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固體廢物氨基甲酸酯類農(nóng)藥的測定柱后衍生-高效液相色譜法ii目 次前言 ii適范圍 1規(guī)性用件 1方原理 1干和除 2試和料 2儀和備 3樣品 4分步驟 6結(jié)計與示 7密和確度 8量證質(zhì)控制 9物理 10附錄A規(guī)性錄)方法出和定限 附錄B資性錄)方法密和確度 1311固體廢物 氨基甲酸酯類農(nóng)藥的測柱后衍生高效液相色譜法本標(biāo)準(zhǔn)規(guī)定了測定固體廢物及其浸出液中氨基甲酸酯類農(nóng)藥的柱后衍生-高效液相色譜法。本標(biāo)準(zhǔn)適用于固體廢物及其浸出液中涕滅威亞砜、涕滅威砜、滅多威、3-羥基克百威、涕滅威、殘殺威、克百威、甲萘威、異丙威、甲硫威等10種氨基甲酸酯類農(nóng)藥的測定。101.015μl100.001mg/kg0.004mg/kg1001.015μl為0.1μg/L,測定下限為0.4μg/L。詳見附錄A。HJ782 HJ/T20 HJ/T298 HJ/T299 HJ/T300 ((1,2(1)22
(2)甲酸O9。NHNa2O4馬弗爐中450℃灼燒4h,稍冷卻后裝入具塞磨口玻璃瓶中密封,于潔凈干燥器中保存。甲醇HOH2C2乙腈H3NNBO71H22SCHO或2C4HNC。C8HO2ρ=4.0g/L。稱取4.0g氫氧化鈉(5.2)溶于水中,定容至1.0L。c(NaOH)=0.05mol/L。稱取20g(521(5.)c(Na2B4O7·10H2O)=0.05mol/L。稱取9.1g(.1(523稱取00g(.10l(.4100l5.121.0l2(5.)或.0g2(5833(5.23)過濾。也可直接購買市售商品。甲醇1+2。用甲醇(5.4)和二氯甲烷(5.5)按1:2體積比混合。1+2。用二氯甲烷(5.5)和甲醇(5.4)按1:2體積比混合。甲醇1+9。用甲醇(5.4)和二氯甲烷(5.5)按1:9體積比混合。ρ=100mg/L。直接購買市售有證標(biāo)準(zhǔn)溶液,按標(biāo)準(zhǔn)溶液證書要求保存。ρ=10.0。5005ml-183/N-(500mg/6500g6。5.21 0.6mm~0.9mm(30目~20目。馬弗爐中450℃灼燒4h,稍冷卻后裝入具塞磨口玻璃瓶中密封,于潔凈干燥器中保存。5.22 150μm~830μm(100目~20目。馬弗爐中450℃灼燒4h,稍冷卻后裝入具塞磨口玻璃瓶中密封,于潔凈干燥器中保存。濾膜Ⅰ:0.45μm濾膜Ⅱ:0.45μm5.25 99.999%。525.0cm4.0mmC8(50ml0.01。44樣品按照HJ/T20和HJ/T2984℃以7d。如-3030d。稱取10(0.1)5.3(5.21)按照HJ/T299或HJ/T300pH4pH3~430pH3~830d。提取采用甲醇-二氯甲烷混合溶劑(5.14)提取樣品中氨基甲酸酯類農(nóng)藥,參考條件:壓力10.345560s3HJ782將濾筒置于索氏提取器回流管中,在圓底溶劑瓶中加入200ml甲醇-二氯甲烷混合溶劑(5.14),回流速度控制在4~6次/h,提取8h,待濃縮。10100(5.10)調(diào)節(jié)水樣pH至6~7。10l甲醇5.、10l水以約4/n(5.14ml/min的速度通5ml25min,8ml(5.15)4ml/min55脫液于洗脫液接收管中,待濃縮。稱取0001g30l(5.2100ml(5.1)(5.10)pH6~7,7.3.1.2b)濃縮(6.5)(7.3.1.17.3.1.3)5.0ml~10(5.24)5.0ml~10.0a)(7.3.1.27.3.1.4)1.0(5.24)7.3.3b)注:定容體積可根據(jù)樣品含水率情況適當(dāng)調(diào)整。凈化7.3.2100(5.10)H至~70l甲醇5.4、10l水以約4/n取柱Ⅰ(5.9,在活化過程中應(yīng)確保萃取柱填料表面不露出液面。調(diào)節(jié)流量使水樣以約ml/min5ml25min8ml二氯甲烷(5.15)4ml/min(6.54oC10,(5.24)7.3.3b)用5l甲醇(.164/n(.20劑潤洗后一并轉(zhuǎn)入柱頭,在柱填料剛要暴露于空氣之前,用5ml甲醇-二氯甲烷混合溶劑(5.16)以約4ml/min的速度洗脫固相萃取柱,收集洗脫液于洗脫液接收管中。