水質(zhì)100種農(nóng)藥殘留的測定 固相萃取-高效液相色譜-串聯(lián)質(zhì)譜法

附錄B（資料性附錄）目標化合物的測定參考參數(shù)表B.1給出了100種農(nóng)藥及內(nèi)標物的保留時間、定量內(nèi)標、多離子反應(yīng)監(jiān)測條件等測定參考參數(shù)。表B.1100種農(nóng)藥及內(nèi)標物的保留時間、定量內(nèi)標、多離子反應(yīng)監(jiān)測條件等測定參考參數(shù)中文名稱英文名稱保留時間（min）采集模式母離子（m/z）定量子離子定性子離子定量內(nèi)標m/z碰撞能/evm/z碰撞能/ev呋蟲胺Dinotefuran6.057ESI+203.1129.112113.110吡蟲啉-D4噻蟲嗪Thiamethoxam7.946ESI+292.0211.111181.123噻蟲胺Clothianidin9.132ESI+250.0169.112132.014吡蟲啉Imidacloprid9.706ESI+256.1175.117209.114啶蟲脒Acetamiprid10.484ESI+223.1126.11556.022噻蟲啉Thiacloprid12.559ESI+253.0126.12099.043氧樂果Omethoate4.861ESI+214.1183.010155.014樂果-D6砜吸磷MethylmercaptophosOxide6.602ESI+247.0169.015109.030蚜滅磷Vamidothion8.332ESI+287.8118.135146.126樂果Dimethoate10.16ESI+230.0199.09125.022磷胺Phosphamidon12.53ESI+300.0174.112127.029甲拌磷亞砜Phorate-Sulfoxide17.938ESI+277.0199.01096.934甲拌磷砜Phorate-Sulfone22.159ESI+293.0171.19115.024滅線磷Ethoprophos24.913ESI+243.1131.02097.032三唑磷Triazophos27.526ESI+314.1162.219119.235地散磷Bensulide31.435ESI+398.0158.120314.05甲基毒蟲畏Dimethylvinphos32.488ESI+331.1127.020219.910雙氟磺草胺Florasulam17.562ESI+360.1129.123109.154雙酰草胺呋吡菌胺Furametpyr18.392ESI+334.1157.020290.010氯蟲苯甲酰胺Chlorantraniliprole21.113ESI+484.0452.919285.916解草嗪Benoxacor23.956ESI+260.0149.116134.132環(huán)酰菌胺Fenhexamid24.857ESI+301.997.12355.140氟唑菌酰胺Fluxapyroxad25.172ESI+382.0362.114342.121敵草胺Napropamide25.709ESI+272.2129.216171.117甲草胺Alachlor27.261ESI+270.1238.110162.219氟酰胺Flutolanil27.527ESI+324.1262.125242.020四唑酰草胺Fentrazamide31.709ESI+372.1219.01083.235環(huán)氟菌胺Cyflufenamid33.483ESI+413.2241.020223.022多菌靈Carbendazim6.295ESI+192.1160.117132.130抑霉唑-D5噻菌靈Thiabendazole6.703ESI+202.0175.124131.133麥穗靈Fuberidazole6.898ESI+185.2157.22092.125抑霉唑Imazalil13.173ESI+297.0159.024201.018十二環(huán)嗎啉Dodemorph15.609ESI+282.3116.01898.028嘧霉胺Pyrimethanil17.618ESI+200.1107.025168.129烯酰嗎啉Dimethomorph21.219ESI+388.1301.020165.134嘧菌環(huán)胺Cyprodinil21.452ESI+226.193.134108.127咪鮮胺Prochloraz22.354ESI+376.0308.011266.017辛噻酮Octhilinone23.574ESI+214.0102.01071.015嘧菌胺Mepanipyrim26.01ESI+224.2106.02577.030霜霉威Propamocarb3.981ESI+189.2102.120144.112克百威-D3涕滅威亞砜AldicarbSulfoxide5.662ESI+229.0166.111109.116殺線威Oxamyl6.866ESI+242.072.120129.111乙硫苯威亞砜EthiofencarbSulfoxide7.692ESI+242.2107.115185.153-羥基克百威3-Hydroxy-Carbofuran9.163ESI+238.1163.114181.2106-氯-4-羥-3-苯基-噠嗪Pyridafol10.67ESI+207.177.025104.035硫雙威Thiodicarb16.446ESI+355.188.120108.116克百威Carbofuran16.903ESI+222.1165.111123.121甲萘威Carbaryl18.187ESI+202.0145.113126.926異丙威Isoprocarb19.695ESI+194.195.014137.1103，4，5-混殺威3,4,5-Trimethacarb19.889ESI+194.2137.25122.220仲丁威Fenobucarb22.366ESI+208.195.113152.39甲硫威Methiocarb22.401ESI+226.1169.110121.118野燕枯difenzoquat10.05ESI+249.1193.130130.040敵草隆-D6特丁隆Tebuthiuron12.147ESI+229.1172.115116.125甲草苯隆Methibenzuron16.93ESI+222.2165.115149.935綠麥隆Chlorotoluron17.729ESI+213.172.021140.123異丙隆Isoproturon18.807ESI+207.172.021165.113綠谷隆Monolinuron19.006ESI+215.1126.015148.110敵草隆Diuron19.044ESI+233.072.021160.126利谷隆Linuron23.14ESI+249.0160.117182.114枯草隆Chloroxuron23.662ESI+291.272.120218.130可滅隆Cumyluron24.559ESI+303.1185.112125.132戊菌隆Pencycuron32.479ESI+329.1125.126218.115噁霜靈Oxadixyl13.797ESI+279.1219.111133.121氯酯磺草胺滅草喹Imazaquin14.435ESI+312.2199.125267.020甲磺隆MetsulfuronMethyl16.477ESI+382.1167.116141.115甲霜靈Metalaxyl18.578ESI+280.1220.213192.218抗倒酯Trinexapac-Ethyl20.473ESI+253.1207.115164.915乙蟲清Ethiprole22.459ESI+396.9350.820254.835螺蟲乙酯Spirotetramat22.801ESI+374