方法一:氣相色譜雙柱法
原理:試樣用乙腈提取,提取液經固相萃取或分散固相萃取凈化,使用帶火焰光度檢測器的氣相色譜儀檢測,根據雙柱色譜峰的保留時間定性,外標法定量。
| 水 |
| 一級水 |
| 乙腈 |
| CH3CN,75-05-8,分析純 |
| 冰箱 |
| -18°C |
| 容量瓶 |
| 50 mL |
| 冰箱 |
| 0-4°C |
| 丙酮 |
| C3H6O,67-64-1,色譜純 |
| 甲苯 |
| C7H8,108-88-3,色譜純 |
| 硫酸鎂 |
| 無水,MgSO4,7487-88-9,分析純 |
| 氯化鈉 |
| NaCl,7647-14-5,分析純 |
| 乙酸鈉 |
| CH3COONa,127-09-3,分析純 |
| 十八烷基硅烷鍵合硅膠 |
| 40μm-60μmn |
| 聚乙烯瓶 |
| – |
| 樣品篩 |
| 425μm的標準網篩 |
| 燒杯 |
| 150mL |
| 量筒 |
| 100 mL具塞量筒 |
| 燒杯 |
| 100 mL |
| 鋁箔 |
| – |
| 離心管 |
| 15mL刻度離心管 |
| 燒杯 |
| 150mL |
| 量筒 |
| 100mL具塞量筒 |
| 氮氣 |
| – |
| 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-丙基硅烷化硅膠 |
| 40μm~60μm |
| 均質子 |
| 陶瓷均質子,2cm(長)X1cm(外徑) |
| 濾膜 |
| 微孔濾膜有相機,0.22μmX25mm |
| 氣相色譜儀 |
| 配有雙火焰光度檢測器(FPD磷濾光片) |
| 天平 |
| 分析天平,感量0.1mg和0.1g |
| 勻漿機 |
| 高速勻漿機,轉速不低于15000r/min |
| 離心機 |
| 轉速不低于4200r/min |
| 搗碎機 |
| 組織搗碎機 |
| 旋轉蒸發儀 |
| – |
| 氮吹儀 |
| 可控溫 |
| 振蕩器 |
| 渦旋振蕩器 |
| 離心管 |
| 15 mL刻度離心管 |
| 離心管 |
| 10 mL刻度離心管 |
| 氣相色譜柱 |
| B柱:100%聚笨基甲硅氧烷石英毛細管柱,30mX0.53mm(內徑)X1.5μm,或相當者 |
| 錐形瓶 |
| 150mL具塞錐形瓶 |
| 量筒 |
| 100 mL具塞量筒 |
| 燒杯 |
| 100mL |
| 試管 |
| 10ml刻度試管 |
| 燒杯 |
| 150ml |
| 量筒 |
| 100ml具塞量筒 |
| 燒杯 |
| 100ml |
| 雞心瓶 |
| 茄形瓶 |
| 離心管 |
| 10ml |
| 離心管 |
| 50ml塑料 |
| 離心管 |
| 15ml |
| 離心管 |
| 10ml刻度 |
| 氮氣 |
| 純度≥99.999% |
| 氫氣 |
| 燃氣,純度≥99.999% |
| 空氣 |
| 助燃氣 |
| 氣相色譜柱 |
| A柱:50%聚笨基甲硅氧烷石英毛細管柱,30mX0.53mm(內徑)X1.0μm,或相當者 |
方法二:氣相色譜單柱法
原理:試樣用乙腈提取,提取液經固相萃取或分散固相萃取凈化,使用帶火焰光度檢測器的氣相色譜儀檢測,根據色譜峰的保留時間定性,外標法定量。
| 氣相色譜儀 |
| 配有火焰光度檢測FPD磷濾光片,毛細管進樣口 |
| 氣相色譜柱 |
| 50%聚苯基甲基硅氧烷石英毛細管柱,30mx0.53mm(內徑)x1.0μm,或相當者 |
附錄A(資料性附錄)90種有機磷類農藥及其代謝物中英文名稱、CAS號、分子式和分組
| 敵敵畏 |
| dichlorvos,C4H7Cl2O4P,62-73-7,含量≥96%,Ⅰ組 |
| 乙酰甲胺磷 |
| acephate,C4H10NO3PS,30560-19-1,含量≥96%,Ⅰ組 |
| 蟲線磷 |
| Ⅰ組,thionazin,297-97-2,C8H13N2O3PS ,純度≥96% |
| 甲基內吸磷 |
| 甲基異內吸磷,demeton-s-methyl,919-86-8,C6H15O3PS2,純度≥96%,Ⅰ組 |
| 百治磷 |
| dicrotophos,C8H16NO5P,141-66-2,含量≥96%,Ⅰ組n |
| 乙拌磷 |
