TZNZ 221-2023 水产品中37 种农药残留量的测定 气相色谱-串联质谱法

ICS67.120.30CCSB50

T/ZNZT/ZNZ221—202337Determinationof37pesticidesresiduesinaquaticproductbygaschromatography-tandemmassspectrometricmethod2023-10-13发布 2023-11-13实施浙江省农产品质量安全学会  发布T/ZNZ221T/ZNZ221—2023II前  言本文件按照GB/T1.1—20201草。请注意本文件的某些内容可能涉及专利。本文件的发布机构不承担识别专利的责任。本文件由浙江省农产品质量安全学会提出并归口。本文件起草单位：绿城农科检测技术有限公司。本文件主要起草人：赵月钧、俞璐萍、倪娟桢、徐冰洁、姜亚琴、王伟、桑力青、王馨瑜、马晓莹、陶杨匀、黄荣博、吴丹虹、李闻洁、童晓玲、梁黎明、徐巧。T/ZNZ221T/ZNZ221—2023PAGEPAGE1水产品中37种农药残留量的测定气相色谱—串联质谱法范围本文件规定了水产品中37种农药残留量的气相色谱—串联质谱测定方法。本文件适用于鱼类、虾类、蟹类、鳖类等水产品中37种农药的测定。规范性引用文件（包括所有的修改单适用于本文件。GB/T6682分析实验室用水规格和试验方法术语和定义本文件没有需要界定的术语和定义。原理试剂和材料除非另有说明，本方法所用试剂均为分析纯，水为GB/T6682规定的一级水。5.1 乙腈CHCNCAS号：7505-）色谱纯。5.2 丙酮CHCOC，CAS号：11-543）色谱纯。5.3 （H，CAS号：11054-）色谱纯。（A3）200目～300目。（MgO）650℃灼烧4h，置于干燥器内冷却后备用。氯化钠（NaCl）500℃灼烧4h，置于干燥器内冷却后备用。N-丙基乙二胺（PSA）粒径范围40μm～60μm，平均孔径100Å。C8吸附剂）粒径范围40μm～60μm，平均孔径60Å。微孔滤膜0.22μm，有机膜。5.10 丙酮-正己烷溶液（10:90）量取10mL丙酮加入90mL正己烷中，混匀。标准品37种农药及环氧七氯的中文名称、英文名称、CAS号、分子式、相对分子量见附录A，纯度应≥95%。标准溶液配制标准储备溶液：分别准确称取标准品（5.11）10mg10mL，此溶液浓1000mg/L。2℃~8℃6个月。1.00mL5.121100mL10m/L的混合标准中间溶液，2℃~8℃避光密封保存，有效期1个月。10mg100100mg/L。仪器和设备气相色谱—串联质谱仪：配有电子轰击源。0.01mg0.01g。低温离心机：转速≥8000r/min。涡旋振荡器：转速≥2000r/min。40kHz200W。分析步骤试样制备与保存-18℃以下冷冻保存；-18℃以下冷冻保存；蟹类取可食部分，绞碎混合均匀后备用，制好后将试样于-18℃以下冷冻保存；龟鳖类取可食部分，绞碎混合均匀后备用，制好后将试样于-18℃以下冷冻保存；提取称取5g（精确至于50mL10mL1min10.0mL乙腈（5.1），涡旋振荡1min，超声提取20min，4℃条件下8000r/min离心5min，取上清液于装有5g氯化钠（5.6）的50mL离心管中，再加10.0mL乙腈（5.1），混匀1min，4℃条件下8000r/min离心5min，合并上清液。净化和浓缩将6.00mL提取液置于装有100mgPSA（5.7）、100mgC18（5.8），500mg中性氧化铝（5.4）和300mg无水硫酸镁（5.5）的15mL离心管中，涡旋混匀3min，4℃下8000r/min离心3min。取4.00mL上清液氮吹近干，准确加入0.500mL丙酮—正己烷溶液（5.10），加入内标溶液（5.12.3）15μL，涡旋混匀10s，过0.22μm微孔滤膜（5.9），供气相色谱—串联质谱联用仪分析。测定色谱参考条件色谱柱：（5%-苯基）-甲基聚硅氧烷石英毛细管柱（30m0.25mm0.25μm），或性能相当者。进样量：1.0μL。进样口温度：250℃。进样方式：不分流进样。7.4.1.5 载气：高纯氮气，纯度≥99.999%。7.4.1.6柱流速：1.41mL/min。7.4.1.7柱温程序：80℃，保持1min40℃/min升至170℃，保持1min20℃/min升至290℃，保持7min。质谱参考条件离子源：电子轰击源（EI），70eV。接口温度：280℃。离子源温度：230℃。溶剂延迟时间：3.2min。标准工作曲线精确吸取一定量的混合标准溶液，逐级用丙酮—正己烷溶液（5.10）稀释成质量浓度为0.005mg/L、0.01mg/L、0.05mg/L、0.1mg/L、0.5mg/L和0.8mg/L的标准工作溶液。空白基质溶液氮气吹干，加入15μL1mL配置成系列基质混合标准工—定性测定2.5之内；表1定性确证时相对离子丰度的最大允许偏差相对丰度（%）＞50＞20-50＞10-20≤10允许偏差（%）±20±25±30±50试样溶液的测定将基质混合标准工作溶液和试样溶液依次注入气相色谱—质谱联用仪中，保留时间和定性离子定平行试验按7.2~7.3的规定对同一试样进行平行试验测定。