固相萃取-高效液相色谱法同时测定噻菌灵和多菌灵在浓缩菠萝汁中的残留量  

Simultaneous Determination of Thiabendazole and Carbendazim Residues in Concentrated Pineapple Juice by Solid Phase Extraction and High Performance Liquid Chromatography

作　　者：刘晓松[1] 童张法[2] 郑玲 卓海华[3] 刘军义 

机构地区：[1]广西出入境检验检疫局技术中心,南宁530021 [2]广西大学化学化工学院,南宁530004 [3]海南出入境检验检疫局技术中心,海口570105

出　　处：《分析科学学报》2007年第3期311-314,共4页Journal of Analytical Science

基　　金：国家质检总局制标项目(No:B105-2003)

摘　　要：建立了一种可同时测定浓缩菠萝汁中噻菌灵和多菌灵残留量的反相高效液相色谱分析法.浓缩菠萝汁样品与水按一定比例稀释后,经过调节溶液的pH值、离心、过滤,用混合相固相萃取小柱（Mixed-mode SPE）进行提取、净化,并用配有二极管阵列检测器（DAD）的液相色谱仪检测,外标法定量.使用噻菌灵和多菌灵对照品进行添加回收率测定,结果显示,本方法对噻菌灵的检出限为0.020 mg/kg,回收率为75.7%～93.3%;对多菌灵的检出限为0.020 mg/kg,回收率为80.8%～99.2%;测定的相对标准偏差均不大于5.7%.本方法简单、快速、准确,能满足常规噻菌灵和多菌灵残留量检测的需要.A solid phase extraction（SPE）-high performance liquid chromatographic （HPLC） method was developed for the simultaneous analysis of thiabendazole and carbendazim residues in concentrated pineapple juice. The samples were first diluted with distilled water, and was then centrifuged and filterd. The pre-treated samples were passed through Mixed-mode SPE column for extraction and cleaning up. Keeping the elution rate at 3. 0 mL/min, the compounds were thus isolated from the sample and concentrated. Finally, the determination was carried out by HPLC, the compounds was identified with the ultraviolet spectrum and compared with that of thiabendazole and carbendazim standards by diode array detector （DAD）. External standard method was adopted for residues quantification. The results showed that the recoveries were 75. 7%-3. 3% for thiabendazole and 80. 8%-99. 2% for carbendazim, the detection limit was 0. 020 mg/kg for both, and the RSD was generally below 5.7%. The method is simple, fast and applicable for routine analysis.

关 键 词：高效液相色谱法 浓缩菠萝汁 固相萃取 噻菌灵 多菌灵 残留量 

分 类 号：O657.72[理学—分析化学]