高效液相色谱法测定饲料中甲硝唑、地美硝唑和异丙硝唑-论文.pdf

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1、南京农业大学学报2014，37(5)：123-127http：／／naaxb．njau．edu．cnJournalofNanjingAgriculturalUniversitydoi：10．7685／j．issn．1000—2030．2014．05．020王延映，彭麟，余祖功，等．高效液相色谱法测定饲料中甲硝唑、地美硝唑和异丙硝唑[J]．南京农业大学学报，2014，37(5)：123—127高效液相色谱法测定饲料中甲硝唑、地美硝唑和异丙硝唑王延映，彭麟，余祖功(南京农业大学动物医学院，江苏南京210095)摘要：为建立能同时检测饲料中甲硝唑、地美硝唑和异丙硝唑的简便、准确的高效液相色

2、谱方法，样品用乙酸乙酯提取、MCX固相萃取柱净化、ZORBAXSB—C8柱(4．6ram~250mm，5m)分离，以甲醇一水为流动相，梯度洗脱，320nm紫外检测，外标法定量。结果表明：此条件下，3种药物分离良好，标准曲线回归系数为0．9997-0．9998，线性范围0．02～1OIxg。mL一；平均回收率75．3％106-3％，批内变异系数1．3％一12．4％，批问变异系数2．4％～9．7％，甲硝唑、地美硝唑和异丙硝唑检测限均为O．O1mg·kg～，定量限为0．02mg·kg一。结论：该法操作简单、结果准确，可用于测定饲料中甲硝唑、地美硝唑和异丙硝唑的含量。关键词：甲硝唑；地美硝唑

3、；异丙硝唑；饲料；高效液相色谱法中图分类号：$859．7文献标志码：A文章编号：1000—2030(2014)05—0123—05Determinationofmetronidazole，dimetridazoleandipronidazoleinfeedsbyHPLCWANGYanying，PENGLin，YUZugong(CollegeofVeterinaryMedicine，NanjingAgriculturalUniversity，Nanjing210095，China)Abstract：Thepurposeofthisstudywastodevelopasimpleande

4、ffectivemethodthatoptimizedthehigh-performanceliquidchroma·-tography(HPLC)methodfordeterminationofmetronidazole，dimetridazoleandipronidazoleinfeedsbyinvestigatingtheextractionandclean—upconditions．Sampleswereweighedinto50mLpolypropylenecentrifugetubesandextractedbymechanicalshakingfor30minwith1

5、5mLethy1acetate．Afterextraction．thecontentwascentrifugedat6000r·min～for10minandtheextractwastrans—ferredtoanewpolypropylenecentrifugetube．Theunsolvedfeedmatrixwasextractedagainbyadding15mLethylacetateandtheextractwascollected．Bothobtainedethylacetateextractionswerecombinedandevaporatedjusttodry

6、nesswithapressureblowingconcentrator(waterbathat35oC)．Theresiduewasdissolvedin300IxLethylacetateand4mLhexaneandthesolutionwastrans．ferredtoa10mLpolypropylenecentrifugetubefirst．Then1．5mLphosphoricacidsolution(0．1mol·L)wasaddedintothetube．Aftervortexing(1min)andcentrifuging(10min，8000r·min)，thel

7、oweraqueousphasewascollectedina5mLpolypropylenecentrifugetube．Thesupernatantorganicphasewasextractedagainbyadding1．5mLphosphoricacidsolution(0．1tool·L)andboththeobtainedloweraqueousphaseswerecombined．Theobtainedsolutionwaspurified