节点文献

食品中苯并咪唑类农药残留的液相色谱—质谱/质谱法(HPLC-MS/MS)分析研究

Determination of Benzimidazoles Residues in Foodstuffs by HPLC-MS/MS

【作者】 王冰

【导师】 熊何健; 徐敦明;

【作者基本信息】 集美大学 , 食品加工与安全, 2010, 硕士

【摘要】 本研究建立了同时测定基质中多菌灵、噻菌灵、麦穗宁、硫菌灵、甲基硫菌灵和烯菌灵残留的液相色谱-质谱/质谱(HPLC-MS/MS)的分析方法。在国内外研究的基础上,通过实验对前处理的提取、净化条件进行了优化,由实验结果表明:采用乙腈提取,PSA-C18-石墨化炭黑粉净化,提取净化的效果最好。在本研究的色谱条件下,多菌灵、噻菌灵、麦穗宁、硫菌灵、甲基硫菌灵和烯菌灵在0.2μg/mL~10μg/mL间呈现良好的线性关系,相关系数≥0.9990。经过实验确定了液相色谱-质谱/质谱(HPLC-MS/MS)法中多菌灵、噻菌灵、麦穗宁、硫菌灵、甲基硫菌灵和烯菌灵的检出限为5μg/kg。在大米、小麦、猪肉、猪肝、牛奶、柑橘、苹果、土豆、核桃仁、菠菜和茶叶基体中进行添加回收实验,添加浓度在5~25μg/kg间,回收率为61.6%~104.8%,变异系数为6.0%~14.4%。本方法的测定低限可达5mg/kg,完全能满足当前各国的残留限量要求。检测本方法前处理过程简便,灵敏度高,定量结果准确,适用于食品中苯并咪唑类农药残留量的检测。外拓性强(可根据要求,增加检测农药品种),值得在进出口食品检测中推广使用。

【Abstract】 One-step extraction and high performance liquid chromatography(HPLC)-MS/MS have been developed and validated for the determination of 6 kinds of benzimidazoles (Carbendazim, Thiabendazole, Fuberidazole, Thiophanate, Thiophanate methyl, and Imazalil)residues in food matrices including rice, corn ,bean, orange, apple, potato, spinach, fish, pork, pig liver, milk, graph, and tea.The extraction efficiency of ethyl acetate and acetonitrile,different cleanup methods including Cl8 solid phase extraction(SPE)cartridge , hydrophilic—lipophilic balance(HLB)SPE cartridge,activated carbon,florisil and Vario GPC and separation by HPLC are extensively investigated.The extraction recoveries of the seven kinds of benzimidazoles are between 61.6% and 104.8% for spiked level of 5-25μg/kg.The limits of quantification are 0.005 mg/kg for the 6 pesticides(S/N=1 0).There are good linear correlations between the peak areas and concentrations of the seven kinds of benzimidazoles,the line arrange is 0.2—10μg/mL and the correlation coefficients are above 0.999.

【关键词】 HPLC-MS/MS苯并咪唑类农药残留固相萃取
【Key words】 HPLC-MS/MSbenzimidazolesfoodstuffresidueLOQ
  • 【网络出版投稿人】 集美大学
  • 【网络出版年期】2012年 02期
  • 【分类号】TS207.53;O657.63
  • 【被引频次】1
  • 【下载频次】223
节点文献中: