方法一:气相色谱双柱法
原理:试样用乙腈提取,提取液经固相萃取或分散固相萃取净化,使用带火焰光度检测器的气相色谱仪检测,根据双柱色谱峰的保留时间定性,外标法定量。
| 水 |
| 一级水 |
| 乙腈 |
| CH3CN,75-05-8,分析纯 |
| 冰箱 |
| -18°C |
| 容量瓶 |
| 50 mL |
| 冰箱 |
| 0-4°C |
| 丙酮 |
| C3H6O,67-64-1,色谱纯 |
| 甲苯 |
| C7H8,108-88-3,色谱纯 |
| 硫酸镁 |
| 无水,MgSO4,7487-88-9,分析纯 |
| 氯化钠 |
| NaCl,7647-14-5,分析纯 |
| 乙酸钠 |
| CH3COONa,127-09-3,分析纯 |
| 十八烷基硅烷键合硅胶 |
| 40μm-60μmn |
| 聚乙烯瓶 |
| – |
| 样品筛 |
| 425μm的标准网筛 |
| 烧杯 |
| 150mL |
| 量筒 |
| 100 mL具塞量筒 |
| 烧杯 |
| 100 mL |
| 铝箔 |
| – |
| 离心管 |
| 15mL刻度离心管 |
| 烧杯 |
| 150mL |
| 量筒 |
| 100mL具塞量筒 |
| 氮气 |
| – |
| 固相萃取柱 |
| 石墨化碳黑填料(GCB)500/mg氨基填料(NH2)500mg,6mL |
| 乙二胺-N-丙基硅烷化硅胶 |
| 40μm~60μm |
| 均质子 |
| 陶瓷均质子,2cm(长)X1cm(外径) |
| 滤膜 |
| 微孔滤膜有相机,0.22μmX25mm |
| 气相色谱仪 |
| 配有双火焰光度检测器(FPD磷滤光片) |
| 天平 |
| 分析天平,感量0.1mg和0.1g |
| 匀浆机 |
| 高速匀浆机,转速不低于15000r/min |
| 离心机 |
| 转速不低于4200r/min |
| 捣碎机 |
| 组织捣碎机 |
| 旋转蒸发仪 |
| – |
| 氮吹仪 |
| 可控温 |
| 振荡器 |
| 涡旋振荡器 |
| 离心管 |
| 15 mL刻度离心管 |
| 离心管 |
| 10 mL刻度离心管 |
| 气相色谱柱 |
| B柱:100%聚笨基甲硅氧烷石英毛细管柱,30mX0.53mm(内径)X1.5μm,或相当者 |
| 锥形瓶 |
| 150mL具塞锥形瓶 |
| 量筒 |
| 100 mL具塞量筒 |
| 烧杯 |
| 100mL |
| 试管 |
| 10ml刻度试管 |
| 烧杯 |
| 150ml |
| 量筒 |
| 100ml具塞量筒 |
| 烧杯 |
| 100ml |
| 鸡心瓶 |
| 茄形瓶 |
| 离心管 |
| 10ml |
| 离心管 |
| 50ml塑料 |
| 离心管 |
| 15ml |
| 离心管 |
| 10ml刻度 |
| 氮气 |
| 纯度≥99.999% |
| 氢气 |
| 燃气,纯度≥99.999% |
| 空气 |
| 助燃气 |
| 气相色谱柱 |
| A柱:50%聚笨基甲硅氧烷石英毛细管柱,30mX0.53mm(内径)X1.0μm,或相当者 |
方法二:气相色谱单柱法
原理:试样用乙腈提取,提取液经固相萃取或分散固相萃取净化,使用带火焰光度检测器的气相色谱仪检测,根据色谱峰的保留时间定性,外标法定量。
| 气相色谱仪 |
| 配有火焰光度检测FPD磷滤光片,毛细管进样口 |
| 气相色谱柱 |
| 50%聚苯基甲基硅氧烷石英毛细管柱,30mx0.53mm(内径)x1.0μm,或相当者 |
附录A(资料性附录)90种有机磷类农药及其代谢物中英文名称、CAS号、分子式和分组
| 敌敌畏 |
| dichlorvos,C4H7Cl2O4P,62-73-7,含量≥96%,Ⅰ组 |
| 乙酰甲胺磷 |
| acephate,C4H10NO3PS,30560-19-1,含量≥96%,Ⅰ组 |
| 虫线磷 |
| Ⅰ组,thionazin,297-97-2,C8H13N2O3PS ,纯度≥96% |
| 甲基内吸磷 |
| 甲基异内吸磷,demeton-s-methyl,919-86-8,C6H15O3PS2,纯度≥96%,Ⅰ组 |
| 百治磷 |
| dicrotophos,C8H16NO5P,141-66-2,含量≥96%,Ⅰ组n |
| 乙拌磷 |