用濃縮裝置(6.5)40oC1.0ml(5.24)-1840。5.2(7.2(7相66(522(7.2(7.)流動相:流動相A(5.6),流動相B0.8ml/min115330nm460nm435nm。1時間(min)流動相A(%)流動相B(%)01288212884266344595548955501288(5.18)5ml(5.4)稀釋50.05μg/ml、0.50μg/ml、1.00μg/ml2.50μg/ml5.00()按照與校準(zhǔn)曲線的建立(8.2)相同的步驟進(jìn)行試樣(7.3)的測定。77按照與試樣測定(8.3)相同的步驟進(jìn)行空白試樣(7.4)的測定。在本標(biāo)準(zhǔn)規(guī)定的儀器參考條件(8.1)下,標(biāo)準(zhǔn)溶液色譜圖見圖1。00511054267938LU01-涕滅威亞砜;2-涕滅威砜;3-滅多威;4-3-羥基克百威;5-涕滅威;6-殘殺威;7-克百威;8-甲萘威;9-異丙威;10-甲硫威。圖1 氨甲酯農(nóng)參考譜(ρ=1.0mg/L)固體廢物樣品中目標(biāo)物的質(zhì)量濃度按照公式(3)進(jìn)行計算:w1V1m
(3)式中:w—mg/kg;1—μg/ml;V1—固體廢物試樣定容體積,ml;m—g;固體廢物浸出液樣品中目標(biāo)物的質(zhì)量濃度按照公式(4)進(jìn)行計算:882V20
(4)V3式中:—浸出液樣品中目標(biāo)物的質(zhì)量濃度,μg/L;2—μg/ml;V2—浸出液試樣定容體積,ml;V3—浸出液的體積,ml。測定結(jié)果小數(shù)點后位數(shù)的保留與方法檢出限保持一致,最多保留3位有效數(shù)字。精密度0.500mg/kg0.200mg/kg0.005mg/kg61.4%~17%1.5%~31%5.5%~12%5.7%~12%和0.133mg/kg~0.156mg/kg0.038mg/kg~0.101mg/kg0.001mg/kg~0.0020.145mg/kg~0.209mg/kg0.050mg/kg~0.119mg/kg和0.002mg/kg~0.003mg/kg。0.500mg/kg0.200mg/kg0.005mg/kg61.8%~21%、2.7%~17%5.4%~22%6.9%~19%、2.2%~9.3%7.9%~17%0.124mg/kg~0.175mg/kg、0.035mg/kg~0.048mg/kg和0.001mg/kg~0.002mg/kg0.151mg/kg~0.288mg/kg、0.040mg/kg~0.063mg/kg和0.002mg/kg~0.003mg/kg。6驗8~3020.09gk;再0.014mg/kg。50.0μg/L、20.0μg/L0.500μg/L的統(tǒng)一空白固體廢物浸出液樣品進(jìn)行了6次重復(fù)測定:實驗室內(nèi)相對標(biāo)準(zhǔn)偏差分別為0.72250.94~24和1.4~1943196.~14%5.5%~13%μg/L~18.4μg/L、4.3μg/L~8.7μg/L0.2μg/L;14.3μg/L~24.6μg/L、6.4μg/L~11.1μg/L0.2μg/L。50.0μg/L、20.0μg/L0.500μg/L62.6%~21%1.3%~19%8.3%~12%和14.2μg/L~18.0μg/L3.5μg/L~7.9μg/L0.299限分別為15.6μg/L~22.2μg/L、5.0μg/L~9.0μg/L和0.2~0.4μg/L。精密度結(jié)果參見附錄B。準(zhǔn)確度0.500mg/kg、0.200mg/kg0.005mg/kg物樣品進(jìn)行了674.4%~124%77.7%~112%和55.7%~和(89.2±32)%~(103±30)%。0.500mg/kg、0.200mg/kg0.005mg/kg6和64.3%~125%;加標(biāo)回收率最終值分別為(85.0±30)%~(101±24)%(88.6±4.0)%~(96.4±17)%(88.1±16)%~(97.5±32)%。