(in Chinese).杨维成,齐庆瑞,刘卫霞,等.稳定同位素标记15NN,N-二甲基苯胺的合成[J].有机化学,2012,32(1):145-148. |
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