.0302.017330.015環(huán)酯草醚Pyriftalid24.654ESI+319.0139.135179.035嘧菌酯Azoxystrobin24.755ESI+404.1372.114329.031甲氧蟲酰肼Methoxyfenozide26.619ESI+369.2149.116313.18稻瘟靈Isoprothiolane27.05ESI+291.1231.111189.121氟嘧菌酯Fluoxastrobin28.004ESI+459.4427.125188.135蟲酰肼Tebufenozide28.882ESI+353.2133.120297.18吡蚜酮Pymetrozine3.906ESI+218.1105.12078.144特丁津-D5二甲嘧酚Dimethirimol7.443ESI+210.2140.12171.131乙嘧酚Ethirimol7.491ESI+210.2140.02298.126苯嗪草酮Metamitron8.903ESI+203.1175.018104.023異戊乙凈Dimethametryn20.146ESI+256.1186.12568.145嗪草酸甲酯Fluthiacet-Methyl28.899ESI+403.9214.835273.835三環(huán)唑Tricyclazole10.644ESI+190.0163.021136.026硅氟唑三唑醇Triadimenol21.282ESI+296.170.11199.215多效唑Paclobutrazol21.603ESI+294.170.121125.140滅菌唑Triticonazole22.083ESI+318.170.121125.139腈菌唑Myclobutanil24.185ESI+289.170.121125.130三唑酮Triadimefon24.979ESI+294.169.222197.115戊唑醇Tebuconazole25.479ESI+308.170.122125.038芐氯三唑醇Diclobutrazol25.55ESI+328.070.022159.021己唑醇Hexaconazole26.277ESI+314.170.221159.229唑草胺Cafenstrole27.409ESI+373.0100.02572.025丙環(huán)唑Propiconazole27.56ESI+342.1159.130205.118烯唑醇Diniconazole27.561ESI+326.170.025159.030芐草唑Pyrazoxyfen28.232ESI+403.091.034105.0222,4-D2,4-Dichlorophenoxyaceticacid18.812ESI-219.0161.111125.026碘苯腈二甲四氯MCPA18.945ESI-199.1141.112105.128綠草定Triclopyr19.98ESI-254.0196.010198.025除蟲脲Diflubenzuron26.662ESI-309.1289.18156.210滅幼脲Chlorbenzuron27.727ESI-307.0154.211126.222吡蟲啉-D4Imidacloprid-D49.645ESI+260.2179.320213.215-樂果-D6Dimethoate-D610.085ESI+236.0205.05131.020雙酰草胺Carbetamide12.803ESI+237.1192.15118.110抑霉唑-D5Imazalil-D513.082ESI+302.2158.91469.014克百威-D3Carbofuran-D316.825ESI+224.9165.211123.221敵草隆-D6Diuron-D618.927ESI+239.078.11252.212氯酯磺草胺CloransulaMMethyl20.538ESI+430.0370.020153.040特丁津-D5Terbutylazine-D522.29ESI+235.1179.115101.015硅氟唑Simeconazole23.534ESI+294.170.121135.121碘苯腈Ioxynil21.234ESI-369.8126.946215.035附錄C（資料性附錄）100種農(nóng)藥及內(nèi)標物的總離子流圖圖C.1給出了100種農(nóng)藥及內(nèi)標物的總離子流圖。1：吡嗪酮；2：霜霉威；3：氧樂果；4：涕滅威亞砜；5：呋蟲胺；6：多菌靈；7：砜吸磷；8：噻菌靈；9：殺線威；10：麥穗靈；11：二甲嘧酚；12：乙嘧酚；13：乙硫苯威亞砜；14：噻蟲嗪；15：蚜滅磷；16：苯嗪草酮；17：噻蟲胺；18：3-羥基克百威；19：內(nèi)標物：吡蟲啉-D4；20：吡蟲啉；21：野燕枯；22：內(nèi)標物：樂果-D6；23：樂果；24：啶蟲脒；25：三環(huán)唑；26：6-氯-4-羥-3-苯基-噠嗪；27：特丁?。?8：磷胺；29：噻蟲啉；30：內(nèi)標物：雙酰草胺；31：內(nèi)標物：抑霉唑-D5；32：抑霉唑；33：噁霜靈；34：滅草喹；35：十二環(huán)嗎啉；36：硫雙威；37：甲磺??；38：內(nèi)標物：克百威-D3；39：克百威；40：甲草苯??；41：雙氟磺草胺；42：嘧霉胺；43：綠麥?。?4：甲拌磷亞砜；45：甲萘威。（1）第一段1：呋吡菌胺；2：甲霜靈；3：異丙?。?：2,4-D；5：內(nèi)標物：敵草隆-D6；6：二甲四氯；7：綠谷??；8：敵草隆；9：異丙威；10：3,4,5-混殺威；11：綠草定；12：異戊乙凈；13：抗倒酯；14：內(nèi)標物：氯酯磺草胺；15：氯蟲苯甲酰胺；16：烯酰嗎啉；17：內(nèi)標物：碘苯腈；18：三唑醇；19：嘧菌環(huán)胺；20：多效唑；21：滅菌唑；22：甲拌磷砜；23：內(nèi)標物：特丁津-D5；24：仲丁威；25：咪鮮胺；26：甲硫威；27：乙蟲清；28：螺蟲乙酯；29：利谷隆；30：內(nèi)標物：硅氟唑；31：辛噻酮；32：枯草??；33：解草嗪；34：腈菌唑；35：可滅??；36：環(huán)酯草醚；37：嘧菌酯；38：環(huán)酰菌胺；39：滅線磷；40：三唑酮；41：氟唑菌酰胺；42：戊唑醇；43：芐氯三唑醇；44：敵草胺；45：嘧菌胺；46：己唑醇；47：甲氧蟲酰肼；48：除蟲脲。（2）第二段1：稻瘟靈；2：甲草胺；3：唑草胺；4：三唑磷；5：氟酰胺；6：丙環(huán)唑；7：烯唑醇；8：滅幼脲；9：氟嘧菌酯；10：蟲酰肼；11：芐草唑；12：嗪草酸甲酯；13：地散磷；14：四唑酰草胺；15：戊菌??；16：甲基毒蟲畏；17：環(huán)氟菌胺。圖C.1100種農(nóng)藥（ρ=50μg/L）及內(nèi)標物（ρ=20μg/L）的總離子流圖附錄D（資料性附錄）方法的精密度和正確度表D.1～D.6給出了方法的精密度和正確度匯總數(shù)據(jù)。