SN∕T 5365-2022 出口植物源性食品中氟唑磺隆和氟吡磺隆殘留量的測定 液相色譜-質(zhì)譜∕質(zhì)譜法

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ICS67.040CCSC53中華人民共和國出入境檢驗(yàn)檢疫行業(yè)標(biāo)準(zhǔn)SN/T5365—2022出口植物源性食品中氟唑磺隆和氟吡磺隆殘留量的測定液相色譜-質(zhì)譜/質(zhì)譜法Determinationofflucarbazone-sodiumandflucetosulfuronresiduesinfoodstuffsofplantoriginforexport—LC-MS/MSmethod2022-03-14發(fā)布2022-10-01實(shí)施中華人民共和國海關(guān)總署發(fā)布

1SN/T5365—2022前言本文件按照GB/T1.1—2020《標(biāo)準(zhǔn)化工作導(dǎo)則第1部分:標(biāo)準(zhǔn)化文件的結(jié)構(gòu)和起草規(guī)則》的規(guī)定起草。本文件由中華人民共和國海關(guān)總署提出并歸口。本文件起草單位:中華人民共和國伊寧海關(guān)技術(shù)中心、伊犁師范大學(xué)、中華人民共和國天津海關(guān)工業(yè)產(chǎn)品安全技術(shù)中心、中華人民共和國成都海關(guān)技術(shù)中心、中華人民共和國天津海關(guān)動植物與食品檢測中心。本文件主要起草人:李芳、粟有志、馮新忠、徐穎潔、王興磊、周磊、劉俊、肖亞兵、雷紅琴、李艷美、羅瓊、袁小雯、尚爽、周均、陸平。Ⅰ

2SN/T5365—2022出口植物源性食品中氟唑磺隆和氟吡磺隆殘留量的測定液相色譜-質(zhì)譜/質(zhì)譜法1范圍本文件規(guī)定了出口植物源性食品中氟唑磺隆和氟吡磺隆殘留量的液相色譜-質(zhì)譜/質(zhì)譜測定方法。本文件適用于菠菜、芹菜、土豆、西紅柿、蘋果、桃子、葡萄、糙米、小麥、核桃、大米等植物源性食品中氟唑磺隆和氟吡磺隆殘留量的檢測和確證。2規(guī)范性引用文件下列文件中的內(nèi)容通過文中的規(guī)范性引用而構(gòu)成本文件必不可少的條款。其中,注日期的引用文件,僅該日期對應(yīng)的版本適用于本文件;不注日期的引用文件,其最新版本(包括所有的修改單)適用于本文件。GB2763—2019食品安全國家標(biāo)準(zhǔn)食品中農(nóng)藥最大殘留限量GB/T6682分析實(shí)驗(yàn)室用水規(guī)格和試驗(yàn)方法3術(shù)語和定義本文件沒有需要界定的術(shù)語和定義。4方法提要樣品經(jīng)乙腈-甲苯(90+10)(v/v)提取、分散固相萃取凈化后,液相色譜-質(zhì)譜/質(zhì)譜檢測,外標(biāo)法定量。5試劑和材料除另有規(guī)定外,所用試劑均為分析純,水為符合GB/T6682規(guī)定的一級水。5.1乙腈:色譜純。5.2乙酸銨:優(yōu)級純。5.3甲酸:優(yōu)級純。5.4甲苯:優(yōu)級純。5.5氯化鈉。5.60.1%甲酸-5mmol/L乙酸銨水溶液:準(zhǔn)確移取1.0mL甲酸(5.3),用水定容至1000mL;準(zhǔn)確稱取0.375g乙酸銨(5.2),加入至定容液中,混勻。5.7乙腈-甲苯(90+10)(v/v):取甲苯(5.4)100mL,用乙腈(5.1)定容至1000mL,混勻。,有機(jī)系。5.8濾膜:0.22μm。5.9十八烷基硅膠填料(C18填料):40μm5.10石墨化碳黑(GCB):120mesh~400mesh。1

