进出口食品中三唑醇残留量的检测方法 气相色谱-质谱法

进出口食品中三唑醇残留量的检测方法气相色谱-质谱法24.7振荡器。5试样制备与保存5.1试样制备5.1.1荷兰豆、什锦蔬菜和橙取代表性样品500g,将其可食用部分切碎后(不可用水洗涤),依次用捣碎机将样品加工成浆状。混匀，均分成两份作为试样，分装入容器内，密闭并标明标记。5.1.2乌龙茶、木薯干、大米和大豆取代表性样品500g,用粉碎机粉碎并通过2.0mm圆孔筛。混匀，分装入容器内，密闭并标明标记。5.1.3牛肉、鲷鱼或龙虾仁取代表性样品500g,将其切碎后，依次用绞碎机将样品绞碎，混匀，分装入容器内，密封并标明标记。5.1.4蜂王浆和蜂蜜取有代表性样品量500g.对无结品的蜂蜜样品将其搅拌均匀；对有结品析出的蜂蜜样品，在密闭情况下，将样品瓶置于不超过60℃的水溶中温热，振荡，待样品全部融化后搅匀，迅速冷却至室温，在融化时应注意防止水分挥发。制备好的试样均分成两份，分别装入样品瓶中，密封，并标明标记。5.2试样的保存大豆、木薯干、乌龙茶、大米、蜂蜜等试样于0℃~4℃保存；荷兰豆、什锦蔬菜、橙、牛肉、鲷鱼、龙虾仁和蜂王浆等试样于一18℃以下冷冻保存。在制样的操作过程中，应防止样品受到污染或发生残留物含量的变化。6测定步骤6.1.1大豆、木薯干、牛肉、鲷鱼、龙虾仁和蜂王浆等试样称取5g试样(精确至0.01g)。6.1.2荷兰豆、什锦蔬菜和橙等试样称取10g试样(精确至0,01g)。6.1.3米、茶叶和蜂蜜等试样称取5g试样(精确至0.01g),并加入4mL水，混匀.浸泡或溶解。茶叶需浸泡30min。将称取的样品置于250mL的具塞锥形瓶中，加入50ml.提取溶剂(3.7),加入15g无水硫酸镁(3,5)和6g无水醋酸钠(3.6),振荡提取40min(牛肉、蜗鱼、龙虾仁等肉制品应均质提取5min),过滤于150mL浓缩瓶中。再加人20ml.提取溶剂(3.7)重复提取一次，合并提取液，40℃下旋转浓缩至干。用2mL.乙腈溶解残渣，待净化。6.3固相分散萃取净化6.3.1荷兰豆、什锦蔬菜、橙、乌龙茶和木薯干提取液将6.1相应样品提取液转移到事先装有50mgPSA填料和200mg石墨化碳黑填料的小试管中，充分涡旋1min,待色素完全消除后，过滤膜，供气相色谱-质谱测定和确证。将6.1相应样品提取液转移到事先装有100mgPSA填料，50mg石墨化碳黑填料和100mgC,填料的小试管中，充分涡旋1min,过滤膜，供气相色谱-质谱测定和确证。37.41min,其监测离子(m/z)丰度比为295:297:127:238=100:35:27:6对其进行确证：根据定 本方法各种基质的测定低限均为0.005mg/kg。不同基质中添加浓度水平下的回收率范围见表2,桩66.4～76.Thisstandardspecifiespreparationoftestsample,determinationandconfirmationofresicuebygaschromatography-negativecthemicalionizationmassThisstandardisapplicabletothedeterminationandsuchassnowpea,assortedseasonalvegetables.orange,bean.drypotatsnoutcatfish,royeljelly,redswampcrayfishandbeTriadimenolresidueisextractedwithacetonitrilecoiquidpartitioningformedbyaddinganhydrousmagnessimplecleanupstepknownbydispersifirmedbygaschromatography-negativechemicalionizationmassUnlessotherwisespecified,allthereagentsusedswater.3.1Acetonitrile;HPL3.7Acetonitrile(saturedbyn-hexane)containing3.8Triadimenol(CuHeCIN,O₂,CASNo:55219-65-3),purit3.9Triadimenolstandardstocksolstandard,dissolveinasmallvolumeofacetonitrile.Dilusolutionof200rg/mLinconcen3.10Triadimenolstandardworkingsolution;Thendilutethestandardstocksolutiotriletotherequiredconcantrationasthestandardworki3.12Bondesil-PSA(Primar4Apparatusandequipm4.1Gaschromotograph/msssspectrometry(MSD)equippedwithnegativ4.4Tissuetriturator.5.1.1Vegetablesorfruits.suchassnowpea,asSarteAbout500grepresentativesamplesshouldbetakenfromthepulpintotwoequalportions.5.1.2Teaorcereals,suAbout500grepresentativesamplesshouldbetakenfromallthenpassedthroughameshtwoportions.Eachportionisputi5.1.3MeatsandmeatproAbout500grepresentativesamplestwoequalportion.Eachportion5.1.4Beeproducts,suchasroyeljellyaAbout500grepresentativesamcrystallizedshallbestirredwalltomakewarmedinawater-bathbelow60Cwiththesasamplehasmelted.thencoolimmediaprecautionsmustbetakentoavoidevaporationtwoequalportions.EachportionThetestsamplesoftea,beeproducts,plesoffreshfruits,vegetablInthecourseofsamplingandsamplepreparation.precauanyfactorswhichmaycausethechangeofres6.1.1bean,drypotato,beef,longsnoutcatfish,redswampcrayWeighca5gofthetestsample(accu