表D.1精密度匯總表（空白水樣）序號目標化合物加標濃度（ng/L）實驗室內(nèi)相對標準偏差（%）實驗室間相對標準偏差（%）重復(fù)性限（ng/L）再現(xiàn)性限（ng/L）1呋蟲胺5.004.3~8.33.86.86.820.06.7~116.49.09.01001.5~4.73.83.55.22噻蟲嗪5.002.0~8.57.45.65.620.01.8~115.97.17.11001.8~8.22.55.55.73噻蟲胺5.004.4~8.34.46.36.320.03.5~4.90.64.14.11001.9~4.74.03.65.34吡蟲啉5.004.9~106.87.47.420.05.5~106.37.67.61002.6~7.77.45.59.35啶蟲脒5.006.2~9.9138.88.820.04.3~8.59.96.56.51002.6~4.82.03.63.96噻蟲啉5.009.0~1216111120.03.1~6.9125.65.71001.2~6.82.64.65.17氧樂果5.006.8~112.39.79.720.03.3~158.39.79.71002.8~4.6143.8138砜吸磷5.004.8~11128.78.720.04.2~148.59.69.61001.9~7.06.45.28.39蚜滅磷5.004.5~8.0186.56.520.03.9~8.1136.06.01005.1~6.5206.01810樂果5.004.8~11157.97.920.06.7~128.09.69.61001.6~5.36.54.27.311磷胺5.007.3~135.4111120.07.1~8.5197.87.81003.3~7.63.65.25.812甲拌磷亞砜5.003.2~12168.78.720.04.4~7.64.95.75.71002.6~4.27.23.78.113甲拌磷砜5.007.6~1620121220.03.8~5.66.94.94.91003.5~8.57.35.98.814滅線磷5.007.5~8.09.27.77.720.04.5~9.2207.17.11002.2~7.6155.61415三唑磷5.006.1~145.6111120.03.2~5.4114.74.71002.9~5.94.04.55.216地散磷5.0011~1312121220.03.3~4.1203.74.61002.2~8.86.95.97.317甲基毒蟲畏5.006.1~117.48.28.220.04.9~5.58.95.15.11001.8~6.3114.18.018雙氟磺草胺5.004.2~7.77.35.95.920.05.8~8.00.66.86.81001.2~6.73.94.35.419呋吡菌胺5.007.9~11168.98.920.06.4~8.29.87.57.51002.8~4.27.83.48.420氯蟲苯甲酰胺5.009.4~1212121220.05.4~9.13.57.17.11002.1~7.05.74.96.721解草嗪5.009.3~1316121220.02.6~6.71.34.94.91003.2~7.3196.01522環(huán)酰菌胺5.0011~158.8121220.06.0~9.73.97.67.61003.0~3.77.13.46.723氟唑菌酰胺5.009.5~1412121220.02.9~9.72.66.96.91002.6~4.38.83.58.724敵草胺5.006.4~1619121220.03.0~5.25.44.14.11002.5~3.85.33.15.025甲草胺5.0011~1419131320.04.6~8.6146.36.31003.6~5.5194.41626氟酰胺5.002.3~5.18.33.63.620.06.5~9.18.78.08.01002.4~2.96.72.86.027四唑酰草胺5.006.0~7.70.76.76.720.04.7~8.00.76.16.11002.6~6.0174.11528環(huán)氟菌胺5.005.8~8.6117.47.420.03.3~7.4165.65.81003.4~7.5195.61629多菌靈5.004.4~8.15.46.46.420.03.8~133.58.58.51003.4~8.4175.81830噻菌靈5.005.4~7.0196.06.020.04.9~122.37.67.61006.9~8.16.47.79.731麥穗靈5.006.7~172.9121220.03.6~7.95.06.16.11002.6~5.6164.11732抑霉唑5.007.0~1315111120.06.5~9.8148.18.11002.7~6.54.04.86.033十二環(huán)嗎啉5.006.3~1614111120.07.5~10178.88.81002.8~4.3183.61434嘧霉胺5.007.1~9.41.68.28.220.07.2~7.6207.47.71004.6~5.2174.91735烯酰嗎啉5.009.0~127.4111120.03.6~6.56.65.65.61004.7~7.77.36.21036嘧菌環(huán)胺5.009.6~149.9121220.04.2~9.15.17.37.31000.9~4.85.13.96.137咪鮮胺5.008.4~144.1131320.06.2~139.99.99.91002.5~5.74.94.16.138辛噻酮5.006.2~13189.59.520.07.0~8.5188.08.01002.3~5.28.34.29.239嘧菌胺5.004.7~6.97.46.16.120.04.3~7.57.36.36.31001.9~6.23.74.25.740霜霉威5.007.0~9.83.48.38.320.07.7~12199.69.61001.3~6.2144.01241涕滅威亞砜5.005.8~144.0111120.07.6~141211111001.5~5.4123.71342殺線威5.006.1~159.69.89.820.05.8~12128.48.41002.4~5.67.14.58.743乙硫苯威亞砜5.009.2~1219111120.03.8~11128.18.11002.4~4.36.33.46.8443-羥基克百威5.0012~141.8131320.06.6~125.89.79.71003.4~5.08.94.010456-氯-4-羥-3-苯基-噠嗪5.004.4~119.78.38.320.06.8~9.2148.18.11002.0~7.14.85.27.046硫雙威5.0012~1813151520.05.2~8.66.87.07.01000.8~5.73.34.65.447克百威5.0010~176.9151520.05.7~143.39.79.71003.0~3.74.73.35.648甲萘威5.009.0~1315121220.08.7~151813131002.5~4.53.63.35.149異丙威5.002.9~117.78.28.220.04.7~117.98.58.51001.7~6.5154.113503,4,5-混殺威5.007.7~13119.89.820.01.8~123.67.67.61004.0~5.00.94.54.551仲丁威5.006.3~8.4137.77.720.05.2~131.88.48.41003.1~9.4166.11352甲硫威5.006.2~137.89.29.220.06.3~9.5157.97.91001.8~2.66.52.26.253野燕枯5.005.5~7.7176.56.520.05.0~7.00.86.36.31002.6~9.89.76.51154特丁隆5.004.7~11137.57.520.04.8~124.48.18.11002.5~6.2124.61255甲草苯隆5.006.0~106.28.58.520.06.8~9.85.68.08.01002.2~7.1125.11156綠麥隆5.006.8~9.07.77.97.920.02.9~9.84.88.08.01002.8~7.62.05.55.557異丙隆5.008.3~12179.89.820.04.6~6.4115.35.31005.0~5.8115.51258綠谷隆5.005.6~123.69.59.520.02.7~119.68.38.31003.2~5.2164.51359敵草隆5.006.4~127.29.99.920.02.3~9.4117.57.51002.5~4.54.23.85.260利谷隆5.007.2~125.49.09.020.02.3~6.2174.55.21002.4~5.58.04.37.761枯草隆5.005.2~7.8146.26.220