3SN/T5365—20225.11氟唑磺隆標(biāo)準(zhǔn)物質(zhì):CAS號145026-88-6。5.12氟吡磺隆標(biāo)準(zhǔn)物質(zhì):CAS號412928-75-7。5.13標(biāo)準(zhǔn)儲備溶液:準(zhǔn)確稱取10mg(精確至0.1mg)氟唑磺隆標(biāo)準(zhǔn)物質(zhì)(5.11)和氟吡磺隆標(biāo)準(zhǔn)物質(zhì)(5.12),用乙腈分別配制成1/mL的標(biāo)準(zhǔn)儲備液,避光4000μg℃保存,有效期6個(gè)月。/mL5.14中間混合標(biāo)準(zhǔn)溶液:分別吸取適量的標(biāo)準(zhǔn)儲備液(5.13),用乙腈稀釋,配置濃度均為10μg的中間混合標(biāo)準(zhǔn)溶液,避光4℃保存,有效期2個(gè)月。5.15基質(zhì)空白溶液:將不同基質(zhì)的陰性空白樣品,按照8.1提取和8.2凈化后,得到基質(zhì)空白溶液。5.16基質(zhì)匹配工作溶液:根據(jù)需要用基質(zhì)空白溶液(5.15)稀釋中間混合標(biāo)準(zhǔn)溶液(5.14)至合適濃度的基質(zhì)匹配工作溶液,現(xiàn)配現(xiàn)用。6儀器和設(shè)備6.1液相色譜-質(zhì)譜/質(zhì)譜儀:配有電噴霧離子源(ESI)。6.2分析天平:感量分別為0.1mg和0.01g。6.3組織搗碎機(jī)。6.4振蕩器。6.5離心機(jī):8000r/min。6.6離心管:50mL和2mL。6.7渦旋器。7試樣制備與保存蔬菜、水果的取樣部位按照GB2763—2019的規(guī)定執(zhí)行,取樣品500g,用組織搗碎機(jī)均質(zhì),充分混勻,均分為2份,裝入潔凈的容器,密封并標(biāo)明標(biāo)記,于-18℃以下冷凍保存。堅(jiān)果樣品去殼取全果500g,用組織搗碎機(jī)均質(zhì),充分混勻,均分為2份,裝入潔凈的容器,密封并標(biāo)明標(biāo)記,于0℃~4℃條件下保存。谷物類樣品取代表性試驗(yàn)500,均分為2份,裝入潔g,粉碎后使其全部可通過425μm的標(biāo)準(zhǔn)網(wǎng)篩凈的容器,密封并標(biāo)明標(biāo)記,于0℃~4℃條件下保存。8測定步驟8.1提取8.1.1蔬菜、水果稱取5g試樣(精確至0.01g)于50mL離心管中,加入5mL水渦旋30s,加入10mL乙腈-甲苯(90+10)(v/v),水平振蕩20min,加入4g氯化鈉(5.5),水平振蕩5min,8000r/min離心5min,取上清液1.0mL于2mL離心管,待凈化。8.1.2谷物、堅(jiān)果稱取2.5g試樣(精確至0.01g)于50mL離心管中,加入7mL水渦旋30s,加入10mL乙腈-甲苯(90+10)(v/v),水平振蕩20,8min,加入4g氯化鈉(5.5),水平振蕩5min000r/min離心5min,取上清液1.0mL于2mL離心管,待凈化。2

4SN/T5365—20228.2凈化蔬菜、水果的待凈化上清液中加入C填料(5.9)5018mg、石墨化碳黑GCB(5.10)30mg,渦旋30s,,濾液待測。8000r/min離心2min,上清液過0.22μm濾膜谷物、堅(jiān)果的待凈化上清液中加入C填料(5.9)1850mg,渦旋30s,8000r/min離心2min,上清液過0.22,濾液待測。μm濾膜8.3測定8.3.1液相色譜條件液相色譜參考條件如下:;a)色譜柱:C18柱,2.1mm×100mm,3μm或相當(dāng)b)流動相A:0.1%甲酸-5mmol/L乙酸銨水溶液(5.6);流動相B:乙腈;洗脫梯度見表1;c)柱溫:30℃;。d)進(jìn)樣體積:10μL表1流動相及梯度洗脫條件時(shí)間/min流速/(μL/min)流動相A/%流動相B/%0.0025090.010.01.0025090.010.01.5025050.050.05.5025010.090.05.6025090.010.010.0025090.010.08.3.2質(zhì)譜條件質(zhì)譜參考條件如下:a)電離方式:電噴霧電離(ESI);b)干燥氣溫度:300℃;c)干燥氣流量:9.0L/min;d)鞘氣溫度:250℃;e)鞘氣流速:11.0L/min;f)毛細(xì)管電壓:4kV;g)掃描方式:正離子掃描。定性離子對、定量離子對、碰撞能量、碎裂電壓等條件見表2。3