0.080mg/kg污泥樣品進(jìn)行了6次重復(fù)測定:加標(biāo)回收率范圍為38.3%~138%;加標(biāo)回收率最終值為(64.7±30)%~(83.4±44)%。50.0μg/L、20.0μg/L0.500μg/L659.1%~118%77.7%~112%55.7%~和(89.2±32)%~(103±30)%。50.0μg/L、20.0μg/L0.500μg/L6和64.3%~125%;加標(biāo)回收率最終值分別為(95.1±18)%~(104±20)%(82.2±12)%~(106±19)%(96.2±20)%~(103±22)%。準(zhǔn)確度結(jié)果參見附錄B。2020/批1校準(zhǔn)校準(zhǔn)曲線的相關(guān)系數(shù)r≥0.995。選擇校準(zhǔn)曲線的中間濃度點進(jìn)行連續(xù)校準(zhǔn),每分析20個樣品或每批次(少于20個樣品/批)進(jìn)行1次連續(xù)校準(zhǔn),測定結(jié)果相對誤差應(yīng)在±20%之內(nèi),否則需重新建立校準(zhǔn)曲線。每20個樣品或每批次(少于20個樣品/批)至少分析1個平行樣,平行樣相對偏差≤40%。10102020/批130%~150%實驗中產(chǎn)生的廢液和廢物應(yīng)分類收集,并做好相應(yīng)標(biāo)識,委托有資質(zhì)的單位進(jìn)行處理。1111附錄A()101001.015μl10A.1。10A.2。表A.1 體物法出限測下限序號化合物英文名稱CASNo.檢出限(mg/kg)測定下限(mg/kg)1涕滅威亞砜AldicarbSulfoxide1646-87-30.0010.0042涕滅威砜AldicarbSulfone1646-88-40.0010.0043滅多威Methomyl16752-77-50.0010.00443-羥基克百威3-Hydroxycarbofuran16655-82-60.0010.0045涕滅威Aldicarb116-06-30.0010.0046殘殺威Propoxur114-26-10.0010.0047克百威Carbofuran1563-66-20.0010.0048甲萘威Carbaryl63-25-20.0010.0049異丙威Isoprocarb2631-40-50.0010.00410甲硫威Mercaptodimethur2032-65-70.0010.0041212表A.2 體物出方法出和定限序號化合物英文名稱CASNo.檢出限(μg/L)測定下限(μg/L)1涕滅威亞砜AldicarbSulfoxide1646-87-30.10.42涕滅威砜AldicarbSulfone1646-88-40.10.43滅多威Methomyl16752-77-50.10.443-羥基克百威3-Hydroxycarbofuran16655-82-60.10.45涕滅威Aldicarb116-06-30.10.46殘殺威Propoxur114-26-10.10.47克百威Carbofuran1563-66-20.10.48甲萘威Carbaryl63-25-20.10.49異丙威Isoprocarb2631-40-50.10.410甲硫威Mercaptodimethur2032-65-70.10.41313附錄B()B.1B.2B.3B.4表B.1 體物法精密度樣品類型序號化合物平均值(mg/kg)實驗室內(nèi)相對(%)實驗室間相對(%)重現(xiàn)性限r(nóng)(mg/kg)再現(xiàn)性限R(mg/kg)空白加標(biāo)濃度:0.500mg/kg1涕滅威亞砜0.5031.9~13120.1340.2092涕滅威砜0.5161.4~17100.1530.2033滅多威0.4961.8~167.90.1510.17643-羥基克百威0.4692.2~138.10.1330.1615涕滅威0.4412.7~177.10.1500.1636殘殺威0.4642.7~145.50.1400.1467克百威0.5012.7~138.60.1470.1818甲萘威0.5071.9~13110.1530.2079異丙威0.4432.8~179.40.1560.18410甲硫威0.4781.4~135.90.1340.145加標(biāo