.04.9~11129.09.01001.7~5.97.34.77.462可滅隆5.008.0~9.5208.78.720.04.1~111.28.18.11001.7~4.7113.91063戊菌隆5.003.1~11106.96.920.06.5~7.5196.96.91003.6~7.49.95.58.264噁霜靈5.005.6~1511131320.02.4~116.07.77.71003.5~7.55.25.37.165滅草喹5.004.6~14119.29.220.05.4~13128.58.51002.1~4.96.73.67.666甲磺隆5.005.9~13169.59.520.04.6~12177.87.81004.5~4.6194.61767甲霜靈5.005.3~129.39.49.420.03.9~15199.69.61002.2~4.75.43.86.368抗倒酯5.006.3~11179.19.120.08.0~121811111003.4~4.09.53.79.869乙蟲清5.003.4~12138.78.720.09.0~116.99.69.61002.1~3.53.03.14.270螺蟲乙酯5.002.9~149.6111120.05.4~153.79.69.61002.9~3.98.23.68.771環(huán)酯草醚5.007.9~143.9111120.04.2~9.23.66.86.81001.7~6.14.73.85.772嘧菌酯5.005.4~14119.99.920.05.6~8.40.87.07.01003.2~6.33.64.95.673甲氧蟲酰肼5.006.1~1513111120.07.3~115.09.39.31002.6~7.08.24.69.574稻瘟靈5.005.2~135.99.39.320.05.2~8.36.77.17.11002.7~5.48.33.98.375氟嘧菌酯5.004.3~1418111120.04.4~168.711111002.7~6.1114.41176蟲酰肼5.008.3~8.8188.68.620.07.1~9.46.18.18.11001.4~4.94.73.25.177吡蚜酮5.008.2~1320101020.06.8~7.6207.37.51002.6~6.4124.81378二甲嘧酚5.002.1~195.4121220.02.9~6.5124.95.11002.6~4.15.83.57.179乙嘧酚5.007.5~1712131320.02.5~7.78.45.25.21002.4~9.32.66.36.580苯嗪草酮5.0013~154.3141420.04.4~146.19.59.51002.2~6.3125.11481異戊乙凈5.008.9~11159.59.520.02.6~6.79.94.74.71001.7~7.44.25.56.782嗪草酸甲酯5.003.4~5.85.65.15.120.06.2~9.39.68.38.31002.7~4.7143.61383三環(huán)唑5.008.3~1412111120.05.5~8.35.77.17.11002.0~11146.91684三唑醇5.006.2~160.210.81120.05.6~113.58.88.81001.4~3.7122.61385多效唑5.007.1~9.49.28.68.620.08.0~129.810101002.5~4.15.33.36.886滅菌唑5.005.1~149.69.49.420.04.8~12129.69.61002.6~6.71.25.15.187腈菌唑5.005.3~9.00.86.96.920.04.5~8.9127.27.21002.6~3.5153.11688三唑酮5.004.2~7.20.45.55.520.06.4~142.611111003.0~5.86.54.27.989戊唑醇5.001.6~9.8116.36.320.02.9~9.6167.37.31003.2~6.63.94.86.290芐氯三唑醇5.002.8~8.75.36.36.320.05.6~9.7128.18.11002.5~5.72.54.24.791己唑醇5.003.6~117.87.27.220.05.3~12189.49.41001.6~4.08.73.49.292唑草胺5.008.2~11119.19.120.02.8~125.57.77.71001.9~5.48.03.99.193丙環(huán)唑5.002.5~133.67.77.720.05.0~112.18.68.61002.0~4.92.63.34.294烯唑醇5.007.6~112.09.49.420.06.2~12178.58.51002.2~6.63.05.15.595芐草唑5.003.1~123.27.87.820.06.6~8.2187.57.51002.6~3.27.42.97.3962,4-D5.004.9~8.22.26.76.720.03.4~8.1126.26.21001.8~8.7186.01897二甲四氯5.003.8~1511121220.03.9~9.7177.17.11003.4~7.7155.21598綠草定5.006.9~138.3111120.06.1~11109.09.01002.4~3.9133.11499除蟲脲5.008.1~11109.29.220.05.9~11168.68.61004.2~6.1124.912100滅幼脲5.006.0~112.37.97.920.05.4~9.77.28.28.21003.2~7.14.75.86.9表D.2精密度匯總表（地表水、地下水和海水）序號目標化合物加標濃度（ng/L）實驗室內(nèi)相對標準偏差（%）地表水地下水海水1呋蟲胺5.0016~1911~188.7~1720.08.1~204.3~8.81.6~131005.4~9.34.8~111.8~7.22噻蟲嗪5.006.3~208.5~189.6~1520.05.5~112.3~121.1~111004.7~125.1~9.42.3~6.13噻蟲胺5.006.1~137.3~1811~1820.07.1~9.81.8~8.26.4~8.91004.5~112.3~112.6~5.34吡蟲啉5.002.3~1611~1912~1720.06.7~129.5~133.1~181006.8~8.83.1~8.22.3~5.15啶蟲脒5.004.0~8.26.7~8.84.7~1220.07.0~127.2~127.4~7.91004.6~7.43.7~111.2~5.36噻蟲啉5.008.0~147.1~137.8~1620.07.1~125.8~112.8~9.91003.0~7.95.1~122.0~4.17氧樂果5.005.6~186.3~125.4~1420.05.3~125.9~147.4~141004.9~7.23.5~8.91.4~4.78砜吸磷5.008.4~168.9~157.1~1820.08.7~145.8~158.7~111003.3~6.73.7~124.2~8.99蚜滅磷5.008.0~1512~148.0~1720.08.0~134.2~116.5~111001.1~7.50.8~113.1~9.510樂果5.006.4~169.0~157.3~1320.05.9~154.0~9.94.7~9.61002.5~7.22.6~152.4~1111磷胺5.009.9~117.2~183.0~1220.06.7~154.6~135.5~9.51003.1~6.70.8~111.4~8.112甲拌磷亞砜5.007.5~116.2~9.09.6~1520.03.8~8.69.6~128.6~111006.4~8.01.6~9.91.8~8.413甲拌磷砜5.005.1~133.5~146.5~1320.07.5~126.3~126