5SN/T5365—2022表2化合物定性離子對、定量離子對、碰撞能量、碎裂電壓、保留時(shí)間序號化合物保留時(shí)間/min定性離子/(m/z)碎裂電壓/V碰撞能量/eV*;397.1/115.08010;581氟唑磺隆4.69397.1/130.0*;488.5/273.012014;182氟吡磺隆5.69488.5/156.0注:帶“*”為定量離子對。8.4定性測定按照上述條件測定樣品和混合基質(zhì)標(biāo)準(zhǔn)工作溶液,如果待測樣品中化合物色譜峰的保留時(shí)間與標(biāo)準(zhǔn)溶液相比變化范圍應(yīng)在±2.5%之內(nèi),定性離子均出現(xiàn)且信噪比大于等于3,定性離子對的相對豐度與濃度相當(dāng)混合基質(zhì)標(biāo)準(zhǔn)工作液的相對豐度一致,相對豐度偏差不超過表3的規(guī)定,可判斷樣品中存在相應(yīng)的被測物。表3定性時(shí)相對離子豐度的最大允許范圍相對離子豐度/%>50>20~5010~20≤10允許的相對偏/%±20±25±30508.5定量測定根據(jù)試樣中被測物的含量,選擇濃度相近的基質(zhì)匹配工作溶液,待測物的響應(yīng)值在儀器檢測的線性范圍內(nèi),如果待測物含量超過標(biāo)準(zhǔn)曲線范圍,應(yīng)用基質(zhì)空白溶液稀釋到合適濃度后分析。在上述儀器條件下,氟唑磺隆和氟吡磺隆的多重反應(yīng)監(jiān)測色譜圖參見附錄A中圖A.1~圖A.2,保留時(shí)間亦可參照附錄A中圖A.1~圖A.2。8.6空白試驗(yàn)除不稱取試樣外,均按上述步驟操作。9結(jié)果計(jì)算和表述試樣中氟唑磺隆和氟吡磺隆的殘留量按式(1)計(jì)算,計(jì)算結(jié)果需扣除空白值。c×V1000X=×…………………………(1)m1000式中:X———試樣中被測物的含量,單位為微克每千克(μg/kg);c———待測組分相應(yīng)值在標(biāo)準(zhǔn)曲線上計(jì)算得到的濃度,單位為納克每毫升(ng/mL);V———提取液的體積,單位為毫升(mL);m———樣品稱樣量,單位為克(g);1000———換算系數(shù)。計(jì)算結(jié)果保留兩位有效數(shù)字。4

6SN/T5365—202210定量限本方法氟唑磺隆和氟吡磺隆的定量限均為5.0/kg。μg11回收率和精密度本方法對波菜、芹菜、土豆、西紅柿、蘋果、桃子、葡萄、糙米、小麥、核桃、大米等基質(zhì)進(jìn)行添加回收率試驗(yàn),不同添加濃度范圍內(nèi)氟唑磺隆和氟吡磺隆的回收率資料參見附錄B。5

7SN/T5365—2022附錄A(資料性)氟唑磺隆和氟吡磺隆標(biāo)準(zhǔn)溶液的多反應(yīng)監(jiān)測(MRM)色譜圖氟唑磺隆和氟吡磺隆標(biāo)準(zhǔn)溶液的多反應(yīng)監(jiān)測(MRM)色譜圖見圖A.1~圖A.2。圖A.1氟唑磺隆標(biāo)準(zhǔn)溶液(10ng/mL)的反應(yīng)監(jiān)測(MRM)色譜圖圖A.2氟吡磺隆標(biāo)準(zhǔn)溶液(10ng/mL)的反應(yīng)監(jiān)測(MRM)色譜圖6