空白试验除不加试样外，均按7.2~7.3的规定进行平行操作。结果计算和表述8.1 定量测定采用标准曲线法或单点内标法定量。按式（1）或仪器数据处理软件计算获得：············（1）式中：——试样中被测物质的残留量，单位为毫克每千克（mg/kg）；——可从标准曲线上或仪器上直接得到被测物质的浓度，单位为毫克每升（mg/L）；f——稀释因子；——溶解残余物所用定容溶液体积，单位为毫升（mL）；——试样质量，单位为克（g）；F——最终分取体积/提取液体积。计算结果应扣除空白值，保留3位有效数字。定量限本方法的定量限为0.01mg/kg~0.03mg/kg（参见附录A）。准确度本方法在0.03mg/kg~0.3mg/kg添加浓度水平上的回收率在70%~120%之间，见附录D。精密度在重复性条件下获得的两次独立测定结果的绝对差值不得超过算术平均值的15%，见附录D。T/ZNZ221T/ZNZ221—2023PAGEPAGE1附 录 A（资料性）37种农药及内标的中英文名称、CAS号、分子式、相对分子量、定量限表A.1给出了37种农药及内标的中英文名称、CAS号、分子式、相对分子量、定量限。表A.137种农药及内标的中文名称、英文名称、CAS号、分子式、相对分子量、定量限序号中文名称英文名称CAS号分子式相对分子量定量限/mg·kg-11α-六六六Alpha-BHC319-84-6C6H6Cl6290.830.032β-六六六Beta-BHC319-85-7C6H6Cl6290.830.033γ-六六六Gamma-BHC58-89-9C6H6Cl6290.830.034δ-六六六Delta-BHC319-86-8C6H6Cl6290.830.035苯醚甲环唑Difenoconazole119446-68-3C19H17Cl2N3O3406.260.026吡唑醚菌酯Pyraclostrobin175013-18-0C19H18ClN3O4387.820.037丙环唑Propiconazole60207-90-1C15H17Cl2N3O2342.220.038虫螨腈Chlorfenapyr122453-73-0C15H11BrClF3N2O407.610.039敌敌畏Dichlorvos62-73-7C4H7Cl2O4P220.980.0310丁草胺Butachlor23184-66-9C17H26ClNO2311.850.0211毒死蜱Chlorpyrifos2921-88-2C9H11Cl3NO3PS350.590.0112二甲戊灵Pendimethalin40487-42-1C13H19N3O4281.310.0213氟虫腈Fipronil120068-37-3C12H4Cl2F6N4OS437.150.0314氟虫腈砜Fipronil-sulfone120068-36-2C12H4Cl2F6N4O2S453.150.0215氟虫腈硫醚Fipronil-sulfide120067-83-6C12H4Cl2F6N4S421.150.0316氟甲腈Fipronil-desulfinyl205650-65-3C12H4Cl2F6N4389.080.0217环氧七氯Hcptachlor-epoxideB17498-34-9C12H14O5238.24/18甲氰菊酯Fenpropathrin64257-84-7C22H23NO3349.420.0319联苯菊酯Bifenthrin82657-04-3C23H22ClF3O2422.870.0120氯氟氰菊酯和高效氯氟氰菊酯CyhalothrinandIambda-cyhalothrin68085-85-891465-08-6C23H19ClF3NO3449.850.0321氯菊酯Permethrin52645-53-1C21H20Cl2O3391.290.03表A.1（续）序号中文名称英文名称CAS号分子式相对分子量定量限/mg·kg-122氯氰菊酯和高效氯氰菊酯Cypermethrinandbeta-cypermethrin52315-07-886752-99-0C22H19Cl2NO3416.30.0323马拉硫磷Malathion121-75-5C10H19O6PS2330.360.0224醚菊酯Etofenprox80844-07-1C25H28O3376.490.0225醚菌酯Kresoxim-methyl143390-89-0C18H19NO4313.850.0226嘧菌酯Azoxystrobin131860-33-8C22H17N3O5403.390.0327氰戊菊酯和FenvalerateandEsfenvalerate51630-58-166230-04-4C25H22ClNO3419.90.0228噻虫嗪Thiamethoxam153719-23-4C8H10ClN5O3S291.710.0329噻呋酰胺Thifluzamide130000-40-7C13H6Br2F6N2O2S528.060.0230三环唑Tricyclazole41814-78-2C9H7N3S189.240.0331三唑醇Triadimenol55219-65-3C14H18