.7~141004.5~6.62.0~131.6~6.514滅線磷5.004.4~6.85.4~177.7~9.020.04.1~165.6~125.7~121002.3~8.04.5~143.0~1115三唑磷5.005.2~164.8~168.3~1320.06.7~144.5~126.8~8.51003.3~7.91.9~4.91.2~8.216地散磷5.004.2~9.38.9~177.3~1720.05.1~124.1~176.8~141002.9~9.22.0~8.43.0~1117甲基毒蟲畏5.003.8~169.5~149.2~1520.04.9~163.2~143.3~6.31005.4~6.33.3~121.2~5.718雙氟磺草胺5.009.7~1511~1411~1320.03.6~113.5~122.9~9.11003.1~132.4~5.61.1~3.819呋吡菌胺5.008.3~9.92.4~177.0~1920.07.3~8.14.8~8.88.0~111003.3~8.91.8~122.2~5.720氯蟲苯甲酰胺5.007.8~133.9~174.5~1520.05.2~9.84.7~176.0~7.71002.4~111.5~7.23.3~5.621解草嗪5.006.5~153.5~176.6~1420.07.7~176.1~9.93.3~8.61003.4~7.94.1~6.71.7~4.222環(huán)酰菌胺5.008.8~197.0~1411~1220.03.4~152.9~135.6~121004.5~9.41.5~9.42.3~5.723氟唑菌酰胺5.0011~188.1~153.1~1320.03.6~115.2~7.96.0~121002.0~112.1~7.31.2~4.524敵草胺5.007.0~147.3~164.2~1220.05.0~8.65.5~173.7~141002.4~9.52.8~111.5~5.125甲草胺5.0011~155.4~9.711~1320.04.5~123.9~164.2~111002.5~9.62.2~6.71.8~7.026氟酰胺5.006.8~159.3~128.3~1420.05.4~115.5~163.8~121001.9~6.70.8~8.22.8~3.927四唑酰草胺5.004.4~109.6~165.0~1220.03.5~134.4~144.6~141004.2~9.13.7~6.23.2~6.428環(huán)氟菌胺5.0011~129.1~157.9~1420.05.7~163.9~162.8~6.91002.6~111.5~5.91.8~6.929多菌靈5.007.7~2014~165.5~1120.07.6~173.0~146.1~121004.6~9.72.6~7.12.4~1130噻菌靈5.006.5~1213~166.4~1120.05.8~175.1~142.4~7.21002.4~6.92.9~6.92.4~3.731麥穗靈5.005.9~149.0~169.3~1220.08.8~113.6~116.3~161004.7~154.2~111.7~8.832抑霉唑5.005.7~126.4~1211~1320.02.6~9.94.8~112.5~131003.7~8.45.0~6.22.2~6.733十二環(huán)嗎啉5.006.1~145.6~116.0~1620.03.5~125.6~113.2~8.51001.5~7.61.6~111.9~4.434嘧霉胺5.004.1~117.1~116.8~1720.07.7~122.8~9.43.8~131002.9~9.83.0~8.91.3~6.035烯酰嗎啉5.006.5~2013~195.0~1620.03.5~144.0~143.2~121005.8~111.9~4.71.3~8.636嘧菌環(huán)胺5.007.0~118.8~167.1~1420.04.2~175.4~110.9~151001.9~6.72.1~113.3~5.737咪鮮胺5.007.6~149.5~155.9~1120.09.4~174.5~129.2~131003.2~7.96.5~9.23.1~4.738辛噻酮5.004.4~137.3~159.2~1220.06.9~9.15.2~112.7~131004.2~9.22.5~112.6~4.139嘧菌胺5.005.9~169.4~156.4~8.120.05.2~146.9~134.1~131002.7~121.8~9.72.8~5.540霜霉威5.005.7~8.97.1~179.2~1320.06.2~8.63.2~133.9~151003.5~6.63.3~8.04.2~6.241涕滅威亞砜5.008.6~137.2~137.9~1120.04.7~7.91.8~116.2~111008.0~104.6~6.71.7~4.442殺線威5.005.1~145.6~116.6~1020.06.1~9.12.8~6.62.8~121005.8~6.64.0~7.54.4~6.343乙硫苯威亞砜5.005.4~178.7~174.1~1520.09.2~111.9~9.65.6~111004.5~8.43.5~122.6~6.5443-羥基克百威5.007.6~168.5~136.0~1420.08.0~156.3~7.85.4~141004.5~7.93.9~8.92.7~5.2456-氯-4-羥-3-苯基-噠嗪5.007.7~159.7~125.9~1320.06.0~157.1~114.5~141004.2~7.33.3~7.31.9~2.346硫雙威5.003.5~134.3~144.8~6.520.03.7~116.3~7.95.2~141003.4~7.04.1~113.5~5.747克百威5.008.7~1711~176.9~1120.02.6~116.7~115.9~121005.4~9.65.5~6.91.8~4.348甲萘威5.004.0~134.8~8.75.5~1720.07.5~132.4~7.64.1~8.31005.9~113.2~5.83.9~7.649異丙威5.006.7~173.8~8.45.4~9.820.08.7~148.9~114.4~121003.3~6.33.6~5.42.8~8.7503,4,5-混殺威5.008.6~129.9~145.2~9.620.06.2~136.3~8.95.7~121004.2~6.35.5~112.0~7.951仲丁威5.006.1~1112~166.4~1320.09.7~163.4~8.33.7~171003.4~5.64.3~7.92.3~8.652甲硫威5.007.4~169.5~144.8~1420.011~126.1~8.37.7~8.61005.0~8.33.1~8.12.2~6.553野燕枯5.0012~1510.7~147.5~1220.06.1~114.8~153.2~111005.0~8.03.3~6.61.9~9.454特丁隆5.004.1~167.8~1312~1420.04.6~127.1~122.0~141003.5~111.8~121.9~7.355甲草苯隆5.0017~1911~1511~1520.04.1~175.3~152.6~131003.3~5.02.3~9.42.3~5.956綠麥隆5.0012~136.9~138.6~1620.08.0~136.3~135.6~121003.1~8.22.7~131.7~1257異丙隆5.008.5~137.9~148.4~1520.04.3~114.9~8.61.6~9.01004.6~8.32.9~4.91.5~9.358綠谷隆5.009.9~1712~148.0~1620.05.3~135.5~155.2~111003.8~8.41.3~9.81.3~9.059敵草隆5.008.