8SN/T5365—2022附錄B(資料性)添加回收率匯總表氟唑磺隆和氟吡磺隆在波菜、芹菜、土豆、西紅柿、蘋果、桃子、葡萄、糙米、小麥、核桃、大米中的添加水平、平均回收率和相對標(biāo)準(zhǔn)偏差(RSD)參見表B.1。表B.111種基質(zhì)中氟唑磺隆和氟吡磺隆的添加水平、平均回收率和相對標(biāo)準(zhǔn)偏差(RSD)(n=6)氟唑磺隆氟吡磺隆基質(zhì)加標(biāo)量平均回收率RSD加標(biāo)量平均回收率RSD種類μg/kg%%μg/kg%%583.809.6581.576.61091.396.61082.303.6菠菜2095.625.720103.4813.010096.043.310098.988.2582.5310.1592.7312.110103.189.810100.1513.1芹菜20100.625.82098.5511.610093.1111.210094.7811.7589.079.5589.9711.31093.479.01096.227.9土豆2098.507.22087.9711.2100101.1812.910097.216.6592.9312.9588.7311.510104.383.51090.029.8西紅柿20102.145.32088.255.9100107.004.310091.846.4587.4313.2584.5010.010114.153.81089.159.5蘋果20103.997.12089.706.3100110.002.210083.947.5587.7310.4580.675.310106.809.01078.706.4桃子20105.504.52077.403.3100112.045.810092.392.57

9SN/T5365—2022表B.111種基質(zhì)中氟唑磺隆和氟吡磺隆的添加水平、平均回收率和相對標(biāo)準(zhǔn)偏差(RSD)(n=6)(續(xù))氟唑磺隆氟吡磺隆基質(zhì)加標(biāo)量平均回收率RSD加標(biāo)量平均回收率RSD種類μg/kg%%μg/kg%%591.3013.5582.579.31096.0012.01081.005.0葡萄20107.854.72018.1112.9100111.478.610090.688.4585.6713.8586.4713.71095.5313.11091.8712.8糙米2092.5710.520114.8612.710087.482.9100105.1112.8588.3014.8586.5313.010103.5814.910103.1712.9小麥2092.5710.52088.586.210078.504.110089.6514.3582.9712.4582.0312.71092.4514.41094.0814.7核桃20106.7312.22093.9310.210090.622.710084.2014.8581.1712.3582.7710.61093.9014.21095.5713.1大米2095.9312.02095.1310.210093.606.810084.219.18

10SN/T5365—2022ForewordThisstandardwasdraftedaccordingtoGB/T1.1—2009.ThisstandardwasproposedbyandwasunderthechargeofGeneralAdministrationofCustomsofthePeople’sRepublicofChina.ThisstandardwasdraftedbyYiningCustomsTechnicalCenter,YiliNormalUniversity,TianjinCus-tomsIndustrialProductSafetyTechnicalCenter,TianjinCustomsAnimalandplantandFoodInspec-tionCenter,ChengduCustomsTechnicalCenter.ThemaindraftersofthisstandardareLiFang,SuYouzhi,FenXinzhong,XuYingjie,WangXinglei,ZhouLei,LiuJun,XiaoYabing,LeiHongqin,LiYanmei,Luoqiong,YuanXiaowen,ShangShuang,ZhouJun,LuPing.9

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12SN/T5365—2022Determinationofflucarbazone-sodiumandflucetosul-furonresiduesinfoodstuffsofplantoriginforex-port—LC-MS/MSmethod1ScopeThisstandardspecifiesthemethodofdeterminationofflucarbazone-sodiumandflucetosulfuronresi-duesinfoodstuffsofplantoriginbyLC-MS/MSmethodforexport.Thisstandardisapplicabletothedeterminationandconfirmationofflucarbazone-sodiumandfluceto-sulfuronresiduesinspinach,celery,potatoes,tomatoes,apples,peaches,grapes,brownrice,wheat,walnutsandriceofplantoriginfoods.2NormativeReferencesThefollowingdocumentsisnecessaryforthisstandard.Fordatedreference,onlydatededitionsshouldapplytothisstandard.Forundatedreference,thelatesteditionofthenormativedocumentreferredtoapplies.GB2763—2019Nationalfoodsafetystandards—Maximumpesticideresiduelimitsforpesticidesinfood.GB/T6682Waterforanalyticallaboratoryuse—Specificationandtestmethods3TermsanddefinitionsThereisnotermordefinitiontobedefinedinthisdocument.4Principle(90+10)(v/v),Thetestsampleswereextractedbyacetonitrile-toluenepurifiedbydispersion-sol-(LC-MS/MS),idphaseextraction,detectedbyliquidchromatography-massspectrometryandquan-tifiedbycurveexternalstandardmethod.11