ClN3O2295.760.0232三唑磷Triazophos24017-47-8C12H16N3O3PS313.310.0233三唑酮Triadimefon43121-43-3C14H16ClN3O2293.750.0234水胺硫磷Isocarbophos24353-61-5C11H16NO4PS289.290.0235肟菌酯Trifloxystrobin141517-21-7C20H19F3N2O4408.370.0236戊唑醇Tebuconazole107534-96-3C16H22ClN3O307.820.0237溴氰菊酯Deltamethrin52918-63-5C22H19Br2NO3505.20.0338乙酰甲胺磷Acephate30560-19-1C4H10NO3PS183.170.03附 录 B（资料性）37种农药及环氧七氯监测离子对和碰撞能量表B.1给出了37种农药及环氧七氯和保留时间、监测离子对、碰撞能量。表B.1 37种农药及环氧七氯和保留时间、监测离子对、碰撞能量序号化合物保留时/min定量离子对（m/z）碰撞电压V定性离子对（m/z）碰撞电压V1α-六六六6.915218.90>182.908218.90>144.90202β-六六六7.184218.90>182.908218.90>144.90203γ-六六六7.301218.90>182.908218.90>144.90204δ-六六六7.604218.90>182.9010218.90>144.90205苯醚甲环唑14.643322.80>264.8015264.90>202.00206吡唑醚菌酯14.098132.00>77.0020132.00>51.00307丙环唑10.173259.00>69.0014259.00>191.0088虫螨腈9.579247.10>227.0016247.10>200.00249敌敌畏3.984185.00>93.0014185.00>109.001410丁草胺9.144188.10>160.2010176.10>147.102211毒死蜱8.364196.90>169.0015198.90>171.001512二甲戊灵8.745252.10>162.1010252.10>191.10813氟虫腈8.739366.80>212.8025368.80>214.802514氟虫腈砜9.343382.90>255.9024382.95>213.003615氟虫腈硫醚8.623350.90>255.9018419.95>350.901516氟甲腈7.843387.95>332.9018383.00>231.002717环氧七氯8.783352.80>262.9015352.80>281.901518甲氰菊酯10.821207.90>181.005264.90>210.001019联苯菊酯10.686181.20>165.2025181.20>166.201020氯氟氰菊酯和高效氯氟氰菊酯11.304197.00>141.0010197.00>161.005表B.1（续）序号化合物保留时间定量离子对（m/z）碰撞电压V定性离子对（m/z）碰撞电压V21氯菊酯12.104183.10>168.1014183.10>165.101422氯氰菊酯和高效氯氰菊酯12.987181.10>152.1022181.10>127.102223马拉硫磷8.293173.10>99.0014173.10>127.00624醚菊酯13.21206.10>116.106206.10>131.101425醚菌酯9.48206.10>131.1014206.10>116.10626嘧菌酯15.383344.10>329.1016344.10>183.102427氰戊菊酯和S-氰戊菊酯13.955167.00>125.105224.90>119.001528噻虫嗪8.731247.00>212.004247.00>182.001229噻呋酰胺9.415448.90>428.9020448.90>402.003430三环唑9.501189.00>161.9012189.00>135.001831三唑醇8.963168.00>70.0010128.00>65.002532三唑磷10.009161.20>134.205161.20>106.101033三唑酮8.513208.00>181.105208.00>111.002034水胺硫磷8.528135.9>108.0015135.90>69.003035肟菌酯10.059222.10>190.104222.10>162.101036戊唑醇10.416250.10>125.1022250.10>153.101237溴氰菊酯15.113252.90>93.0015250.70>172.00538乙酰甲胺磷5.106136.00>42.005136.00>94.0010T/ZNZ221T/ZNZ221—202311附 录 C（资料性）37种农药及环氧七氯的多反应监测（MRM）色谱图37种农药及环氧七氯的多反应监测（MRM）色谱图见图C.1。2.5(x10,000)2.01.51.00.5

