_重要有机污染物痕量与超痕量检测技术_

© 1994-2010 China Academic Journal Electronic Publishing House. All rights reserved. S i m ult aneous D eterm i n a ti on of Acti ve Co m ponen ts and An ti 2d i a beti c

D rugs i n Propolis Hea lth Foods by Ultra Performance L i qu i d

Chroma tography Tande m M a ss Spectrom etry

ZHU M ing 2Da

1,2,3,MA W ei 1,2,CHE N Dong 2Dong 2,PE NG Tao 2,L I Shu 2Juan 2,ZHAO Guang 2Hua 1,T ANG Ying 2Zhang 31,21(College of Food Science &N utritional Engineering,China A gricultural U niversity,B eijing 100083)

2

(Chinese A cade m y of Inspection and Q uarantine,B eijing 100025)3(Inner 2M ongolia Entry 2Exit Inspection and Q uarantine B ureau,Hohhot 011100)

Abstract A comp rehensive analytical method based on ultra perf or mance liquid chr omat ography tande m mass s pectr ometry (UP LC 2MS/MS )was devel oped f or the si m ultaneous deter m inati on of active components and anti 2diabetic drugs in p r opolis health foods .The sa mp les were extracted by ultras ound extracti on with methanol .The ins oluble residue of extract was re moved by freeze 2centrifuging .The analysis was perf or med on an ACQU I TY UP LC C 18column (50mm ×1mm ,i .d .,1.7μm )utilizing a gradient eluti on p r ofile and a mobile phase of 0.3%for m ic acid in water and acet onitrile .The analytes were detected using an electr o s p ray i onizati on tande m mass s pectr ometry with multi p le reacti on monit oring .Qualitative and quantitative analysis was based on the peak area of the parent i on and t w o frag ment i ons .The LOD and LOQ level f or 14active components ranged fr om 0.7mg/kg t o 42.0mg/kg and 2.2mg/kg t o 140mg/kg res pectively,and recoveries were 7718%-11316%,with the intra 2and inter 2day p recisi on less than 15%.The LOD and LOQ level f or 9anti 2diabetics ranged fr om 0.1mg/kg t o 0.9mg/kg and 0.3mg/kg t o 2.5mg/kg res pectively,and recoveries were 79.3%-108.5%,with the intra 2and inter 2day p recisi on less than 15%.The method is si m p le and sensitive,and can be used f or quality contr ol of p r opolis .

Keywords U ltra perf or mance liquid chr omat ography tande m mass s pectr ometry;

Pr opolis;Active

compounds;Anti 2diabetic drugs

(Received 22July 2009;accep ted 9November 2009)《重要有机污染物痕量与超痕量检测技术》

全书分为:第一篇重要技术进展概论,第二篇持久性有机污染物,第三篇食品中致癌物,第四篇食品中有机金属化合物的检测技术,第五篇其他重要有机污染物(共二十三章)。该书全面总结了我国科技部“九五食品安全关键技术”课题、“十五”的“食品安全关键技术研究”等国家攻关计划的重大项目的研究成果。重点介绍了色质谱联用中的选择性离子监测、高分辨质谱、液相色谱串联质谱、离子阱串联质谱和等离子诱导发射质谱等新技术进展,所涉及的重要有机污染物不仅包括持久性有机污染物公约规定的二噁英、多氯联苯、有机氯农药等,也包括氯丙醇、丙烯酰胺、多环芳烃、杂环胺和亚硝胺等重要致癌物和有机锡、有机汞、有机砷和有机硒等元素有机形态,还包括了溴代二噁英、多氯联苯醚、多氯萘、全氟有机化合物、烷基酚、酞酸酯等可能列入持久性有机污染物公约的“新二噁英”环境内分泌干扰物。从其健康效应风险评估与控制标准入手,在重点介绍前样品处理和仪器检测金属进展的基础上,以应用实例对检测技术予以详细介绍。

该书内容全面,综合性强,是从事食品安全监督检验人员的重要参考书,对于环境和农业领域的研究人员也有重要参考价值,可供高等院校与相关专业师生作参考。

该书由吴永宁(中国疾病预防控制中心营养与食品安全所)和江桂斌(中国科学院生态环境研究中心)主编,化学工业出版社出版,定价85.00元。

471 分析化学第38卷