6~1511~1511~1820.04.1~8.86.8~114.4~111004.0~6.93.0~8.12.1~1160利谷隆5.0011~158.5~159.1~1520.07.8~8.74.2~5.23.5~131003.0~8.61.8~7.62.2~7.661枯草隆5.007.1~9.57.9~139.8~1620.04.4~115.1~135.6~8.51004.2~6.61.2~8.12.3~7.562可滅隆5.004.9~1313~1513~1520.03.8~166.0~162.3~111002.8~6.31.7~8.11.2~3.563戊菌隆5.005.8~136.4~149.0~1220.06.1~117.9~123.4~111003.5~7.91.8~9.91.8~2.864噁霜靈5.009.0~155.0~1111~2020.07.5~117.0~7.84.5~191002.4~6.74.8~8.02.8~1565滅草喹5.0011~146.4~115.7~1120.04.8~157.6~142.7~121001.6~7.83.2~9.82.2~1566甲磺隆5.0011~145.1~149.3~1420.09.6~155.8~136.1~151003.9~4.73.5~9.52.3~1367甲霜靈5.005.7~128.2~1911~1620.04.0~7.26.8~8.45.1~141002.6~5.43.4~8.02.8~1268抗倒酯5.005.7~127.7~165.9~9.320.08.0~127.8~144.8~161002.6~6.05.1~132.5~1269乙蟲清5.0012~176.3~154.2~1320.04.5~156.3~177.8~8.91004.6~8.15.2~9.81.3~1370螺蟲乙酯5.0012~1514~193.2~1120.03.4~127.0~9.74.9~9.51001.9~4.92.9~7.91.2~1271環(huán)酯草醚5.007.3~157.2~148.0~1220.00.8~117.1~8.84.7~161001.5~5.74.6~131.8~1472嘧菌酯5.004.5~144.5~203.9~1320.02.1~176.6~116.6~101001.3~114.4~9.12.8~1473甲氧蟲酰肼5.006.9~1112.0~145.3~1320.04.3~125.3~136.8~161002.8~5.93.4~8.61.9~1574稻瘟靈5.008.0~197.0~124.7~6.620.02.5~206.3~119.2~141002.2~9.94.1~121.1~1475氟嘧菌酯5.0011.6~146.1~137.8~1520.02.6~137.5~117.1~8.51001.3~114.7~102.6~1576蟲酰肼5.009.5~155.0~135.2~1220.07.0~117.6~9.74.0~141001.3~7.53.8~8.41.5~1377吡蚜酮5.007.0~169.8~196.7~1420.011.0~164.9~9.83.8~131002.8~115.5~121.6~7.178二甲嘧酚5.009.1~153.5~122.6~1120.04.0~173.5~124.2~111003.8~8.86.1~112.6~9.679乙嘧酚5.005.2~116.9~113.2~1320.03.9~153.8~112.5~151003.9~9.14.2~132.1~6.280苯嗪草酮5.007.3~176.8~145.3~1520.02.8~187.4~186.1~151002.6~6.85.4~7.22.0~1181異戊乙凈5.006.5~176.2~134.3~1120.04.4~185.5~144.7~131003.7~115.2~112.4~9.882嗪草酸甲酯5.006.9~177.1~165.2~1220.03.3~172.3~112.4~121002.8~8.95.5~8.31.9~5.283三環(huán)唑5.005.7~174.9~112.9~1520.010.1~172.5~135.6~131003.6~122.9~5.61.1~9.184三唑醇5.006.4~129.0~139.3~1420.06.8~116.7~9.57.3~131000.6~122.0~132.2~6.285多效唑5.008.3~169.6~168.9~1720.07.6~112.7~116.7~171002.2~144.5~8.21.7~6.986滅菌唑5.0010.2~166.7~1411~1520.03.4~126.2~154.2~8.91004.4~122.9~6.41.5~7.487腈菌唑5.008.3~1113~1414~1520.012~156.5~127.3~141004.5~9.74.5~9.51.3~7.688三唑酮5.005.5~1412~148.9~1620.09.8~107.2~8.87.6~131004.8~8.64.3~103.1~5.989戊唑醇5.008.8~195.0~1511~1520.07.0~176.5~125.4~161004.0~9.43.3~7.82.0~3.290芐氯三唑醇5.006.1~173.4~137.8~9.720.06.9~176.0~157.0~111003.9~134.2~132.9~6.791己唑醇5.008.1~159.3~1411~1820.09.3~166.0~6.27.0~131006.1~143.6~112.6~7.592唑草胺5.005.5~166.8~138.9~1520.08.3~155.0~128.9~151004.4~173.7~8.02.7~5.793丙環(huán)唑5.007.6~189.9~187.1~2020.08.8~146.9~146.5~141003.7~8.52.6~7.92.7~6.794烯唑醇5.003.7~9.76.1~155.6~1220.011~174.7~148.5~111005.7~133.0~9.81.7~7.795芐草唑5.005.6~1611~206.1~1220.05.3~164.5~154.2~141004.5~133.0~8.42.2~12962,4-D5.009.1~177.0~176.0~1420.07.4~145.2~123.5~8.51003.4~5.66.6~123.4~1197二甲四氯5.007.4~178.2~147.4~1320.07.4~1612~125.0~111003.4~8.22.6~141.6~7.498綠草定5.006.6~147.7~124.0~1620.05.1~136.6~133.3~121005.3~124.3~111.1~6.999除蟲脲5.007.9~129.2~154.1~1520.07.6~165.6~137.1~131007.1~9.83.5~7.53.9~7.8100滅幼脲5.007.5~148.6~185.9~1720.07.6~155.1~132.2~9.21006.5~9.32.1~7.34.5~6.7表D.3精密度匯總表（廢水）序號目標化合物加標濃度（ng/L）實驗室內(nèi)相對標準偏差（%）1呋蟲胺20.015~2040.07.9~161603.8~9.12噻蟲嗪20.07.5~1040.03.4~9.71602.4~7.83噻蟲胺20.09.7~1840.08.7~9.21603.8~4.74吡蟲啉20.011~1640.011~131603.5~175啶蟲脒20.09.7~1640.08.5~141603.7~8.36噻蟲啉20.07.1~9.940.07.5~141601.7~8.37氧樂果20.05.1~1440.07.3~9.51602.2~6.58砜吸磷20.06.1~1440.09.2~111603.7~119蚜滅磷20.04.1~9.740.08.