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8.60 8.65 8.70氟甲腈

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三唑酮

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8.60

8.70 8.75 8.80水胺硫磷

毒死蜱

氟虫腈硫醚图C.1 37种农药及环氧七氯的多反应监测（MRM）色谱图（50μg/L）

(x1,000)

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(x10,000)噻虫嗪

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噻呋酰胺

醚菌酯

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(x10,000)9.85 9.90 9.9510.00三环唑

虫螨腈

三唑磷图C.1（续）

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10.5010.5510.6010.6510.7010.75

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10.9511.00

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11.3511.4011.4511.50联苯菊酯

甲氰菊酯

氯氟氰菊酯和高效氯氟氰菊酯

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33氰戊菊酯和S-氰戊菊酯

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13.0513.1013.1513.2013.25

13.3013.3513.40吡唑醚菌酯

苯醚甲环唑图C.1（续）

醚菊酯(x1,000) (x1,000)4.03.0 5.0

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15.2015.2515.3015.3515.4015.4515.5015.5537溴氰菊酯

38嘧菌酯图C.1（续）T/ZNZ221T/ZNZ221—2023PAGEPAGE1附 录 D（资料性）37种农药在不同基质样品中添加浓度及回收率与精密度范围表D.1给出了37中农药实际在不同基质样品中添加浓度及回收率与精密度范围。表D.1 37种农药在不同基质样品中添加浓度及回收率与精密度范围（n=24）序号参数添加浓度（mg/kg）中华鳖梭子蟹青蟹大黄鱼沼虾草鱼回收率范精密度范回收率范精密度范回收率范精密度范回收率范精密度范回收率范精密度范围（%）回收率范精密度范1α-六六六0.0382.0~108.02.5~8.876.7~1072.2~7.875.0~103.72.0~6.084.0~109.01.2~6.674.3~101.32.2~6.374.0~102.32.6~7.40.0982.2~100.31.8~5.381.2~99.91.9~5.579.4~98.90.7~4.280.6~100.11.4~4.873.6~100.42.1~7.579.6~99.91.8~4.70.3082.0~98.31.1~4.176.3~1001.2~5.183.0~100.71.4~4.381.0~99.30.4~5.779.7~99.01.6~4.479.3~101.02.6~3.22β-六六六0.0378.0~103.04.1~6.074.3~107.02.2~6.173.0~100.03.8~5.979.0~106.31.3~8.572.3~101.31.8~7.572.0~101.32.1~7.90.0981.4~96.01.7~5.678.2~98.71.2~4.373.2~96.40.9~7.174.3~99.20.7~4.475.8~100.61.8~4.373.9~99.41.4~6.20.3090.3~100.71.6~3.980.7~99.71.5~4.879.7~1001.0~6.278.3~110.01.0~5.577.0~100.71.2~5.272.3~100.31.7~2.83γ-六六六0.0382.0~101.02.5~5.874.0~99.72.2~4.475.7~98.03.9~4.378.3~112.04.4~5.170.7~100.74.2~7.871.7~100.01.6~5.90.0984.0~99.92.9~6.278.2~99.43.2~5.175.3~99.00.9~8.479.3~109.31.6~4.574.9~99.91.2~4.671.8~101.71.5~6.90.3086.7~100.71.9~4.681.3~100.30.9~4.381.7~100.00.7~4.681.3~108.01.2~5.473.0~100.71.2~3.871.3~98.71.0~2.44δ-六六六0.0379.3~107.02.6~7.875.0~105.32.8~8.473.7~101.72.8~7.780.0~108