| disulfoton,C8H19O2PS3,298-04-4,含量≥96%,Ⅰ組 |
| 樂果 |
| Dimethoate,C5H12NO3PS2,60-51-5,含量≥96%,Ⅰ組 |
| 甲基對硫磷 |
| methylparathion,C8H10NO5PS,298-00-0,含量≥96%,Ⅰ組 |
| 毒死蜱 |
| Chlorpyrifos,nC9H11C13NO3PS,2921-88-2,純度≥96%,Ⅰ組 |
| 嘧啶磷 |
| Pirimiphos ethyl,C13H24N3O3PS,23505-41-1,純度≥96%,Ⅰ組 |
| 倍硫磷 |
| Fenthion,C10H15O3PS2,55-38-9,含量≥96%,Ⅰ組 |
| 滅蚜磷 |
| mecarbam,C10H20NO5PS2,2595-54-2,含量≥6%,Ⅰ組 |
| 丙蟲磷 |
| Propaphos,7292-16-2,C13H21O4PS,純度≥96%,Ⅰ組 |
| 抑草磷 |
| Butamifos,C13H21N2O4PS,36335-67-8,純度≥96%,Ⅰ組 |
| 滅菌磷 |
| Ditalimfos,5131-24-8,C12H14NO4PS,純度≥96%,Ⅰ組 |
| 硫丙磷 |
| Sulprofos,C12H19O2PS3,35400-43-2,純度≥96%,Ⅰ組 |
| 三唑磷 |
| triazophos,C12H16N3O3PS,24017-47-8,含量≥96%,Ⅰ組 |
| 莎稗磷 |
| anilofos,64249-01-0,C13H19ClNO3PS2,純度≥96%,Ⅰ組 |
| 亞胺硫磷 |
| Phosmet,C11H12NO4PS2,732-11-6,含量≥6%,Ⅰ組 |
| 滅線磷 |
| Ethoprophos,C8H19O2PS2,13194-48-4,含量≥96%,Ⅱ組 |
| 甲拌磷 |
| phorate,C7H17O2PS3,298-02-2,含量≥96%,Ⅱ組 |
| 氧樂果 |
| omethoate,C5H12NO4PS,1113-02-6,含量≥96%,Ⅱ組 |
| 二嗪磷 |
| Diazinon,333-41-5,C4H4N2O,含量≥96%,Ⅱ組 |
| 地蟲硫磷 |
| Fonofos,C10H15OPS2,944-22-9,含量≥96%,Ⅱ組n |
| 異稻瘟凈 |
| iprobenfos,26087-47-8,C13H21O3PS,純度≥96%,Ⅱ組 |
| 甲基毒死蜱 |
| Chlorpyrifos-methyl,C7H7Cl3NO3PS,5598-13-0,含量≥96%,Ⅱ組 |
| 對氧磷 |
| paraoxon-ethyl,C10H14NO6P,311-45-5,含量≥96%,Ⅱ組 |
| 殺螟硫磷 |
| fenitrothion,C9H12NO5PS,122-14-5,含量≥96%,Ⅱ組 |
| 溴硫磷 |
| Bromophos,C8H8BrCl2O3PS,2104-96-3,含量≥96%,Ⅱ組 |
| 乙基溴硫磷 |
| bromophos,C10H12BrCl2O3PS ,4824-78-6,含量≥96%,Ⅱ組 |
| 巴毒磷 |
| Crotoxyphos,C14H19O6P,7700-17-6,純度≥96%,Ⅱ組 |
| 丙溴磷 |
| Profenofos,C11H15BrClO3PS,CAS號:41198-08-7,純度≥96%,Ⅱ組 |
| 乙拌磷砜 |
| disulfotonnsulfone,2497-06-5,C8H19O4PS3,純度≥96%,Ⅱ組 |
| 乙硫磷 |
| ethion,C9H22O4P2S4,563-12-2,含量≥96%,Ⅱ組 |
| 溴苯磷 |
| Leptophos,C33H48O6,21609-90-5,含量≥96%,Ⅱ組 |
| 吡菌磷 |
| Pyrazophos,C14H20N3O5PS,13457-18-6,純度≥96%,Ⅱ組 |
| 甲胺磷 |
| Methamidophos,C2H8NO2PS,10265-92-6,含量≥96%,Ⅲ組 |
| 治螟磷 |
| sulfotep,3689-24-5,C8H20O6P2S,純度≥96%,Ⅲ組 |
| 特丁硫磷 |
| Terbufos ,C9H21O2PS3,13071-79-9,含量≥96%,Ⅲ組 |