| disulfoton,C8H19O2PS3,298-04-4,含量≥96%,Ⅰ组 |
| 乐果 |
| Dimethoate,C5H12NO3PS2,60-51-5,含量≥96%,Ⅰ组 |
| 甲基对硫磷 |
| methylparathion,C8H10NO5PS,298-00-0,含量≥96%,Ⅰ组 |
| 毒死蜱 |
| Chlorpyrifos,nC9H11C13NO3PS,2921-88-2,纯度≥96%,Ⅰ组 |
| 嘧啶磷 |
| Pirimiphos ethyl,C13H24N3O3PS,23505-41-1,纯度≥96%,Ⅰ组 |
| 倍硫磷 |
| Fenthion,C10H15O3PS2,55-38-9,含量≥96%,Ⅰ组 |
| 灭蚜磷 |
| mecarbam,C10H20NO5PS2,2595-54-2,含量≥6%,Ⅰ组 |
| 丙虫磷 |
| Propaphos,7292-16-2,C13H21O4PS,纯度≥96%,Ⅰ组 |
| 抑草磷 |
| Butamifos,C13H21N2O4PS,36335-67-8,纯度≥96%,Ⅰ组 |
| 灭菌磷 |
| Ditalimfos,5131-24-8,C12H14NO4PS,纯度≥96%,Ⅰ组 |
| 硫丙磷 |
| Sulprofos,C12H19O2PS3,35400-43-2,纯度≥96%,Ⅰ组 |
| 三唑磷 |
| triazophos,C12H16N3O3PS,24017-47-8,含量≥96%,Ⅰ组 |
| 莎稗磷 |
| anilofos,64249-01-0,C13H19ClNO3PS2,纯度≥96%,Ⅰ组 |
| 亚胺硫磷 |
| Phosmet,C11H12NO4PS2,732-11-6,含量≥6%,Ⅰ组 |
| 灭线磷 |
| Ethoprophos,C8H19O2PS2,13194-48-4,含量≥96%,Ⅱ组 |
| 甲拌磷 |
| phorate,C7H17O2PS3,298-02-2,含量≥96%,Ⅱ组 |
| 氧乐果 |
| omethoate,C5H12NO4PS,1113-02-6,含量≥96%,Ⅱ组 |
| 二嗪磷 |
| Diazinon,333-41-5,C4H4N2O,含量≥96%,Ⅱ组 |
| 地虫硫磷 |
| Fonofos,C10H15OPS2,944-22-9,含量≥96%,Ⅱ组n |
| 异稻瘟净 |
| iprobenfos,26087-47-8,C13H21O3PS,纯度≥96%,Ⅱ组 |
| 甲基毒死蜱 |
| Chlorpyrifos-methyl,C7H7Cl3NO3PS,5598-13-0,含量≥96%,Ⅱ组 |
| 对氧磷 |
| paraoxon-ethyl,C10H14NO6P,311-45-5,含量≥96%,Ⅱ组 |
| 杀螟硫磷 |
| fenitrothion,C9H12NO5PS,122-14-5,含量≥96%,Ⅱ组 |
| 溴硫磷 |
| Bromophos,C8H8BrCl2O3PS,2104-96-3,含量≥96%,Ⅱ组 |
| 乙基溴硫磷 |
| bromophos,C10H12BrCl2O3PS ,4824-78-6,含量≥96%,Ⅱ组 |
| 巴毒磷 |
| Crotoxyphos,C14H19O6P,7700-17-6,纯度≥96%,Ⅱ组 |
| 丙溴磷 |
| Profenofos,C11H15BrClO3PS,CAS号:41198-08-7,纯度≥96%,Ⅱ组 |
| 乙拌磷砜 |
| disulfotonnsulfone,2497-06-5,C8H19O4PS3,纯度≥96%,Ⅱ组 |
| 乙硫磷 |
| ethion,C9H22O4P2S4,563-12-2,含量≥96%,Ⅱ组 |
| 溴苯磷 |
| Leptophos,C33H48O6,21609-90-5,含量≥96%,Ⅱ组 |
| 吡菌磷 |
| Pyrazophos,C14H20N3O5PS,13457-18-6,纯度≥96%,Ⅱ组 |
| 甲胺磷 |
| Methamidophos,C2H8NO2PS,10265-92-6,含量≥96%,Ⅲ组 |
| 治螟磷 |
| sulfotep,3689-24-5,C8H20O6P2S,纯度≥96%,Ⅲ组 |
| 特丁硫磷 |
| Terbufos ,C9H21O2PS3,13071-79-9,含量≥96%,Ⅲ组 |