13SN/T5365—20225ReagentsandmaterialsUnlessotherwisespecified,allreagentsshouldbeofanalyticalgrade.WateristhefirstgradewaterprescribedbyGB/T6682.5.1Acetonitrile:ChromatographicGrade.5.2Ammoniumacetate:GuaranteedreagentGrade.5.3Formicacid:GuaranteedreagentGrade.5.4Toluene:GuaranteedreagentGrade.5.5Sodiumchloride.(5.3)5.60.1%formic-5mmol/Lammoniumacetatesolution:Diluteformicacid1mLto1000mL(5.2),withwater;accuratelyweigh0.375gammoniumacetateaddittotheconstantvolumesolu-tion,andmixwell.(90+10)(v/v):(5.4)(5.1)5.7Acetonitrile-tolueneDilutetoluene100mLwithacetonitrileso-lutionto1000mL.5.8Filtrationmembrane:0.22μm,nylonmembrane.5.9Octadecylsilicagelfiller(C18filler):40μm.5.10GraphitizedcarbonGCB:120~400mesh.5.11Flucarbazone-sodiumstandardsubstance:CAS145026-88-6.5.12Flucetosulfuronstandardsubstance:CAS412928-75-7.(accurate5.13Standardreservesolution:10mgto0.1mg)flucarbazone-sodiumstandardsub-(5.11)(5.12)stanceandflucetosulfuronstandardsubstancewasaccuratelyweighedandpreparedinto1000μg/mLstandardreservesolutionwithacetonitrile,respectively.Thesolutionwasstoredat4℃awayfromlightandwasvalidfor6months.5.14Intermediatemixedstandardsolution:appropriateamountofstandardreservesolution(5.13)wasabsorbedanddilutedwithacetonitrile.Intermediatemixedstandardsolutionwithcon-centrationof10μg/mLwaspreparedandstoredat4℃awayfromlightfor2months.5.15Blankmatrixsolution:blankmatrixsolutionwasobtainedafterthenegativeblanksamplesof12

14SN/T5365—2022differentsubstrateswereextractedandpurifiedaccordingto7.1and7.2.(5.14)5.16Matrixmatchingworkingsolution:Dilutethemediummixedstandardsolutiontothe(5.15)appropriateconcentrationofmatrixmatchingworkingsolutionwithmatrixblanksolutionasrequired,needcompoundatoncewhenusing.6Apparatusandequipment6.1Liquidchromatograhywithelectrosprayionizationmassspectrometry.6.2Balances(0.1mg,0.01g).6.3Tissueblender.6.4Vibrator./min.6.5Centrifuge:8000r6.6Centrifugetubes:50mLand2mL.6.7Vortexdevice.7SamplepreparationandstorageThesamplingpartsofvegetablesandfruitsshallbecarriedoutinaccordancewiththeprovisionsofGB2763—2019.500gofsamplesaretaken,homogenizedwithatissuemower,thoroughlymixed,anddividedinto2parts.Thesamplesareputintoacleancontainer,sealedandmarked,andfrozenunder-18℃.Thewholenutsamplewasshelled500g,homogenizedwithatissuemower,mixedthoroughly,di-videdinto2parts,putintoacleancontainer,sealedandmarked,andstoredat0℃~4℃.500grepresentativegrainsampleswerecrushedtopassthrough425μmstandardmeshsieve.Thesamplesweredividedinto2partsandplacedinacleancontainer,sealedandmarked.Thesampleswerestoredat0℃~4℃.13

15SN/T5365—20228Procedure8.1Extraction8.1.1Vegetablesandfruits(accurate,vor-Weight5gto0.01g)ofthetestsampleinto50mLcentrifugetube,add5mLwater,(90+10)(v/v)texfor30s10mLacetonitrile-toluenewereaddedandhorizontallyshockedfor(5.5)20min,Then4gsodiumchloridewereaddedandhorizontallyoscillatedfor5min,centrifugedat8000r/minfor5min.Take1mLsupernatantinto2mLpluggedcentrifugetubeforpurification.8.1.2Grainsandnuts(accurate,Weight2.5gto0.01g)ofthetestsampleinto50mLcentrifugetube,add7mLwater,(90+10)(v/v)vortexfor30s10mLacetonitrile-toluenewereaddedandhorizontallyshocked(5.5)for20min,Then4gsodiumchloridewereaddedandhorizontallyoscillatedfor5min,centri-fugedat8000r/minfor5min.Take1mLsupernatantinto2mLpluggedcentrifugetubeforpurifica-tion.8.2Clean-upForvegetablesandfruits,50mgC18filler(5.9)and30mgGCB(5.10)wereaddedintothesuperna-tanttobepurified.Thesupernatantwasvortexfor30sandcentrifugedat8000r/minfor2min.Thesupernatantwastakenandfilteredthroughthe0.22μmnylonfilterfilm.ThefiltrateisreadyforLC-MS/MSanalysis.C18filler(5.9)50mgwereaddedintograinandnutsupernatanttobepurified,vortexfor30sandcentrifugedat8000r/minfor2min.Thesupernatantwastakenandfilteredthroughthe0.22μmnylonfilterfilm.ThefiltrateisreadyforLC-MS/MSanalysis.ThegrainandnutsupernatanttobepurifiedwasaddedwithC18filler(5.9)50mg,vortex30s,cen-trifugationat8000r/minfor2min,andthesupernatantwasfilteredthrougha0.22μmmembrane,andthefiltratewastested.8.3Determination8.3.1LCoperatingconditionReferenceLCoperatingconditionwereasfollows:a)Column:C18,3μm,100mm×2.1mm(i.d);ortheequivalent;14