| 久效磷 |
| Monocrotophos,C7H14NO5P,6923-22-4,含量≥96%,Ⅲ組 |
| 除線磷 |
| dichlofenthion,C10H13Cl2O3PS,97-17-6,含量≥96%,Ⅲ組 |
| 皮蠅磷 |
| ronnel(fenchlorphos),C8H8Cl3O3PS,299-84-3,含量≥96%,Ⅲ組 |
| 甲基嘧啶磷 |
| pirimiphosmethyl,C11H20N3O3PS,29232-93-7,含量≥96%,Ⅲ組 |
| 對硫磷 |
| Parathion,C10H14NO5PS,56-38-2,含量≥96%,Ⅲ組 |
| 異柳磷 |
| ISOFENPHOS,C15H24NO4PS,25311-71-1,含量≥96%,Ⅲ組 |
| 脫葉亞磷 |
| 脫葉亞磷,Merphos,C12H27PS3,150-50-5,純度≥96%,Ⅲ組n |
| 殺撲磷 |
| methidathion,C6H11N2O4PS3,950-37-8,含量≥96%,Ⅲ組 |
| 蟲螨磷 |
| Chlorthiophos,60238-56-4,C11H15Cl2O3PS2,純度≥96%,Ⅲ組 |
| 伐滅磷 |
| Famphur,C10H16NO5PS2,52-85-7,含量≥96%,Ⅲ組 |
| 哌草磷 |
| Piperophos,C14H28NO3PS2,24151-93-7,純度≥96%,Ⅲ組 |
| 伏殺硫磷 |
| phosalone,C28H25O8F,2310-17-0,純度≥96%,Ⅲ組 |
| 益棉磷 |
| Azinphos-ethyl,C12H16N3O3PS2,2642-71-9,含量≥96%,Ⅲ組 |
| 速滅磷 |
| Mevinphos,C7H13O6P,7786-34-7,含量≥96%,Ⅳ組 |
| 胺丙畏 |
| Propetamphos,C12H20NO4PS,31218-83-4,含量≥96%,Ⅳ組 |
| 八甲磷 |
| SCHRADAN,152-16-9,C8H24N4O3P2,純度≥96%,Ⅳ組 |
| 磷胺 |
| phosphamidon I,C10H19ClNO5P ,13171-21-6,含量≥96%,Ⅳ組n |
| 毒壤磷 |
| Trichloronat,C10H12Cl3O2PS,327-98-0,含量≥96%,Ⅳ組 |
| 馬拉硫磷 |
| malathion,C10H19O6PS2,121-75-5,含量≥96%,Ⅳ組 |
| 甲拌磷亞砜 |
| PHORATE SULFOXIDE,2588-05-8,C7H17O4PS2,純度≥96%,Ⅳ組 |
| 水胺硫磷 |
| Isocarbophos,C11H16NO4PS,24353-61-5,含量≥96%,Ⅳ組 |
| 喹硫磷 |
| Quinalphos,C12H15N2O3PS,13593-03-8,含量≥96%,Ⅳ組 |
| 丙硫磷 |
| Prothiophos,C11H15Cl2O2PS2,34643-46-4,含量≥96%,Ⅳ組 |
| 殺蟲畏 |
| tetrachlorvinphos,C10H9Cl4O4P,22248-79-9,含量≥96%,Ⅳ組 |
| 苯線磷 |
| fenamiphos,22224-92-6,C13H22NO3PS,純度≥96%,Ⅳ組 |
| 甲基硫環磷 |
| Phosphfolan-methyl,5120-23-0,C5H10NO3PS2 ,純度≥96%,Ⅳ組 |
| 三硫磷 |
| Carbofenothion,C11H16ClO2PS3,786-19-6,含量≥96%,Ⅳ組 |
| 苯硫磷 |
| EPN,C14H14NO4PS,2104-64-5,含量≥96%,Ⅳ組 |
| 苯線磷亞砜 |
| fenamiphosnsulfoxide,31972-43-7,C13H22NO4PS,純度≥96%,Ⅳ組 |
| 乙拌磷亞砜 |
| disulfoton-sulfoxnide,2497-07-6,C8H19O3PS3,純度≥96%,V組 |
| 硫趕內吸磷 |
| 內吸磷-S,demeton-s,126-75-0,純度≥96%,Ⅴ組 |
| 內吸磷-O |
| DEMETON O,C8H19O3PS2,298-03-3,,純度≥96%,Ⅴ組 |