0~101602.0~1210樂果20.03.9~6.840.06.4~131602.0~9.611磷胺20.04.3~9.840.05.4~8.71601.8~7.712甲拌磷亞砜20.05.7~1740.04.1~131602.3~6.213甲拌磷砜20.06.0~8.540.04.4~121604.9~1114滅線磷20.03.3~1340.06.9~121602.3~1115三唑磷20.05.5~1340.07.4~121600.9~1216地散磷20.04.2~1840.03.4~7.81601.3~1317甲基毒蟲畏20.07.1~1440.06.8~7.81602.8~5.518雙氟磺草胺20.05.9~1540.03.0~9.31601.5~7.819呋吡菌胺20.06.3~1340.06.4~121601.8~8.920氯蟲苯甲酰胺20.08.9~1940.05.4~131603.8~7.721解草嗪20.02.0~1340.06.7~121602.7~1122環(huán)酰菌胺20.013~1440.04.6~131601.0~6.723氟唑菌酰胺20.05.2~1540.03.6~131601.1~9.524敵草胺20.09.4~1540.03.7~7.21602.0~6.625甲草胺20.06.6~1440.02.2~131603.0~4.126氟酰胺20.08.2~1840.04.4~121602.6~1327四唑酰草胺20.06.0~9.740.03.2~8.71602.4~9.828環(huán)氟菌胺20.011~1540.06.4~121602.9~9.929多菌靈20.012~1940.06.7~121605.5~8.930噻菌靈20.08.5~1140.03.2~6.61605.6~1331麥穗靈20.05.2~1240.07.0~9.31603.0~5.932抑霉唑20.06.3~1340.05.2~111603.3~3.933十二環(huán)嗎啉20.07.8~1340.04.1~8.01604.5~6.534嘧霉胺20.03.3~5.040.05.8~8.71602.7~6.035烯酰嗎啉20.06.3~2040.09.3~171605.0~7.136嘧菌環(huán)胺20.03.1~9.440.04.8~6.91604.1~4.637咪鮮胺20.02.8~1140.04.6~6.51606.5~7.838辛噻酮20.05.7~1240.05.3~7.71603.0~8.839嘧菌胺20.05.5~1240.05.0~9.21603.9~8.840霜霉威20.02.3~1240.06.9~8.01601.4~8.341涕滅威亞砜20.05.3~1340.06.0~9.11603.3~9.042殺線威20.06.8~1340.05.1~9.81602.9~7.443乙硫苯威亞砜20.04.2~8.740.04.1~8.91605.6~6.4443-羥基克百威20.05.2~1140.04.3~8.31601.0~9.9456-氯-4-羥-3-苯基-噠嗪20.09.1~9.740.05.5~9.51603.1~9.246硫雙威20.08.6~1540.06.8~8.71601.7~8.247克百威20.09.7~1340.07.2~111604.5~6.348甲萘威20.07.0~9.340.05.7~111604.2~7.549異丙威20.07.4~1340.04.0~111601.4~7.5503,4,5-混殺威20.05.6~1640.05.4~121602.8~8.151仲丁威20.06.1~9.540.04.0~7.11602.2~9.452甲硫威20.03.5~1540.03.4~9.11601.1~5.053野燕枯20.04.5~9.140.07.4~111604.9~1154特丁隆20.06.7~9.740.06.7~7.91604.2~8.955甲草苯隆20.07.7~1240.06.4~8.11605.3~8.356綠麥隆20.05.8~1340.05.2~8.31604.5~7.057異丙隆20.07.5~1340.04.5~8.21605.3~1158綠谷隆20.06.2~1140.03.3~9.41605.5~6.659敵草隆20.09.9~1340.02.6~7.41606.4~7.960利谷隆20.04.1~1740.03.0~131604.7~1661枯草隆20.06.7~1340.05.8~8.01604.8~9.062可滅隆20.06.5~1240.04.0~9.21604.5~1063戊菌隆20.07.0~1340.04.1~8.51606.7~1464噁霜靈20.06.5~1440.03.8~8.01603.6~7.465滅草喹20.06.3~1440.06.2~7.71602.6~9.266甲磺隆20.05.6~1240.04.1~161604.0~1167甲霜靈20.03.4~1540.02.5~9.31603.1~1168抗倒酯20.06.7~2040.06.5~9.51602.1~8.169乙蟲清20.07.1~9.740.06.3~181603.8~9.870螺蟲乙酯20.011~1740.04.9~141602.6~6.871環(huán)酯草醚20.03.0~1840.02.9~9.21604.1~1072嘧菌酯20.011~1740.04.5~181603.1~7.973甲氧蟲酰肼20.06.2~1940.07.3~141602.0~7.474稻瘟靈20.011~1540.03.2~8.81603.6~9.875氟嘧菌酯20.09.9~1640.03.8~141602.4~8.976蟲酰肼20.06.3~1440.04.0~131601.7~6.977吡蚜酮20.02.7~1240.05.7~151604.5~1078二甲嘧酚20.06.0~1240.04.3~7.11603.9~6.479乙嘧酚20.03.9~1240.03.4~7.91603.1~7.480苯嗪草酮20.09.3~1240.05.0~9.41604.3~8.081異戊乙凈20.07.1~1640.06.2~8.71603.3~9.782嗪草酸甲酯20.07.9~1340.06.3~8.11602.2~1283三環(huán)唑20.04.2~1840.04.8~121603.8~4.684三唑醇20.04.4~6.040.05.5~9.21602.9~6.585多效唑20.05.4~1740.07.4~111602.4~6.086滅菌唑20.04.4~1540.05.0~8.91604.2~8.187腈菌唑20.05.4~1340.02.7~9.41603.3~5.788三唑酮20.05.7~1440.03.5~121601.7~8.489戊唑醇20.06.0~8.440.05.7~8.31603.5~1190芐氯三唑醇20.03.3~9.040.03.2~6.01604.4~7.991己唑醇20.06.6~8.440.05.6~8.11602.4~1292唑草胺20.03.6~1140.06.7~121603.5~5.793丙環(huán)唑20.07.0~1140.06.1~131603.2~9.894烯唑醇20.03.4~5.040.04.9~111603.1~8.895芐草唑20.04.1~8.340.05.3~6.91603.5~12962,4-D20.08.0~1340.08.6~131604.6~7.697二甲四氯20.05.0~8.640.05.2~9.61604.1~8.498綠草定20.08.8~1240.08.9~151603.6~8.899除蟲脲20.05.5~8.340.05.8~131605.8~9.8100滅幼脲20.05.5~7.640.06.2~111604.2~7.2表D.4正確度匯總表（空白水樣）序號目標化合物加標濃度（ng/L）回收率范圍（%）P