ICSCCSX T/SQIA066—389Rapiddeterminationof389pesticidesresiduesinmixedsamplesofagriculturalproductsHighperformanceliquidchromatographytandemmassspectrometry2024年8月20日發(fā)布 2024年9月1日實(shí)施深圳市質(zhì)量檢驗(yàn)協(xié)會(huì)發(fā)布T/SQIAT/SQIA066—T/SQIAT/SQIA066—目 前本文件按照GB/T1.1-20201部分：標(biāo)準(zhǔn)化文件的結(jié)構(gòu)和起草規(guī)則》給出的規(guī)T/SQIAT/SQIA066—T/SQIAT/SQIA066—389389GB2763GB/T6682分析實(shí)驗(yàn)室用水規(guī)格和試驗(yàn)方法GB/T27404238610。NPSGC）Xi，Xi通過轉(zhuǎn)換，得到單樣品中各農(nóng)藥GB/T6682：色譜純;無水硫酸鎂（MgSO4），5254h，置于干燥器中備用；CAS7487-88-9乙二胺-N-丙基硅烷吸附劑(PSA40μm～60μm甲酸銨-甲酸水溶液(2mmol/L)0.1261g0.0110001000mL,微孔濾膜（有機(jī)相）：13mm×0.22μm十八烷基硅烷鍵合硅膠（C18）40μm～60μm石墨化炭黑（GCB）40μm～120μm陶瓷均質(zhì)子：2cm（長）×1cm（外徑）號(hào)：號(hào)：389種農(nóng)藥標(biāo)準(zhǔn)品名稱和CAS號(hào),參見附錄A；每種農(nóng)藥標(biāo)準(zhǔn)品均為1000mg/L，純度≥95%。6種內(nèi)標(biāo)D（CAS74223-613CCAS1808990-7，每種內(nèi)標(biāo)農(nóng)藥標(biāo)準(zhǔn)品均為100mg/L取5.2.1標(biāo)準(zhǔn)品（1000mg/L）用乙腈定容配制成20mg/L混合標(biāo)準(zhǔn)儲(chǔ)備液，-18取5.2.1內(nèi)標(biāo)（100mg/L）用乙腈定容配制成10mg/L混合內(nèi)標(biāo)儲(chǔ)備液，-0mg/L18℃冰箱中保存，有0mg/L18℃冰箱中保存，有0.01g12000r/minGB2763A3003020.00g80mL10mg/L)20μL20mL10min8g2g2gr/min6min6mL900mg150mgPSA45mgGCB15mL2min，9000r/min6min1mL色譜柱：C18（2.1mm（內(nèi)徑）100mm1.8μm）1；流速：0.3柱溫：40進(jìn)樣量：4μL~6μL1流動(dòng)相及其梯度條件5500V，負(fù)離子-4500離子源溫度：350霧化氣：60輔助加熱氣：55氣簾氣：400.5μg/L、1.0μg/L、5.0μg/L、10.0μg/L、50.0μg/L、100μg/L、200μg/L，過微孔2LC-MS/MSCωρAPiAsiV

ASPsiAi A—試樣溶液中被測物的質(zhì)量色譜圖峰面積；Pi—試樣溶液中內(nèi)標(biāo)物的質(zhì)量濃度,單位為微克每毫升（μg/mL）；Ai—試樣溶液中內(nèi)標(biāo)物的色譜峰面積；本方法被測組分含量≥0.1mg/kg80%~110%；被測組分含量＜0.1mg/kg，回收率范圍60%~120%。DD.13DD.20.5μg/kg~5μg/kgA附錄A.1。A.13896（按英文字母順序）A以毒死蜱-D10azinphos內(nèi)吸磷-SdisulfotondisulfotonT/SQIAT/SQIA066—T/SQIAT/SQIA066—fenamiphosfenamiphosfensulfothionfensulfothionoxonfensulfothionfenthionfenthionphoratephoratephosmetterbufosterbufosB以吡蟲啉-D4piperonyl乙基多殺菌素spinetoram乙基多殺菌素spinetoram多殺霉素spinosad多殺霉素spinosadC以滅蠅胺-13C3clethodimclethodimprochlorazmetaboliteprochlorazmetaboliteD以醚菊酯-D5cyazofamidmetabolitefipronilfipronilfipronil除蟲菊素pyrethrins除蟲菊素pyrethrinstriflumizolemetaboliteFM-6-E以甲萘威-D7aldicarbaldicarb3-hydroxydiethylaminoethylemamectinivermectinmethiocarbmethiocarboxamylF以甲磺隆-D3 