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1、高效液相色谱法快速测定葡萄干和葡萄酒中3种糠醛类物质汪辉1,黎瑛2,夏立新1,彭新凯1,李秀娟3,袁靖2(1.长沙市食品质量安全监督检测中心,长沙410013;2.湖南省食品安全生产工程技术研究中心,长沙410013;3.新疆吐鲁番地区质量与计量检测所,吐鲁番838000)摘要:建立高效液相色谱法快速测定葡萄干和葡萄酒中3种糠醛类物质。样品经甲醇-0.02mol/L醋酸铵(用冰醋酸调pH=3.5)(20+80)溶液超声提取后,离心,取上清液过微孔滤膜待分析。分析时流动相A为0.02mol/L醋酸铵(用冰醋酸调pH=3.5),B为甲醇,对目标化合物进行梯度洗
2、脱。流缺少样品提取净化步骤描述速为1.0mL/min,C18色谱柱分离,柱温为40℃,检测波长为285nm。5-羟甲基糠醛、糠醛、5-甲基糠醛在0.7-500mg/L浓度范围内线性良好,方法检出限分别为0.4,0.5,0.3mg/kg,回收率在90.36.8-109%之间,相对标准偏差在4.5925%以下。该方法前处理过程简单,快速、准确,适于同时快速测定葡萄干和葡萄酒中3种糠醛类物质。关键词:高效液相色谱法;葡萄干;葡萄酒;5-羟甲基糠醛;糠醛;5-甲基糠醛中图分类号:文献标志码:文章编号:RapidDeterminationofThreeFurfura
3、lsinRaisinandWinebyHighPerformanceLiquidChromatographyWANGHui1,LIYing2,XIALi-xin1,PENGXin-kai1,LIXiu-juan3,YUANJing2(1.ChangshaCenterofSupervisionandInspectiononFoodQualitySafety,Changsha410013China;2.FoodsafetyproductionEngineeringResearchCenterofHunanProvinceChangsha410013,China
4、;3.XinjiangTurpanareatestinginstituteofqualityandmetrology,Tulufan838000,China)Abstract:Amethodofhighperformanceliquidchromatographywasdevelopedforrapiddeterminationofthreefurfuralsinraisinandwine.Thesampleswereextractedbythesolutionof0.02mol/Lammoniumacetate(pH=3.5)usingultrasoni
5、c,then,centrifuged.Afterfilteredthrough0.45μmfilters,thefiltratewouldbeanalyzedbyhighperformanceliquidchromatography.MobilephaseAwas0.02mol/Lammoniumacetate(pH=3.5)andthemobilephaseBwasmethanolwithcurrentvelocityof1.0mL/min.Undergradientelution,thetargetcompoundswereseparatedbyC18
6、columnat40℃whichweredetectedon285nm.Thecalibrationcurvesshowedgoodlinearityfor5-Hydroxymethylfurfuralhydroxymethylfurfural,furfuraland5-Methylfurfuralmethylfurfuralintherangeof0.7-500mg/L.Thelimitsofdetectionofthreetargetcompoundswere0.4,0.5,0.3mg/kg,respectively.Thespikedrecoveri
7、esrangedfrom90.3%to109%withRSDslessthan4.59%.Thisproposedmethodwassimplepretreatment,rapidandaccuratewhichwassuitablefordeterminationofthreefurfuralsinraisinandwine.Keyword:Highperformanceliquidchromatography;Raisin;Wine;5-Hydroxymethylfurfural;Furfural;5-Methylfurfural收稿日期:2013-0
8、5-17、修订日期:2013-06-16基金项目:湖南省科技计划重