.03.4~4.575.3~99.72.4~6.175.3~100.02.2~6.20.0977.8~95.81.6~4.579.6~98.81.8~6.672.0~96.61.4~8.078.4~100.33.3~4.875.1~99.61.8~7.472.3~101.42.1~7.70.3087.0~99.31.4~4.581.7~98.70.9~3.676.0~101.72.2~4.878.7~99.30.5~4.378.7~100.01.5~5.574.0~97.31.0~5.8T/ZNZ221—T/ZNZ221—2023表D.1（续）PAGEPAGE2序号参数添加浓度（mg/kg）中华鳖梭子蟹青蟹大黄鱼沼虾草鱼回收率范精密度范回收率范精密度范回收率范精密度范回收率范精密度范回收率范精密度范围（%）回收率范精密度范5苯醚甲环唑0.0376.0~103.32.3~6.378.0~97.72.8~5.677.3~102.70.8~6.482.7~99.73.4~4.574.7~103.03.0~7.481.7~100.32.0~7.00.0976.3~97.72.3~3.475.1~99.33.5~5.475.3~108.71.7~7.574.0~98.41.8~4.375.1~100.03.1~6.177.1~96.32.1~5.00.3080.3~97.71.3~5.478.3~1012.4~5.680.3~105.34.4~6.575.7~100.32.9~7.173.0~100.01.8~4.773.3~99.32.3~4.96吡唑醚菌酯0.0374.0~104.02.6~4.474.3~108.72.3~5.084.0~110.73.0~7.281.3~112.73.0~6.977.7~108.72.7~7.385.0~106.71.9~4.20.0972.9~92.91.8~4.275.0~103.91.6~6.076.9~107.61.7~6.474.2~111.12.5~5.378.9~96.11.7~4.777.7~99.82.8~3.90.3091.3~95.72.2~3.378.3~102.32.5~6.884.3~101.02.1~5.174.3~101.71.5~5.774.3~105.32.0~3.379.3~102.74.0~5.87丙环唑0.0377.7~106.71.1~9.582.0~98.02.9~4.782.0~101.32.0~5.285.0~104.31.2~7.773.7~101.32.6~9.376.7~98.04.8~7.70.0977.4~99.01.3~6.786.1~101.71.9~5.983.0~101.70.7~6.784.8~107.81.2~5.176.9~100.71.3~7.579.4~99.62.9~4.80.3085.0~100.71.9~2.983.7~102.02.3~3.877.0~104.71.4~7.282.3~102.71.1~5.277.0~103.31.7~4.577.3~104.02.5~3.98虫螨腈0.0376.3~102.02.7~6.573.7~98.03.3~7.572.7~101.71.7~8.175.3~110.03.1~8.480.3~100.72.3~7.575.0~102.33.3~5.70.0982.7~95.71.7~4.970.7~101.12.2~7.579.4~101.31.1~7.480.2~113.92.0~7.780.9~100.01.8~8.280.3~105.63.5~9.80.3078.7~102.73.0~4.974.3~104.34.7~6.576.3~109.32.7~5.175.7~106.31.7~7.277.0~107.31.8·8.577.0~102.71.5~5.89敌敌畏0.0374.7~100.71.4~7.874.3~101.32.3~8.174.3~102.02.2~7.378.3~101.31.6~7.674.3~99.31.4~7.277.3~101.01.9~6.90.0982.4~97.91.8~4.681.3~97.61.6~6.080.8~97.11.9~5.983.9~108.62.4~4.080.0~103.41.5~4.280.2~101.61.0~5.00.3083.7~99.02.0~3.881.7~100.02.0~4.379.0~98.32.1~4.381.0~103.01.4~5.476.7~100.01.1~3.577.7~104.02.3~3.6序号参数添加浓度（mg/kg）中华鳖梭子蟹青蟹大黄鱼沼虾草鱼回收率范精密度范回收率范精密度范回收率范精密度范回收率范精密度范回收率范精密度范围（%）回收率范精密度范10丁草胺0.0380.7~107.32.3~5.177.0~102.33.0~6.073.0~102.32.2~7.582.7~101.01.5~4.776.3~108.01.1~8.676.0~100.01.9~7.60.0980.2~95.41.8~3.582.1~100.11.2~4.180.7~98.61.0~5.681.9~100.92.0~7.783.1~103.02.0~8.178.4~103.22.5~4.90.3084.7~98.31.5~3.982.7~98.31.8~3.281.3~95.71.9~5.784.3~97.71.2~4.380