2341农药残留量测定法

2020年版第一次征求意见稿“略”表示与2015年版相应内容一致2341农药残留量测定法本方法系用气相色谱法（通则0521）和质谱法（通则0431）测定药材、饮片及制剂中部分农药残留量。除另有规定外，按下列方法测定。第一法有机氯类农药残留量测定法-色谱法略限度除另有规定外，每1kg中药材或饮片中含总六六六（α-BHC，β-BHC，γ-BHC，δ-BHC之和）不得过0.2mg；总滴滴涕（p，p’-DDE，p，p’-DDD，o，p’-DDT，p，p’-DDT之和）不得过0.2mg；五氯硝基苯（Quintozene）不得过0.1mg；六氯苯（Hexachlorobenzene）不得过0.1mg；七氯（Heptachlor）、顺式环氧七氯（Heptachlor-exo-epoxide）和反式环氧七氯（Heptachlor-endo-epoxide）之和不得过0.05mg；艾氏剂（Aldrin）和狄氏剂（Dieldrin）之和不得过0.05mg；异狄氏剂（Endrin）不得过0.05mg；顺式氯丹（cis-Chlordane）、反式氯丹（trans-Chlordane）和氧化氯丹（oxy-Chlordane）之和不得过0.05mg；α-硫丹（α-Endosulfan）、β-硫丹（β-Endosulfan）和硫丹硫酸盐（Endosulfansulfate）之和不得过3mg。【附注】（1）当供试品中有农药检出时，可在验证柱中确认检出的结果，再进行定量。必要时，可用气相色谱-质谱法对检出的结果用气相色谱质谱联用法进行确证。（2）加样回收率应在70％～120％之间。（3）限度参考值除另有规定外，每1kg中药材或饮片中含总六六六（α-BHC，β-BHC，γ-BHC，δ-BHC之和）不得过0.2mg；总滴滴涕（p，p’-DDE，p，p’-DDD，o，p’-DDT，p，p’-DDT之和）不得过0.2mg；五氯硝基苯（Quintozene）不得过0.1mg；六氯苯（Hexachlorobenzene）不得过0.1mg；七氯（Heptachlor）、顺式环氧七氯（Heptachlor-exo-epoxide）和反式环氧七氯（Heptachlor-endo-epoxide）之和不得过0.05mg；艾氏剂（Aldrin）和狄氏剂（Dieldrin）之和不得过0.05mg；异狄氏剂（Endrin）不得过0.05mg；顺式氯丹（cis-Chlordane）、反式氯丹（trans-Chlordane）和氧化氯丹（oxy-Chlordane）之和不得过0.05mg；α-硫丹（α-Endosulfan）、β-硫丹（β-Endosulfan）和硫丹硫酸盐（Endosulfansulfate）之和不得过3mg。2020年版第一次征求意见稿“略”表示与2015年版相应内容一致第二法有机磷类农药残留量测定法-色谱法略第三法拟除虫菊酯类农药残留量测定法-色谱法略第四法农药多残留量测定法-质谱法一、定性测定方法本法系用气相色谱质谱联用法与液相色谱质谱联用法对中药中农药残留的快速定性筛查，发现残留农药，便于农药定量测定。实验室应建立必要的质控手段，保证定性结果准确。1.气相色谱质谱联用法色谱条件以5%苯基甲基聚硅氧烷为固定液的弹性石英毛细管柱（30m×0.25mm×0.25μm色谱柱）。进样口温度240℃，不分流进样。载气为高纯氦气（He）。进样口为恒压模式，柱前压力为146kPa（可依据表2中农药保留时间调整柱前压力）。程序升温：初始温度70℃，保持2分钟，先以每分钟25℃升温至150℃，再以每分钟3℃升温至200℃，最后以每分钟8℃升温至280℃，保持10分钟。质谱条件以三重四极杆串联质谱仪检测；离子源为电子轰击源（EI），离子源温度230℃。碰撞气为氮气或氩气，流速1.5ml/min。质谱传输接口温度280℃。质谱监测模式为多反应监测（MRM），各化合物参考保留时间、监测离子对、碰撞电压（CE）与检出限参考值见表2。为提高检测灵敏度，可根据保留时间分段监测各农药。表291种农药及内标对照品的保留时间、监测离子对、碰撞电压（CE）与检出限参考值编号中文名英文名保留时间（min）母离子子离子CE(V)检出限（mg/kg）1氟丙菊酯Acrinathrin30.4207.8181.1100.005181.0152.0302艾氏剂Aldrin18.5262.9192.9350.01254.9220.020264.9192.935262.9190.9353氘代莠去津Atrazine-d5(ethyl-d5)13.1205.0127.010_2020年版第一次征求意见稿“略”表示与2015年版相应内容一致205.0105.0154α-六六六α-BHC12.1216.9181.150.005181.1145.115219.0183.055β-六六六β-BHC13.2219.0183.050.005216.9181.15181.0145.0156γ-六六六γ-BHC(Lindane)13.4219.0183.050.005216.9181.15181.1145.1157δ-六六六δ-BHC14.6216.9181.150.005181.1145.115219.0183.05217.0145.020219.0147.0158联苯菊酯Bifenthrin28.9181.0166.0200.005181.0165.0259乙基溴硫磷Bromophos-ethyl22.6358.7302.8150.005302.8284.71510溴硫磷Bromophos-methyl20.1330.8315.8150.005328.8313.81511溴螨酯Bromopropylate28.6341.0185.0300.005341.0183.01512#仲丁灵#Butralin20.2266.0220.2100.05266.0174.22013顺式氯丹Chlordane-cis22