)濃度:0.200mg/kg1涕滅威亞砜0.1942.2~11120.0380.0722涕滅威砜0.2061.5~14120.0510.0843滅多威0.2002.6~125.80.0420.05043-羥基克百威0.1914.3~12100.0490.0705涕滅威0.1906.4~116.30.0490.0566殘殺威0.1934.7~126.10.0490.0567克百威0.2005.5~108.10.0430.0608甲萘威0.1926.2~31140.1010.1199異丙威0.1955.0~155.70.0540.05810甲硫威0.1884.9~23120.0680.0901414續(xù)表樣品類型序號化合物平均值(mg/kg)實驗室內(nèi)相對(%)實驗室間相對(%)重現(xiàn)性限r(nóng)(mg/kg)再現(xiàn)性限R(mg/kg)空白加標(biāo)濃度:0.005mg/kg1涕滅威亞砜0.0052.2~19150.0020.0032涕滅威砜0.0053.7~13150.0010.0023滅多威0.0054.3~14120.0010.00243-羥基克百威0.0054.0~14100.0010.0025涕滅威0.0055.4~17140.0010.0026殘殺威0.0055.7~11150.0010.0027克百威0.0055.3~15170.0010.0038甲萘威0.0044.7~18180.0010.0039異丙威0.0058.0~14160.0010.00210甲硫威0.0053.6~16230.0010.003殘渣加標(biāo)濃度:0.500mg/kg1涕滅威亞砜0.5063.8~136.90.1280.1532涕滅威砜0.4865.4~169.80.1420.1863滅多威0.5036.4~18120.1650.22743-羥基克百威0.4584.3~17190.1640.2885涕滅威0.4575.0~199.20.1620.1896殘殺威0.4584.4~128.60.1270.1607克百威0.4726.3~127.60.1240.1518甲萘威0.4251.8~19180.1750.2639異丙威0.4564.2~14130.1340.20210甲硫威0.4272.6~21180.1380.252加標(biāo)濃度:0.200mg/kg1涕滅威亞砜0.1932.9~128.60.0470.0632涕滅威砜0.1842.7~9.89.30.0410.0613滅多威0.1893.6~107.80.0420.05643-羥基克百威0.1793.5~142.20.0420.0435涕滅威0.1803.3~133.90.0390.0416殘殺威0.1823.4~104.40.0360.0407克百威0.1844.1~8.78.10.0430.0608甲萘威0.1793.6~115.90.0400.0479異丙威0.1823.2~175.10.0480.05110甲硫威0.1783.2~9.05.30.0350.0411515續(xù)表樣品類型序號化合物平均值(mg/kg)實驗室內(nèi)相對(%)實驗室間相對(%)重現(xiàn)性限r(nóng)(mg/kg)再現(xiàn)性限R(mg/kg)殘渣加標(biāo)濃度:0.005mg/kg1涕滅威亞砜0.0058.0~18170.0020.0032涕滅威砜0.0046.4~229.00.0020.0023滅多威0.0058.4~16100.0020.00243-羥基克百威0.0058.1~17160.0020.0035涕滅威0.0057.8~17160.0020.0036殘殺威0.0048.5~19120.0020.0027克百威0.0058.3~187.90.0020.0028甲萘威0.0046.7~169.20.0020.0029異丙威0.0055.4~158.90.0010.00210甲硫威0.0055.6~14100.0010.002污泥1涕滅威亞砜ND////2涕滅威砜ND////3滅多威0.0138.3~30320.0090.01443-羥基克百威ND////5涕滅威ND////6殘殺威ND////7克百威ND////8甲萘威ND////9異丙威ND////10甲硫威ND////1616表B.2 