.3~101.31.7~3.880.3~100.31.9~3.211毒死蜱0.0381.3~103.31.3~5.075.0~105.32.7~5.580.0~100.31.7~7.881.7~101.71.5~4.272.0~104.31.4~6.878.7~102.02.9~4.60.0979.0~89.91.4~3.183.0~98.91.6~4.281.0~101.00.8~6.582.0~100.62.2~3.674.4~100.12.6`7.880.6~98.41.3~6.80.3080.0~98.71.7~3.080.3~100.32.3~2.680.0~100.30.6~8.079.0~99.30.5~5.179.7~104.02.4~4.278.7~101.01.9~4.712二甲戊灵0.0377.3~105.72.4~3.776.0~110.01.8~7.477.0~108.74.6~8.677.7~118.02.1~7.176.7~104.72.1~5.872.3~109.73.3~9.60.0979.4~91.32.0~5.175.9~102.72.7~6.372.7~98.72.2~7.473.7~101.61.8~6.274.2~91.22.7~5.677.2~93.32.1~5.80.3080.7~99.71.8~3.377.3~101.30.8~3.478.7~105.30.9~8.477.7~112.01.6~6.482.3~98.72.3~5.077.0~100.01.8~2.913氟虫腈0.0376.7~107.31.2~9.479.7~108.73.6~7.179.3~115.31.9~7.780.0~107.02.6~6.774.7~102.02.8~7.584.3~107.32.3~8.00.0984.0~96.02.5~4.180.9~99.32.8~4.280.7~98.10.7~5.981.8~101.72.5~3.980.0~99.72.1~7.383.7~107.01.9~5.80.3083.0~104.32.3~5.079.0~104.72.5~7.875.3~103.02.8~8.278.7~101.01.5~5.681.7~105.31.6~5.683.3~103.01.3~5.614氟虫腈砜0.0379.3~111.32.7~7.280.0~116.03.9~7.776.3~110.33.9~8.776.0~109.04.8~8.974.7~109.74.1~7.479.3~112.73.1~6.40.0979.9~88.91.2~3.482.9~94.82.1~5.380.9~101.41.0~7.978.7~106.44.1~7.378.7~100.92.4~7.083.4~99.41.4~4.70.3085.0~101.71.5~3.983.0~102.31.9~3.381.0~106.03.9~6.776.0~102.02.3~4.879.7~102.32.3~4.478.7~99.02.5~4.115氟虫腈硫醚0.0377.3~107.72.7~8.873.7~1114.3~8.575.3~111.04.7~7.780.3~99.72.8~6.775.0~109.33.3~6.083.3~112.71.5~5.90.0978.3~98.83.1~7.585.2~99.12.2~3.479.8~99.03.3~6.482.0~98.61.5~4.377.9~99.71.4~7.283.2~99.82.6~6.20.3073.7~97.32.5~5.573.7~90.01.9~4.876.7~99.02.9~7.274.7~101.01.8~6.476.7~96.32.7~4.873.7~95.71.2~5.2序号参数添加浓度（mg/kg）中华鳖梭子蟹青蟹大黄鱼沼虾草鱼回收率范精密度范回收率范精密度范回收率范精密度范回收率范精密度范回收率范精密度范围（%）回收率范精密度范16氟甲腈0.0375.3~110.02.3~6.676.0~107.71.9~6.977.0~108.72.0~5.479.0~106.02.3~9.373.3~109.73.1~6.781.0~107.31.9~5.80.0982.1~98.41.7~5.684.3~99.32.0~3.882.0~98.71.1~6.283.9~101.84.4~4.875.1~97.31.4~8.682.9~102.32.2~6.40.3075.7~98.30.8~3.372.7~98.01.5~3.975.0~98.01.5~6.671.7~97.71.1~5.575.0~96.01.6~4.173.7~102.32.0~3.517甲氰菊酯0.0381.3~102.31.7~5.673.3~109.31.9~8.176.3~109.31.8~6.675.3~103.72.0~8.075.0~114.01.9~8.678.0~106.02.0~6.80.0976.1~99.91.9~6.375.3~99.10.7~8.778.2~99.21.3~8.581.4~99.71.6~6.675.4~106.31.7~8.179.1~100.81.6~7.50.3080.0~104.32.7~4.877.3~103.71.5~4.578.3~110.31.9~7.481.0~102.00.9~5.475.0~105.71.3~5.778