| 乙嘧硫磷 |
| etrimfos,C10H17N2O4PS,38260-54-7,含量≥96%,Ⅴ組 |
| 氯唑磷 |
| isazofos,42509-80-8,C9H17ClN3O3PS,純度≥96%,Ⅴ組 |
| 甲基立枯磷 |
| Tolclofos-methyl,C9H11Cl2O3PS,57018-04-9,含量≥96%,Ⅴ組 |
| 甲基異柳磷 |
| Isofenphos-methyl,99675-03-3,C14H22NO4PS,純度≥96%,Ⅴ組 |
| 特丁硫磷砜 |
| terbufossulfone,56070-16-7,C9H21O4PS3,純度≥96%,Ⅴ組 |
| 噻唑硫磷 |
| fosthiazate,98886-44-3,C9H18NO3PS2,純度≥96%,Ⅴ組 |
| 溴苯烯磷 |
| Bromfenvinfos,33399-00-7,C12H14BrCl2O4P,純度≥96%,Ⅴ組 |
| 蚜滅磷 |
| vamidothion,2275-23-2,C8H18NO4PS2,純度≥96%,Ⅴ組 |
| 豐索磷 |
| Fensulfothion,C11H17O4PS2,115-90-2,含量≥96%,Ⅴ組 |
| 倍硫磷砜 |
| fenthion sulfone,3761-42-0,C10H15O5PS2,純度≥96%,Ⅴ組 |
| 甲基吡啶磷 |
| azamethiphos,C9H10ClN2O5PS,35575-96-3,含量≥96%,Ⅴ組 |
| 噠嗪硫磷 |
| pyridaphenthion,119-12-0,C14H17N2O4PS,純度≥96%,Ⅴ組 |
| 保棉磷 |
| azinphos-methyl,C10H12N3O3PS2,86-50-0,含量≥96%,Ⅴ組 |
| 蠅毒磷 |
| Coumaphos,C14H16ClO5PS,56-72-4,含量≥96%,Ⅴ組 |
| 吡唑硫磷 |
| pyraclofos,C14H18ClN2O3PS,89784-60-1,純度≥96%,Ⅵ組 |
| 甲基內吸磷 |
| Demeton methyl ,8022-00-2,2C6H15O3PS2,,純度≥96%,Ⅵ組 |
| 硫線磷 |
| cadusafos,C10H28O2PS2 ,95465-99-9,含量≥96%,Ⅵ組 |
| 丁基嘧啶磷 |
| tebupirimfos,96182-53-5,C13H23N2O3PS,純度≥96%,Ⅵ組 |
| 敵噁磷 |
| Dioxathion,C12H26O6P2S4,78-34-2,含量≥936%,Ⅵ組 |
| 甲基對氧磷 |
| Paraoxon-methyl,950-35-6,C8H10NO6P,純度≥96%,Ⅵ組 |
| 安硫磷 |
| Formothion,2540-82-1,C6H12NO4PS2,純度≥96%,Ⅵ組 |
| 氧異柳磷 |
| Isofenphos oxon,31120-85-1,C15H24NO5P,純度≥96%,Ⅵ組 |
| 甲拌磷砜 |
| phorate sulfone,2588-04-7,C7H17O4PS3,純度≥96%,Ⅵ組n |
| 稻豐散 |
| phenthoate,C12H17O4PS2,2597-03-7,含量≥96%,Ⅵ組 |
| 碘硫磷 |
| Iodofenphos,C8H8Cl2IO3PS,18181-70-9,含量≥96%,Ⅵ組 |
| 噁唑磷 |
| Isoxathion,C13H16NO4PS,18854-01-8,含量≥96%,Ⅵ組 |
| 硫環磷 |
| Phosfolan,C7H14NO3PS2 ,947-02-4,含量≥96%,Ⅵ組 |
| 倍硫磷亞砜 |
| fenthion sulfoxide,3761-41-9,C10H15O4PS2,純度≥95%,Ⅵ組 |
| 敵瘟磷 |
| Edifenphos,C14H15O2PS2,17109-49-8,含量≥96%,Ⅵ組 |
| 苯線磷砜 |
| fenamiphosnsulfone,31972-44-8,C13H22NO5PS,純度≥96%,Ⅵ組 |











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