| 久效磷 |
| Monocrotophos,C7H14NO5P,6923-22-4,含量≥96%,Ⅲ组 |
| 除线磷 |
| dichlofenthion,C10H13Cl2O3PS,97-17-6,含量≥96%,Ⅲ组 |
| 皮蝇磷 |
| ronnel(fenchlorphos),C8H8Cl3O3PS,299-84-3,含量≥96%,Ⅲ组 |
| 甲基嘧啶磷 |
| pirimiphosmethyl,C11H20N3O3PS,29232-93-7,含量≥96%,Ⅲ组 |
| 对硫磷 |
| Parathion,C10H14NO5PS,56-38-2,含量≥96%,Ⅲ组 |
| 异柳磷 |
| ISOFENPHOS,C15H24NO4PS,25311-71-1,含量≥96%,Ⅲ组 |
| 脱叶亚磷 |
| 脱叶亚磷,Merphos,C12H27PS3,150-50-5,纯度≥96%,Ⅲ组n |
| 杀扑磷 |
| methidathion,C6H11N2O4PS3,950-37-8,含量≥96%,Ⅲ组 |
| 虫螨磷 |
| Chlorthiophos,60238-56-4,C11H15Cl2O3PS2,纯度≥96%,Ⅲ组 |
| 伐灭磷 |
| Famphur,C10H16NO5PS2,52-85-7,含量≥96%,Ⅲ组 |
| 哌草磷 |
| Piperophos,C14H28NO3PS2,24151-93-7,纯度≥96%,Ⅲ组 |
| 伏杀硫磷 |
| phosalone,C28H25O8F,2310-17-0,纯度≥96%,Ⅲ组 |
| 益棉磷 |
| Azinphos-ethyl,C12H16N3O3PS2,2642-71-9,含量≥96%,Ⅲ组 |
| 速灭磷 |
| Mevinphos,C7H13O6P,7786-34-7,含量≥96%,Ⅳ组 |
| 胺丙畏 |
| Propetamphos,C12H20NO4PS,31218-83-4,含量≥96%,Ⅳ组 |
| 八甲磷 |
| SCHRADAN,152-16-9,C8H24N4O3P2,纯度≥96%,Ⅳ组 |
| 磷胺 |
| phosphamidon I,C10H19ClNO5P ,13171-21-6,含量≥96%,Ⅳ组n |
| 毒壤磷 |
| Trichloronat,C10H12Cl3O2PS,327-98-0,含量≥96%,Ⅳ组 |
| 马拉硫磷 |
| malathion,C10H19O6PS2,121-75-5,含量≥96%,Ⅳ组 |
| 甲拌磷亚砜 |
| PHORATE SULFOXIDE,2588-05-8,C7H17O4PS2,纯度≥96%,Ⅳ组 |
| 水胺硫磷 |
| Isocarbophos,C11H16NO4PS,24353-61-5,含量≥96%,Ⅳ组 |
| 喹硫磷 |
| Quinalphos,C12H15N2O3PS,13593-03-8,含量≥96%,Ⅳ组 |
| 丙硫磷 |
| Prothiophos,C11H15Cl2O2PS2,34643-46-4,含量≥96%,Ⅳ组 |
| 杀虫畏 |
| tetrachlorvinphos,C10H9Cl4O4P,22248-79-9,含量≥96%,Ⅳ组 |
| 苯线磷 |
| fenamiphos,22224-92-6,C13H22NO3PS,纯度≥96%,Ⅳ组 |
| 甲基硫环磷 |
| Phosphfolan-methyl,5120-23-0,C5H10NO3PS2 ,纯度≥96%,Ⅳ组 |
| 三硫磷 |
| Carbofenothion,C11H16ClO2PS3,786-19-6,含量≥96%,Ⅳ组 |
| 苯硫磷 |
| EPN,C14H14NO4PS,2104-64-5,含量≥96%,Ⅳ组 |
| 苯线磷亚砜 |
| fenamiphosnsulfoxide,31972-43-7,C13H22NO4PS,纯度≥96%,Ⅳ组 |
| 乙拌磷亚砜 |
| disulfoton-sulfoxnide,2497-07-6,C8H19O3PS3,纯度≥96%,V组 |
| 硫赶内吸磷 |
| 内吸磷-S,demeton-s,126-75-0,纯度≥96%,Ⅴ组 |
| 内吸磷-O |
| DEMETON O,C8H19O3PS2,298-03-3,,纯度≥96%,Ⅴ组 |