.0~103.71.3~3.918联苯菊酯0.0376.3~101.72.4~6.281.0~98.32.9~5.980.0~103.32.8~5.276.7~100.71.9~6.479.0~101.30.9~6.477.7~97.01.8~5.00.0981.9~104.31.5~5.287.6~103.31.6~4.180.9~100.21.2~5.787.6~101.90.8~5.082.0~102.41.7~7.184.2~100.31.7~3.80.3088.7~101.31.0~3.682.0~102.33.1~4.579.0~105.02.0~7.378.3~103.01.1~5.779.0~103.70.5~3.478.3~101.01.0~4.2序号参数添加浓度（mg/kg）中华鳖梭子蟹青蟹大黄鱼沼虾草鱼回收率范精密度范回收率范精密度范回收率范精密度范回收率范精密度范回收率范精密度范围（%）回收率范精密度范19氯氟氰菊酯和高效氯氟氰菊酯0.0377.7~103.32.1~5.575.3~101.03.1~7.475.7~103.35.4~7.078.7~102.03.1~8.771.0~115.72.3~7.775.3~98.01.9~6.40.0972.1~94.91.4~4.076.9~100.62.1~6.477.9~105.62.3~8.776.6~100.62.2~6.176.3~99.61.5~5.481.1~101.41.4~3.80.3078.0~100.01.3~3.378.7~101.31.8~5.176.3~104.32.2~6.775.3~100.30.8~5.774.7~103.71.8~4.978.0~99.32.7~3.720氯菊酯0.0377.3~98.02.5~5.479.0~98.31.2~7.776.0~99.32.7~8.977.0~99.32.6~9.375.7~104.01.7~6.875.7~100.03.9~8.00.0977.2~95.41.8~6.378.8~98.81.7~7.074.3~99.22.1~9.476.7~99.82.0~5.477.2~103.31.2~7.178.1~102.21.6~6.00.3083.0~103.01.8~3.077.0~102.33.8~5.173.0~107.71.6~8.378.0~102.31.5~6.575.0~113.72.5~4.178.0~106.72.5~4.1序号参数添加浓度（mg/kg）中华鳖梭子蟹青蟹大黄鱼沼虾草鱼回收率范精密度范回收率范精密度范回收率范精密度范回收率范精密度范回收率范精密度范围（%）回收率范精密度范21氯氰菊酯和高效氯氰菊酯0.0377.7~100.32.4~5.979.3~101.32.6~8.972.7~99.31.5~6.774.7~100.03.9~6.474.0~97.31.9~8.274.0~94.32.9~6.00.0975.3~91.91.8~5.280.7~109.02.4~6.675.7~110.21.6·8.076.1~94.12.4~7.872.1~96.60.6~5.875.8~98.41.9~6.60.3075.3~95.32.1~5.181.0~104.72.4~7.275.3~106.02.5~7.476.3~97.31.2~5.976.0~101.31.1~8.074.0~100.71.3~4.722马拉硫磷0.0374.3~102.31.1~6.975.0~103.73.1~8.373.3~97.71.7~6.875.3~101.32.7~7.975.3~100.02.1~5.773.3~100.32.0~6.70.0979.0~94.92.2~4.579.8~98.91.8~5.179.1~103.11.3~8.679.8~101.20.7~6.277.3~100.61.0·5.978.7~101.21.7~6.10.3076.3~99.31.8~3.975.0~98.32.5~3.679.7~103.71.5~6.074.3~98.30.8~6.377.7~100.02.3~4.478.0~98.31.1~3.023醚菊酯0.0380.3~100.02.1~4.376.3~97.31.7~6.979.3~98.72.8~5.476.0~103.02.7~7.072.3~101.72.6~7.177.3~99.02.1~5.60.0975.3~90.32.3~3.583.1~98.62.5~5.480.1~100.12.4~6.678.1~98.21.8~5.876.4~97.01.9~5.781.8~95.31.0~4.20.3078.7~96.71.5~3.182.3~99.02.3~4.573.0~101.32.4~8.376.7~99.01.8~6.478.3~99.72.7~3.881.3~99.71.8~4.424醚菌酯0.0382.3~103.32.0~6.381.3~105.01.7·6.875.0~106.71.0~6.578.7~101.71.5~5.473.7~106.00.8~7.376.0~108.33.3~5.90.0980.6~118.21.8~8.388.4~1012.0~2.674.7~99.60.5~5.385.2~101.20.9~5.781.4~99.81.8~7.381.4~99.72.6~5.00.3084.3~101.32