.8271.9236.9150.005372.9265.92014氧化氯丹Chlordane-oxy20.7386.7262.7150.005184.985.03015反式氯丹Chlordane-trans22.0372.8265.8150.005374.8265.81516杀虫脒Chlordimeform11.2195.9181.050.025151.9117.110180.9140.015195.9152.01517溴虫腈Chlorfenapyr25.3246.9227.0150.01327.8246.81518百菌清Chlorothalonil14.8263.8229.0200.025263.8168.02519#毒死蜱#Chlorpyrifos19.3313.8285.850.005313.8257.81520#甲基毒死蜱#Chlorpyrifos-methyl16.7286.0271.0150.0052020年版第一次征求意见稿“略”表示与2015年版相应内容一致286.093.02021氯酞酸二甲酯Chlorthal-dimethyl19.4300.9223.0250.005298.9221.02522氟氯氰菊酯Cyfluthrin32.3，32.4163.0127.050.025226.0206.01223氯氟氰菊酯Cyhalothrin30.4208.0181.050.005197.0141.01024氯氰菊酯Cypermethrin32.7，32.9181.0152.0100.025181.0127.03025o,p'-滴滴滴o,p'-DDD24.4237.0165.2200.005235.0165.22026p,p'-滴滴滴p,p'-DDD25.7237.0165.2200.005235.0165.220234.9199.115199.0163.13027o,p'-滴滴伊o,p'-DDE22.5248.0176.2300.005246.0176.23028p,p'-滴滴伊p,p'-DDE24.0246.1176.2300.005315.8246.015317.8248.015317.8246.01529o,p'-滴滴涕o,p'-DDT25.8237.0165.2200.005235.0165.220237.0199.115235.0199.115199.0163.13530p,p'-滴滴涕p,p'-DDT27.0237.0165.2200.005235.0165.22031溴氰菊酯Deltamethrin36.0181.0152.1250.025252.7174.0832氘代二嗪磷Diazinon-d10(diethyl-d10)14.3314.9184.215_183.8168.92033苯氟磺胺Dichlofluanid18.4223.9123.1100.01123.077.12034敌敌畏Dichlorvos5.9184.993.0100.005109.079.0535氯硝胺Dicloran12.6206.1176.0100.0052020年版第一次征求意见稿“略”表示与2015年版相应内容一致206.0148.02036三氯杀螨醇Dicofol19.2139.0111.0150.01251.0139.010250.0215.0337狄氏剂Dieldrin23.9277.0241.050.01262.9193.035345.0262.7538#苯醚甲环唑#Difenoconazole35.3322.8264.8150.005264.9202.02039哌草丹Dimepiperate21.6144.9112.150.01144.969.11540二苯胺Diphenylamine10.5169.0168.2150.005169.0140.03541α-硫丹α-Endosulfan22.6194.9159.050.01276.7241.915236.8118.925194.9125.020262.8192.930236.8142.93042β－硫丹β-Endosulfan25.2206.9172.0150.01267.0196.014236.8118.830194.9158.910276.7240.9543硫丹硫酸盐Endosulfansulfate26.8271.9237.0150.01387.0289.04273.8238.91544异狄氏剂Endrin24.7262.8193.0350.01244.8173.03045#皮蝇磷#Fenchlorphos17.4286.0271.0150.005285.0269.91546#氧皮蝇磷#Fenchlorphosoxon15.8268.9254.0150.01270.9256.01547杀螟硫磷Fenitrothion18.2277.0109.0150.01260.0125.01048甲氰菊酯Fenpropathrin29.0265.0210.080.005208.0181.0549氘代倍硫磷Fenthion-d6(o,o-dimethyl-d6)19.0284.0169.015_284.0115.02050氰戊菊酯Fenvalerate34.3，34.7167.0125.150.0252020年版第一次征求意见稿“略”表示与2015年版相应内容一致225.0119.01851#氟虫腈#Fipronil21.9366.8212.8350.005350.8254.815368.8214.825254.9228.01552#氟甲腈#Fipronildesulfinyl17.4388.0332.9200.005388.0281.03253#氟虫腈亚砜#Fipronilsulfide21.4351.0254.9200.005420.0350.910254.9227.915351.0227.93554#氟虫腈砜#Fipronilsulfone24.8384.8