甲萘威-毒死蜱-滅蠅胺-醚菊酯-吡蟲啉-甲磺隆-T/SQIAT/SQIA066—T/SQIAT/SQIA066—附錄B.13896離子對(duì)184.0/184.0/223.0/223.0/270.1/270.1/559.0/559.0/270.0/270.0/266.0/266.0/208.0/208.0/aldicarb240.1/240.1/aldicarb207.0/207.0/303.0/303.0/276.2/276.2/228.1/228.1/370.0/370.0/466.0/466.0/368.0/368.0/216.1/216.1/895.5/895.5/318.0/318.0/404.1/404.1/326.0/326.0/272.0/272.0/224.1/224.1/411.1/411.1/-396.0/-396.0/-364.1/364.1/離子對(duì)359.0/359.0/440.3/440.3/339.2/339.2/338.2/338.2/343.0/343.0/378.0/378.0/317.0/317.0/306.2/306.2/312.1/312.1/296.1/296.1/271.0/271.0/202.1/202.1/192.0/192.0/222.1/222.1/3-hydroxy238.0/238.0/236.1/236.1/412.0/412.0/483.9/483.9/309.0/309.0/197.1/197.1/359.0/359.0/540.0/542.0/222.0/222.0/415.0/415.0/-244.6/-244.6/-214.0/214.0/350.0/350.0/322.0/324.0/358.0/358.0/213.1/213.1/395.2/395.2/T/SQIAT/SQIA066—T/SQIAT/SQIA066—離子對(duì)414.1/414.1/360.0/360.0/clethodim392.1/392.1/clethodim376.1/376.1/303.0/303.0/240.1/240.1/250.0/250.0/363.0/363.0/437.1/437.1/241.1/241.1/475.0/475.0/325.0/325.0/氰霜唑代謝物cyazofamid-216.0/-216.0/-422.1/422.1/326.2/326.2/413.0/413.0/465.2/465.2/451.0/453.0/467.1/469.1/199.1/199.1/433.2/433.2/393.2/393.2/292.2/292.2/226.1/226.1/167.0/167.0/523.0/523.0/259.0/259.0/231.0/231.0/263.1/263.1/離子對(duì)291.0/291.0/內(nèi)吸磷-S275.1/275.1/305.0/305.0/221.0/221.0/328.0/330.0/358.0/358.0/251.0/251.0/238.1/238.1/268.0/268.0/diethyl216.1/216.1/406.1/406.1/311.0/311.0/395.1/395.1/264.1/264.1/276.1/276.1/230.0/230.0/388.1/388.1/327.2/327.2/326.0/326.0/-295.1/-295.1/-203.1/203.1/275.1/275.1/disulfoton307.0/307.0/disulfoton291.0/291.0/233.1/233.1/311.0/311.0/emamectin886.5/886.5/400.1/400.1/324.1/324.1/330.0/330.0/離子對(duì)385.0/385.0/397.0/397.0/210.0/210.0/287.1/287.1/243.0/243.0/399.1/399.1/394.2/394.2/360.2/360.2/293.1/293.1/392.0/392.0/312.1/312.1/434.1/434.1/304.2/304.2/fenamiphos336.0/336.0/fenamiphos320.1/320.1/331.0/331.0/307.2/307.2/337.1/337.1/302.0/302.0/278.0/278.0/208.1/208.1/254.1/254.1/329.1/329.1/362.0/362.0/302.2/302.2/350.3/350.3/274.3/274.3/304.1/304.1/332.0/332.0/422.0/422.0/309.0/309.0/離子對(duì)fensulfothion293.1/293.1/fensulfothion309.1/309.1/fensulfothion325.0/325.0/279.1/279.1/fenthion311.0/311.0/fenthion295.0/295.0/437.0/437.0/-435.0/-435.0/-fipronil-387.0/-387.0/-fipronil-419.0/-419.0/-fipronil-451.0/-451.0/-230.0/230.0/360.0/360.0/384.0/384.0/-463.0/-463.0/-705.1/705.1/488.1/488.1/469.0/469.0/266.1/266.1/364.0/364.0/489.0/489.0/422.1/422.1/326.1/326.1/372.1/372.1/382.9/382.9/397.0/397.0/465.1/465.1/334.1/334.1/316.0/316.0/404.0/404.0/324.1/324.1/離子對(duì)302.1/302.1/382.1/382.1/247.1/247.1/248.1/248.1/258.0/258.0/284.0/284.0/383.2/383.2/435.0/435.0/251.0/251.0/314.1/314.1/460.9/460.9/253.1/253.1/353.0/353.0/297.1/297.1/411.0/411.0/256.1/256.1/262.1/262.1/319.2/319.2/528.0/528.0/508.0/508.0/334.0/334.0/289.1/289.1/330.1/330.1/321.2/321.2/316.