高效液相色谱法快速测定小麦粉及其添加剂中三聚硫氰酸三钠盐  

Rapid determination of 2,4,6-trimercaptotriazine trisodium(TMT)in wheat flour and flour treatment agents by high performance liquid chromatography

作　　者：尹丽丽 张艳侠 武传香 薛霞 孙珊珊 王明栋 胡梅 刘艳明 祝建华 YIN Lili;ZHANG Yanxia;WU Chuanxiang;XUE Xia;SUN Shanshan;WANG Mingdong;HU Mei;LIU Yanming;ZHU Jianhua(Shandong Institute for Food and Drug Control,Shanrlong Research Center of Engineering and Technology for Quality Control of Food for Special Medical Puqioses,Shandong Research Center of Engineering and Technology for Safety Inspection of Food and Drug,Jinan 250101)

机构地区：[1]山东省食品药品检验研究院,山东省特殊医学用途配方食品质量控制工程技术研究中心,山东省食品药品安全检测工程技术研究中心,济南250101

出　　处：《分析试验室》2021年第4期416-421,共6页Chinese Journal of Analysis Laboratory

基　　金：山东省重点研发计划(2019YYSP020);食品安全关键技术研发重点专项(2017YFC1601600)项目资助。

摘　　要：建立了小麦粉及其添加剂中非食用物质三聚硫氰酸三钠盐(TMT)的高效液相色谱检测方法。优化了缓冲盐提取体系对TMT的提取,比较了不同色谱条件对TMT及杂质的分离效果。样品中TMT用乙腈-甲酸铵缓冲溶液体系提取,以甲醇-酸化乙酸铵为流动相梯度洗脱,Atlantis T3色谱柱进行分离,二极管阵列检测器检测,外标法定量。结果显示,TMT质量浓度在0.05~10.0μg/mL范围内线性关系良好(R^(2)=0.9997)。方法检出限为0.3 mg/kg,定量限为1.0 mg/kg,加标回收率在90.3%~105.1%之间,相对标准偏差均小于5.1%。通过控制提取条件和色谱分离条件实现了总TMT的测定,克服了酶式面粉处理剂易胶化问题。方法适用于小麦粉及其添加剂中总TMT的快速定性、定量分析。A method for the determination of 2,4,6 trimercaptotriazine trisodium(TMT)in wheat flour and flour treatment agents by high performance liquid chromatography was established.The samples were extracted with80%acetonitrile-formic acid/ammonium formate(p H 2.5).The target compound was separated on a Atlantis T3 column using methanol-acidified ammonium acetate as mobile phase with gradient elution mode,and detected by diode-array detector using external standard method.The calibration curves of TMT showed a satisfactory linearity in the concentration range of 0.05-10.0μg/m L with a correlation coefficient of 0.9997.The limit of detection was 0.3 mg/kg,and the quantitation limit was 1.0 mg/kg.The average recoveries ranged from 90.3%to 105.1%at three spiked levels with the RSDs less than 5.1%.This method is suitable for the detection of total TMT in wheat flour and flour treatment agents.

关 键 词：小麦粉 面粉处理剂 三聚硫氰酸三钠盐(TMT) 高效液相色谱法(HPLC) 

分 类 号：O657.7[理学—分析化学]