| 乙嘧硫磷 |
| etrimfos,C10H17N2O4PS,38260-54-7,含量≥96%,Ⅴ组 |
| 氯唑磷 |
| isazofos,42509-80-8,C9H17ClN3O3PS,纯度≥96%,Ⅴ组 |
| 甲基立枯磷 |
| Tolclofos-methyl,C9H11Cl2O3PS,57018-04-9,含量≥96%,Ⅴ组 |
| 甲基异柳磷 |
| Isofenphos-methyl,99675-03-3,C14H22NO4PS,纯度≥96%,Ⅴ组 |
| 特丁硫磷砜 |
| terbufossulfone,56070-16-7,C9H21O4PS3,纯度≥96%,Ⅴ组 |
| 噻唑硫磷 |
| fosthiazate,98886-44-3,C9H18NO3PS2,纯度≥96%,Ⅴ组 |
| 溴苯烯磷 |
| Bromfenvinfos,33399-00-7,C12H14BrCl2O4P,纯度≥96%,Ⅴ组 |
| 蚜灭磷 |
| vamidothion,2275-23-2,C8H18NO4PS2,纯度≥96%,Ⅴ组 |
| 丰索磷 |
| Fensulfothion,C11H17O4PS2,115-90-2,含量≥96%,Ⅴ组 |
| 倍硫磷砜 |
| fenthion sulfone,3761-42-0,C10H15O5PS2,纯度≥96%,Ⅴ组 |
| 甲基吡啶磷 |
| azamethiphos,C9H10ClN2O5PS,35575-96-3,含量≥96%,Ⅴ组 |
| 哒嗪硫磷 |
| pyridaphenthion,119-12-0,C14H17N2O4PS,纯度≥96%,Ⅴ组 |
| 保棉磷 |
| azinphos-methyl,C10H12N3O3PS2,86-50-0,含量≥96%,Ⅴ组 |
| 蝇毒磷 |
| Coumaphos,C14H16ClO5PS,56-72-4,含量≥96%,Ⅴ组 |
| 吡唑硫磷 |
| pyraclofos,C14H18ClN2O3PS,89784-60-1,纯度≥96%,Ⅵ组 |
| 甲基内吸磷 |
| Demeton methyl ,8022-00-2,2C6H15O3PS2,,纯度≥96%,Ⅵ组 |
| 硫线磷 |
| cadusafos,C10H28O2PS2 ,95465-99-9,含量≥96%,Ⅵ组 |
| 丁基嘧啶磷 |
| tebupirimfos,96182-53-5,C13H23N2O3PS,纯度≥96%,Ⅵ组 |
| 敌噁磷 |
| Dioxathion,C12H26O6P2S4,78-34-2,含量≥936%,Ⅵ组 |
| 甲基对氧磷 |
| Paraoxon-methyl,950-35-6,C8H10NO6P,纯度≥96%,Ⅵ组 |
| 安硫磷 |
| Formothion,2540-82-1,C6H12NO4PS2,纯度≥96%,Ⅵ组 |
| 氧异柳磷 |
| Isofenphos oxon,31120-85-1,C15H24NO5P,纯度≥96%,Ⅵ组 |
| 甲拌磷砜 |
| phorate sulfone,2588-04-7,C7H17O4PS3,纯度≥96%,Ⅵ组n |
| 稻丰散 |
| phenthoate,C12H17O4PS2,2597-03-7,含量≥96%,Ⅵ组 |
| 碘硫磷 |
| Iodofenphos,C8H8Cl2IO3PS,18181-70-9,含量≥96%,Ⅵ组 |
| 噁唑磷 |
| Isoxathion,C13H16NO4PS,18854-01-8,含量≥96%,Ⅵ组 |
| 硫环磷 |
| Phosfolan,C7H14NO3PS2 ,947-02-4,含量≥96%,Ⅵ组 |
| 倍硫磷亚砜 |
| fenthion sulfoxide,3761-41-9,C10H15O4PS2,纯度≥95%,Ⅵ组 |
| 敌瘟磷 |
| Edifenphos,C14H15O2PS2,17109-49-8,含量≥96%,Ⅵ组 |
| 苯线磷砜 |
| fenamiphosnsulfone,31972-44-8,C13H22NO5PS,纯度≥96%,Ⅵ组 |











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