0/316.0/231.0/231.0/332.0/332.0/194.0/194.0/291.1/291.1/207.1/207.1/離子對(duì)360.2/360.2/360.0/360.0/-358.0/-358.0/-ivermectin897.5/897.5/314.1/314.1/479.1/479.1/249.0/249.0/511.0/511.0/315.0/315.0/331.0/331.0/412.1/412.1/299.1/299.1/270.1/270.1/504.1/504.1/507.0/507.0/280.2/280.2/441.1/441.1/203.1/203.1/278.0/278.0/476.1/476.1/320.2/320.2/241.0/241.0/142.0/142.0/303.0/303.0/226.1/226.1/methiocarb258.0/258.0/methiocarb242.0/242.0/163.0/163.0/279.0/279.0/303.2/303.2/離子對(duì)369.2/369.2/284.1/284.1/166.1/166.1/409.0/409.0/215.1/215.1/382.1/382.1/225.0/225.0/188.1/188.1/224.1/224.1/289.0/289.0/272.1/272.1/271.1/271.1/493.0/493.0/214.0/214.0/425.1/425.1/341.0/341.0/345.0/345.0/279.1/279.1/237.1/237.1/oxamyl163.0/163.0/376.1/376.1/247.0/247.0/362.0/362.0/294.0/294.0/292.0/292.0/264.0/264.0/284.0/284.0/329.0/329.0/282.1/282.1/318.0/318.0/484.1/484.1/離子對(duì)360.0/360.0/408.2/408.2/217.1/217.1/301.1/301.1/321.0/321.0/261.0/261.0/phorate293.0/293.0/phorate277.0/277.0/368.0/368.0/256.1/256.1/228.0/228.0/318.0/318.0/phosmet302.0/302.0/300.1/300.1/299.0/299.0/377.0/377.0/368.1/368.1/piperonyl356.2/356.2/239.2/239.2/225.1/225.1/253.0/253.0/306.1/306.1/312.1/312.1/224.0/224.0/376.2/376.2/prochloraz325.0/327.0/prochloraz353.0/355.0/284.0/286.0/373.0/373.0/離子對(duì)208.1/208.1/242.1/242.1/212.1/212.1/189.0/189.0/218.1/218.1/444.0/444.0/368.0/368.0/342.1/344.1/284.1/284.1/210.1/210.1/456.1/456.1/256.0/256.0/373.0/373.0/252.0/252.0/388.1/388.1/413.0/413.0/382.1/382.1/413.1/413.1/415.1/415.1/329.2/329.2/373.2/373.2/610.2/610.2/365.0/365.0/492.0/492.0/341.0/341.0/319.0/319.0/200.0/200.0/385.2/385.2/322.1/322.1/289.1/289.1/299.0/299.0/373.1/373.1/395.0/395.0/501.1/501.1/離子對(duì)303.2/303.2/332.0/332.0/328.1/328.1/268.1/268.1/202.0/202.0/214.1/214.1/乙基多殺菌素spinetoram748.5/748.5/乙基多殺菌素spinetoram760.4/760.4/多殺霉素spinosad732.4/732.4/多殺霉素spinosad746.4/746.4/411.2/411.2/388.0/388.0/374.0/374.0/302.1/302.1/464.0/464.0/318.0/318.0/-304.1/304.1/387.0/387.0/323.0/323.0/278.0/278.0/503.1/503.1/308.0/308.0/353.1/353.1/229.1/229.1/381.1/381.1/289.1/289.1/terbufos321.0/321.0/terbufos305.0/305.0/230.1/230.1/372.0/372.0/202.0/202.0/253.1/253.1/離子對(duì)292.0/292.0/221.0/221.0/388.0/388.0/528.8/528.8/343.0/343.0/301.0/301.0/384.1/384.1/330.1/330.1/294.0/294.0/296.1/296.1/304.0/304.0/402.1/402.1/314.0/314.0/396.1/396.1/256.9/256.9/190.0/190.0/409.1/409.1/346.0/346.0/triflumizole295.0/295.0/359.1/359.1/493.1/493.1/318.0/318.0/446.0/446.0/292.1/292.1/288.0/288.0/336.0