SN-T 0605-2012出口糧谷中雙苯唑菌醇?xì)埩袅繖z測(cè)方法液相色譜-質(zhì)譜質(zhì)譜法

中華人民共和國(guó)出入境檢驗(yàn)檢疫行業(yè)標(biāo)準(zhǔn)出口糧谷中雙苯唑菌醇?xì)埩袅繖z測(cè)方法液相色譜-質(zhì)譜/質(zhì)譜法2012-05-07發(fā)布2012-11-16實(shí)施I—更改了標(biāo)準(zhǔn)名稱；—修改了前處理方法。出口糧谷中雙苯唑菌醇?xì)埩袅繖z測(cè)方法本標(biāo)準(zhǔn)規(guī)定了出口糧谷中雙苯唑菌醇?xì)埩袅康臏y(cè)定方法。下列文件對(duì)于本文件的應(yīng)用是必不可少的。凡是注日期的引用文件，僅注日期的版本適用于本文分析實(shí)驗(yàn)室用水規(guī)格和試驗(yàn)方法度≥98.0%。準(zhǔn)儲(chǔ)備溶液。該溶液在一18℃冰箱中保存有效期為12個(gè)月。成適當(dāng)濃度的混合標(biāo)準(zhǔn)工作溶液。低于4℃避光冷藏保存，現(xiàn)用現(xiàn)配。12將試樣于-5℃以下避光保存。在抽樣及制樣的操作過(guò)程中，應(yīng)防止樣品受到污染或發(fā)生殘留物7分析步驟上混合2min,在3000r/min下離心5min。將上清液轉(zhuǎn)移至具刻度玻璃試管，并用乙腈定容至試管中。于40℃下氮吹至近干；加入4mL水-乙腈(9+1,體積比3時(shí)間/min0.1%甲酸溶液/%090.090.090.090.090.090.0按照液相色譜-質(zhì)譜/質(zhì)譜條件測(cè)定樣品和標(biāo)準(zhǔn)工作溶液，樣品的質(zhì)量色譜峰保留時(shí)間與標(biāo)準(zhǔn)品中對(duì)應(yīng)的保留時(shí)間一致；且樣品中各組分定性離子的相對(duì)豐度與接近濃度的標(biāo)準(zhǔn)工作溶液中相應(yīng)的定性相對(duì)離子豐度/%士20件下雙苯唑菌醇的參考保留時(shí)間約為4.45min,雙苯唑菌醇標(biāo)準(zhǔn)品多反應(yīng)檢測(cè)(MRM)色譜圖參4樣品名稱添加濃度/(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大麥0.02582.0～101.20.05077.2～92.00.10073.8～86.4小麥0.02576.0～100.40.05075.8~95.80.10073.4～92.45表3(續(xù))樣品名稱添加濃度/(mg/kg)回收率范圍/%蕎麥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燕麥78.0～100.080.2～91.673.4～98.26參考條件!)j)△EMV:400V;名稱母離子電荷狀態(tài)源內(nèi)碎裂電壓/V定性離子對(duì)駐留時(shí)間/ms定量離子對(duì)雙苯唑菌醇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(CASN4.10Standardstocksolutio4.12Workingstandardsolutionswithsastandardstosampleblankmatrixblankforpreparationofcalibarationcurve4.13NH?SPEcolum4.14Membranefilter: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