16SN/T5365—2022b)MobilephaseA:0.1%formicacid-5mmol/Lammoniumacetatesolution(5.6);mobilephaseB:acetonitrile;gradientofmobilephaseseetable1;c)Columntemperature:30℃;d)Injectionvolume:10μL.Table1—Gradietofmobilephasetime/minFlowrate/(μL/min)MoblieA/%MoblieB/%phasephase0.0025090.010.01.0025090.010.01.5025050.050.05.5025010.090.05.6025090.010.010.0025090.010.08.3.2MSoperatingconditionReferenceLCoperatingconditionwereasfollows:a)Ionsource:ESI;b)Dryingtemperature:300℃;/min;c)Drygasflowrate:9.0Ld)Sheathgastemperature:250℃;/min;e)Sheathgasflowrate:11.0Lf)Capillaryvoltage:4kV;g)Scanningmode:positiveionscanning.Quantitativeandqualitativeionpair,collisionenergy,fragmentorvoltageareshowninTable2.15

17SN/T5365—2022Table2—Quantitativeandqualitativeionpair,collisionenergy,fragmentorvoltage,retentiontimeQuantitativeandqualitativeFragmentorCollisionNO.CompoundRetentiontime/minionvoltage/Venergy/eVpair/(m/z)flucarbazone-*;397.1/115.08010;5814.69397.1/130.0sodium*;488.5/273.012014;182flucetosulfuron5.69488.5/156.0*Quantitativeionpair8.4QualificationtestInaccordancewiththeaboveconditionsforthedeterminationofsamplesandthemixedmatrixstandardworkingsolution,theretentiontimeofcompoundsinthesampletobetestedshouldbewithin±2.5%comparedwiththestandardsolution.Qualitativeionswereallpresent,andtheS/N≥3,Therelativeabundanceofthequalitativeionpairisconsistentwiththerelativeabundanceofthemixedmatrixstandardworking,thedeviationoftherelativeabundancedoesnotexceedtheprovisionsinTable3,itcanbejudgedthattherearecorrespondingmeasuredobjectsinthesample.Table3—MaximumpermittedtoleranceofrelativeionintensitiesforqualificationRelativeionintensity/%>50>20~5010~20≤10Permittedtolerances/%±20±25±30508.5QuantificationtestAccordingtothecontentofthetestedobjectinthesample,thestandardsolutionofmatrixwithsimilarconcentrationshouldbeselected.Theresponsevalueofthetestedobjectshouldbewithinthelinearrangeoftheinstrumentdetection.Ifthecontentofthetestedobjectexceedstherangeofthestandardcurve,thematrixblanksamplesolutionshouldbedilutedtotheappropriateconcentra-tionforanalysis.Undertheaboveconditions,themonitoringchromatogramsofmultiplereactionsofflucarbazone-sodiumandflucetosulfuronareshowninFigureA.1~A.2inAnnexA,andalsotheretentiontime.8.6BlanktestTheoperationoftheblanktestisthesameastheproceduredescribedabove,butwithomissionofsampleaddition.16