.9~5.183.7~102.72.5~5.173.0~104.71.8~6.085.7~101.71.1~5.680.0~101.70.6~3.481.7~102.30.9~2.8序号参数添加浓度（mg/kg）中华鳖梭子蟹青蟹大黄鱼沼虾草鱼回收率范精密度范回收率范精密度范回收率范精密度范回收率范精密度范回收率范精密度范围（%）回收率范精密度范25嘧菌酯0.0378.7~100.71.9~7.275.0~105.03.2~8.071.3~100.33.8~11.482.0~98.71.6~4.874.0~108.34.2~8.077.7~99.32.1~7.70.0973.3~89.71.4~4.175.2~102.72.2~5.473.3~102.13.4~8.574.2~96.12.2~6.072.9~101.02.0~7.277.0~99.03.3~6.00.3076.3~96.72.0~4.973.7~96.02.2~5.880.3~97.01.7~5.876.3~102.01.6~8.177.3~97.01.2~4.577.7~104.02.9~5.826氰戊菊酯和S-氰戊菊酯0.0378.0~101.02.5~4.478.0~98.72.2~8.474.7~100.04.5~8.075.3~98.72.7~7.871.0~98.02.1~7.775.3~99.73.5~8.50.0978.2~97.71.6~6.776.6~103.32.1~8.276.6~98.42.8~5.376.4~99.63.5~5.974.8~100.01.5~7.177.6~99.91.6~4.10.3080.0~98.30.8~5.476.3~100.03.4~4.878.7~100.71.4~7.974.0~1021.9~5.478.3~100.32.6~3.476.7~100.01.8~4.827噻虫嗪0.0378.3~101.32.7~4.171.3~97.33.1~6.671.0~1032.3~8.080.3~108.71.4~8.677.7~109.02.5~8.472.0~100.31.2~6.00.0976.4~95.31.8~5.175.0~101.93.6~6.476.8~95.61.2~8.376.0~103.92.4~6.275.6~110.02.8~7.971.7~98.90.9~6.70.3084.3~102.73.5~6.178.0~1052.4~5.276.7~100.32.3~9.474.3~112.32.5~5.679.7~109.30.7~7.671.0~102.32.6~7.028噻呋酰胺0.0374.0~104.32.8~6.780.7~104.31.9~7.578.0~105.73.6~4.982.7~97.72.6~5.873.7~104.31.6~5.383.7~106.72.2~6.20.0972.4~91.70.7~5.170.6~102.01.1~5.472.6~98.11.9~5.973.4~107.01.7~6.370.1~97.92.3~7.878.1~98.83.0~4.40.3084.3~103.31.6~4.681.0~101.01.4~4.072.3~104.02.2~7.482.7~104.02.5~4.882.7~104.02.4~3.880.0~102.02.0~3.5序号参数添加浓度（mg/kg）中华鳖梭子蟹青蟹大黄鱼沼虾草鱼回收率范精密度范回收率范精密度范回收率范精密度范回收率范精密度范回收率范精密度范围（%）回收率范精密度范29三环唑0.0376.3~100.33.0~3.975.0~103.34.1~9.370.7~102.03.8~8.575.3~100.71.6~7.073.0~111.33.1~6.680.7~111.02.5~5.90.0977.1~97.41.2~4.275.9~101.81.0~3.878.2~100.21.6~7.274.1~101.21.5~3.873.7~107.81.5~8.575.0~100.22.3~4.80.3085.3~107.02.0~3.676.7~109.32.4~4.779.3~108.31.7~6.774.7~105.71.4~4.878.3~113.31.8~4.874.3~108.02.5~4.530三唑醇0.0376.3~100.73.0~5.277.3~103.34.5~7.672.3~102.03.0~5.680.3~99.73.4~5.874.3~100.02.8~6.578.0~105.03.9~8.70.0980.4~94.42.1~5.980.8~95.31.2~4.373.3~98.61.8~9.380.6~106.42.3~7.777.3~99.42.4~8.178.9~98.71.9~6.80.3082.3~104.32.0~5.683.7~103.71.3~6.176.0~108.31.2~6.479.7~103.32.2~5.481.7~103.31.8~4.977.0~101.72.1~4.531三唑磷0.0381.0~102.01.8~5.270.3~102.31.2~8.976.0~103.03.9~6.278.0~100.01.2~7.075.3~103.01.5~7.875.7~100.72.3~5.10.0976.1~96.71.3~2.475.9~107.82.4~9.384.9~102