+2SP1呋蟲胺5.00110~118114±8.020.098.7~112105±13.9100105~112108±7.62噻蟲嗪5.0099.1~115107±15.920.0101~113108±12.5100111~116114±5.03噻蟲胺5.00104~113109±9.020.096.6~97.897.1±1.210099.0~108104±9.04吡蟲啉5.0097.1~111104±14.020.0104~117112±13.610097.7~114106±16.35啶蟲脒5.0086.0~111101±26.120.084.9~10495.2±19.310099.2~103102±4.46噻蟲啉5.0078.4~10892.9±29.620.090.8~115106±25.6100109~114112±5.37氧樂果5.0077.5~81.279.5±3.820.085.1~99.190.6±14.910076.2~10187.4±25.18砜吸磷5.0085.3~10798.4±23.120.094.8~112103±17.410099.9~114108±14.29蚜滅磷5.0070.7~11890.6±49.120.082.2~10496.4±24.610072.0~10485.5±33.210樂果5.0077.5~10392.6±26.820.085.2~98.393.9±15.010088.1~10195.2±13.111磷胺5.0074.1~82.578.4±8.420.071.7~99.482.1±30.210088.7~95.392.5±6.812甲拌磷亞砜5.0086.1~118102±32.020.095.7~106102±10.610095.1~110103±14.913甲拌磷砜5.0077.8~115101±40.420.083.8~95.791.0±12.610088.1~10296.0±14.314滅線磷5.0075.3~11490.1±41.820.069.0~10391.0±38.210068.2~10385.6±34.815三唑磷5.0072.3~80.876.6±8.520.078.5~95.585.5±17.710076.8~83.279.9±6.416地散磷5.0066.2~11080.9±50.420.064.0~95.581.0±31.810066.4~75.172.1±9.917甲基毒蟲畏5.0068.8~79.874.4±11.020.069.4~82.975.9±13.510061.8~75.367.4±14.118雙氟磺草胺5.00103~119112±16.020.084.0~85.184.5±1.110090.1~97.393.5±7.219呋吡菌胺5.0077.7~97.787.3±20.120.079.5~83.781.4±4.210084.0~10192.4±17.020氯蟲苯甲酰胺5.0078.2~98.087.0±20.120.082.0~87.984.6±6.010084.2~94.088.4±10.121解草嗪5.0088.8~118100.0±31.520.091.3~93.692.6±2.410062.8~99.676.5±40.222環(huán)酰菌胺5.0081.9~97.689.5±15.720.076.2~82.479.3±6.210077.8~89.584.1±11.823氟唑菌酰胺5.0077.7~97.787.3±20.120.079.5~83.781.4±4.210084.0~10192.4±17.024敵草胺5.0072.6~10789.1±34.520.070.9~78.974.9±8.010073.8~82.078.5±8.425甲草胺5.0063.0~86.371.0±26.520.070.6~89.983.3±22.010066.6~97.182.0±30.526氟酰胺5.0078.2~92.384.9±14.220.071.7~84.479.6±13.810075.3~86.081.1±10.827四唑酰草胺5.00117~119118±2.020.0106~108107±2.010069.5~97.285.3±28.528環(huán)氟菌胺5.0070.6~87.980.3±17.720.077.3~10394.1±29.110069.6~98.081.4±29.629多菌靈5.0099.2~111105±12.020.0106~114110±8.310085.0~119102±34.230噻菌靈5.0083.8~11998.0±37.120.099.1~104102±4.910099.5~113106±13.731麥穗靈5.0086.3~91.189.2±5.120.095.1~106102±11.010088.7~118108±33.332抑霉唑5.0081.8~10997.6±28.220.071.8~93.584.1±22.310097.4~106103±9.033十二環(huán)嗎啉5.0090.0~11599.6±26.920.062.3~11091.1±50.710063.8~11983.5±61.734嘧霉胺5.0085.1~87.986.3±2.920.081.8~11997.8±38.310083.2~11596.3±33.235烯酰嗎啉5.0097.8~114107±16.620.0102~115111±15.0100104~119113±15.536嘧菌環(huán)胺5.0081.4~99.391.1±18.120.073.7~81.178.2±7.910091.2~10195.4±10.137咪鮮胺5.0088.2~95.290.9±7.520.097.4~119108±21.610093.0~10398.6±10.238辛噻酮5.0076.5~10895.5±33.520.061.0~96.679.5±35.710093.4~111102±17.839嘧菌胺5.00102~118111±16.020.083.6~95.791.3±13.4100108~116113±8.340霜霉威5.0079.9~85.583.0±5.720.070.1~99.189.4±33.410068.4~10484.1±36.341涕滅威亞砜5.0085.6~92.889.1±7.220.092.3~117104±25.110095.0~118104±25.042殺線威5.0067.2~11391.3±46.020.094.1~117103±25.510073.3~11798.8±45.543乙硫苯威亞砜5.0078.9~11393.9±34.920.073.7~10886.4±37.610066.2~10386.4±37.3443-羥基克百威5.0079.4~82.280.5±3.020.0101~114108±13.010099.0~116105±19.5456-氯-4-羥-3-苯基-噠嗪5.0098.0~119110±21.620.079.5~10394.1±25.5100103~112107±9.246硫雙威5.0085.0~11097.8±25.020.0104~120112±16.010098.7~106103±7.547克百威5.0088.9~10193.3±13.320.0109~116113±7.010094.8~10498.6±9.648甲萘威5.0065.2~86.178.2±22.620.076.1~10996.0±35.0100110~118114±8.049異丙威5.0073.9~85.578.7±12.120.082.5~96.390.5±14.310075.2~98.184.3±24.3503,4,5-混殺威5.0070.0~87.178.0±17.220.083.8~90.086.8±6.210086.6~88.187.2±1.651仲丁威5.0063.1~80.074.1±19.120