18SN/T5365—20229CalculationandexpressionoftheresultTheresidualamountsofflucarbazone-sodiumandflucetosulfuroninthesampleswerecalculatedac-(1),BlankcordingtoFormulavaluesshouldbedeductedfromthecalculationresults.c×V1000X=×…………………………(1)m1000Type:(μg/kg);XThecontentofthemeasuredobjectinthesampleinmicrogramsperkilogram,cTheconcentrationofthemeasuredcomponentsolutionobtainedfromthestandardworking(ng/mL);curve,(mL);VThevolumeoftheextract,(g);mThecorrespondingmassofthetestsample,1000Conversionfactor.Thecalculationresultsretaintwosignificantdigits.10Limitofdetermination(LOD)Thelimitofdetectionofflucarbazone-sodiumandflucetosulfuronwere5.0μg/kg.11RecoveryandprecisionTheadditionrecoverytestwasconductedonthematrixofspinach,celery,potato,tomato,apple,peach,grape,brownrice,wheat,rice,walnutandsoon.TherecoverydataofdifferentmatrixswithdifferentadditionlevelswereshowninAnnexB.17

19SN/T5365—2022AppendixA(Informative)MRMchromatogramofflucarbazone-sodiumandflucetosulfuronMRMchromatogramofflucarbazone-sodiumandflucetosulfuronseeFigureA.1~FigureA.2.FigureA.1MRMchromatogramofflucarbazone-sodium(10ng/mL)FigureA.2MRMchromatogramofflucetosulfuron(10ng/mL)18

20SN/T5365—2022AppendixB(Informative)Azithromycinanditsinternalstandardchromatogram(RSD)Spikedlevel,averagerecoveryandrelativestandarddeviationofflucarbazone-sodiumandflucetosulfuroninspinach,celery,potato,tomato,apple,peach,grape,brownrice,wheat,wal-nutandriceseeTableB.1.(RSD)TableB.1—Spikedlevel,averagerecoveryandrelativestandarddeviationofflucarbazone-sodiumandflucetosulfuronin11kindsofmatrix(n=6)Flucarbazone-sodiumFlucetosulfuronMatrixSpikedlevelAveragerecoveryRSDSpikedlevelAveragerecoveryRSDμg/kg%%μg/kg%%583.809.6581.576.61091.396.61082.303.6spinach2095.625.720103.4813.010096.043.310098.988.2582.5310.1592.7312.110103.189.810100.1513.1celery20100.625.82098.5511.610093.1111.210094.7811.7589.079.5589.9711.31093.479.01096.227.9potato2098.507.22087.9711.2100101.1812.910097.216.6592.9312.9588.7311.510104.383.51090.029.8tomato20102.145.32088.255.9100107.004.310091.846.4587.4313.2584.5010.010114.153.81089.159.5apple20103.997.12089.706.3100110.002.210083.947.5587.7310.4580.675.310106.809.01078.706.4peach20105.504.52077.403.3100112.045.810092.392.519

21SN/T5365—2022(RSD)TableB.1—Spikedlevel,averagerecoveryandrelativestandarddeviationof(Continued)flucarbazone-sodiumandflucetosulfuronin11kindsofmatrix(n=6)Flucarbazone-sodiumFlucetosulfuronMatrixSpikedlevelAveragerecoveryRSDSpikedlevelAveragerecoveryRSDμg/kg%%(μg/kg)%%591.3013.5582.579.31096.0012.01081.005.0grape20107.854.72018.1112.9100111.478.610090.688.4585.6713.8586.4713.71095.5313.11091.8712.8brownrice2092.5710.520114.8612.710087.482.9100105.1112.8588.3014.8582.0312.710103.5814.91094.0814.7wheat2092.5710.52093.9310.210078.504.110084.2014.8582.9712.4582.7710.61092.4514.41095.5713.1walnut20106.7312.22095.1310.210090.622.710084.219.1581.1712.3586.5313.01093.9014.210103.1712.9rice2095.9312.02088.586.210093.606.810089.6514.320

222022—5365/TSN中華人民共和國出入境檢驗(yàn)檢疫行業(yè)標(biāo)準(zhǔn)出口植物源性食品中氟唑磺隆和氟吡磺隆殘留量的測定液相色譜-質(zhì)譜/質(zhì)譜法SN/T5365—2022*中國海關(guān)出版社有限公司出版發(fā)行北京市朝陽區(qū)東四環(huán)南路甲1號(100023)編輯部:(010)65194242-7530網(wǎng)址www.customskb.com/book中國標(biāo)準(zhǔn)出版社秦皇島印刷廠印刷*開本880×12301/16印張1.5字?jǐn)?shù)46千字2022年9月第一版2022年9月第一次印刷印數(shù)1—*書號:155175·722定價(jià)24.00元