SN-T 0605-2012出口粮谷中双苯唑菌醇残留量检测方法液相色谱-质谱质谱法

中华人民共和国出入境检验检疫行业标准出口粮谷中双苯唑菌醇残留量检测方法液相色谱-质谱/质谱法2012-05-07发布2012-11-16实施I—更改了标准名称；—修改了前处理方法。出口粮谷中双苯唑菌醇残留量检测方法本标准规定了出口粮谷中双苯唑菌醇残留量的测定方法。下列文件对于本文件的应用是必不可少的。凡是注日期的引用文件，仅注日期的版本适用于本文分析实验室用水规格和试验方法度≥98.0%。准储备溶液。该溶液在一18℃冰箱中保存有效期为12个月。成适当浓度的混合标准工作溶液。低于4℃避光冷藏保存，现用现配。12将试样于-5℃以下避光保存。在抽样及制样的操作过程中，应防止样品受到污染或发生残留物7分析步骤上混合2min,在3000r/min下离心5min。将上清液转移至具刻度玻璃试管，并用乙腈定容至试管中。于40℃下氮吹至近干；加入4mL水-乙腈(9+1,体积比3时间/min0.1%甲酸溶液/%090.090.090.090.090.090.0按照液相色谱-质谱/质谱条件测定样品和标准工作溶液，样品的质量色谱峰保留时间与标准品中对应的保留时间一致；且样品中各组分定性离子的相对丰度与接近浓度的标准工作溶液中相应的定性相对离子丰度/%士20件下双苯唑菌醇的参考保留时间约为4.45min,双苯唑菌醇标准品多反应检测(MRM)色谱图参4样品名称添加浓度/(mg/kg)糙米76.0～99.20.05073.4～92.685.2～98.2玉米72.0～97.675.6～98.80.10073.6～98.2大麦0.02582.0～101.20.05077.2～92.00.10073.8～86.4小麦0.02576.0～100.40.05075.8~95.80.10073.4～92.45表3(续)样品名称添加浓度/(mg/kg)回收率范围/%荞麦78.0～100.073.6～93.0大米78.0-~98.073.2～98.8高梁76.0～102.40.05074.0～94.8燕麦78.0～100.080.2～91.673.4～98.26参考条件!)j)△EMV:400V;名称母离子电荷状态源内碎裂电压/V定性离子对驻留时间/ms定量离子对双苯唑菌醇517b)8ThestandardisdraftedaccordingtoGB/T1.1—2009principleforexport.—Thesamplingprocessureisommited—ThemethodischangedtoLC-MS/MS—Thecleanupprocessureisimproved.ThisstandardwasproposePeople'sRepublicofChina.ThemaindraftersofthisstandardareYiXionghai,YangHuiain.G—SN0605—1996.9brownrice,corm,barley,wheat,buckwheat,rico,broomcornandoatfdrexportThefollowingdocumen4.3Acetone:HPLCgrade.SN/T0605—20124.4Sodiumhydroxide.4.5Anhydrousmagnesiumsulfate4.7Water:Acetonitrile(9+1,V/V)4.9Standards:Bitertanol(CASN4.10Standardstocksolutio4.12Workingstandardsolutionswithsastandardstosampleblankmatrixblankforpreparationofcalibarationcurve4.13NH₂SPEcolum4.14Membranefilter:0.22μm,organicphase5.1Liquidchromatograph5.3Homogenizer.5.6Vortexmixer6.1PreparationoftestsampleBrownrice,corn,barley,wheat,buckwheat,riavoidcontaminationoranyfactorsthatmaychangeresidueclonsource:ESl.Scanningmodel:positiveion.ReferencedconditionsseenannexATime/min0.1%Fomicacid/%Acetonitrile/%0relativeintensity/%permittedtolerances/%士30Accordingtotheapproximateconcentration~ofanalYteinsampfesolution,sUndergoaccordingtotheaboveproceduresexcludingthesample.XX-theresiduecontentofTheresultofcalculationshouldbedeductedwithblankvalue.is0.025mg/kg.Fortifiedcontent/(mg/kg)Recoveryrange/%brownrice0.02576.0～99.20.05073.4～92.60.10085.2～98.20.02572.0～97.60.05075.6～98.80.10073.6～98.2barley0.02582.0～101.20.05077.2～92.00.10073.8~86.4wheat0.02576.0～100.40.05075.8～95.80.10073.4～92.4buckwheat0.02578.0～100.00.05073.6～93.00.10075.4～97.6rice0.02578.0～98.00.05074.0～96.20.10073.2～98.8broomcorn0.02576.0～102.40.05073.4～98.20.10074.0～94.80.02578.0～100.00.05080.2～91.60.10073.4～98.2ReferencedconditionsbyLC-MS/MS:j)△EMV:400V;(m/z)andTransitonsforquantititation(m/z),seetableA.1.precursorFragementor/VBitertanol511)Non-commercials