體物出方法精度樣品類型序號化合物平均值(μg/L)實驗室內(nèi)相對(%)實驗室間相對(%)重現(xiàn)性限r(nóng)(μg/L)再現(xiàn)性限R(μg/L)空白浸出液加標(biāo)濃度:50.0μg/L1涕滅威亞砜47.50.78~206.112.814.32涕滅威砜48.12.6~238.513.116.53滅多威49.82.9~248.518.420.643-羥基克百威43.01.2~211511.220.85涕滅威43.42.7~254.315.916.76殘殺威45.12.7~247.714.916.77克百威47.62.7~231314.722.08甲萘威45.70.72~171611.923.49異丙威43.12.8~258.717.218.810甲硫威42.22.0~191911.824.6加標(biāo)濃度:20.0μg/L1涕滅威亞砜19.40.94~13104.36.92涕滅威砜21.46.8~13125.68.73滅多威20.02.8~20115.98.043-羥基克百威19.77.6~146.95.66.45涕滅威19.27.8~16105.77.66殘殺威20.18.0~13135.99.27克百威20.37.9~128.75.67.18甲萘威19.67.8~26148.711.19異丙威19.47.9~147.05.96.610甲硫威19.55.1~24127.29.4加標(biāo)濃度:0.5μg/L1涕滅威亞砜0.52.3~125.50.20.22涕滅威砜0.53.5~177.10.20.23滅多威0.52.1~159.90.20.243-羥基克百威0.51.8~137.40.20.25涕滅威0.52.3~125.90.20.26殘殺威0.53.5~148.00.20.27克百威0.51.4~178.90.20.28甲萘威0.41.6~16130.20.29異丙威0.43.0~16100.20.210甲硫威0.43.7~19110.20.21717續(xù)表樣品類型序號化合物平均值(μg/L)實驗室內(nèi)相對實驗室間相對標(biāo)準(zhǔn)偏差(%)重現(xiàn)性限r(nóng)(μg/L)再現(xiàn)性限R(μg/L)殘渣浸出液加標(biāo)濃度:50.0μg/L1涕滅威亞砜52.22.6~149.115.619.52涕滅威砜51.56.4~161017.521.73滅多威51.85.7~189.518.021.443-羥基克百威49.66.0~171116.922.25涕滅威48.35.9~194.716.918.06殘殺威47.94.6~136.914.215.97克百威48.85.1~137.714.316.88甲萘威47.56.6~219.317.019.89異丙威49.32.8~146.114.415.610甲硫威48.77.9~136.915.016.6加標(biāo)濃度:20.0μg/L1涕滅威亞砜19.92.6~15105.37.62涕滅威砜19.95.6~16115.17.73滅多威21.11.4~8.48.94.26.543-羥基克百威16.64.3~118.33.55.05涕滅威19.24.2~10114.37.26殘殺威19.62.1~9.2114.16.97克百威19.92.4~8.8113.87.38甲萘威18.76.7~19107.99.09異丙威19.81.3~10123.77.510甲硫威19.34.3~12124.27.5加標(biāo)濃度:0.5μg/L1涕滅威亞砜0.51.6~177.90.20.22涕滅威砜0.55.7~22110.20.23滅多威0.53.9~14100.20.343-羥基克百威0.52.1~17210.20.45涕滅威0.53.5~16110.20.36殘殺威0.56.1~178.50.20.27克百威0.52.9~199.00.20.28甲萘威0.52.4~13110.20.29異丙威0.54.8~16110.20.210甲硫威0.52.4~17100.20.21818表B.3 體物法準(zhǔn)確度樣品類型序號化合物樣品濃度(mg/kg)加標(biāo)回收率范圍P(%)P(%)SP(%)加標(biāo)回收率最終值P2SP(%)空白加標(biāo)濃度:0.500mg/kg1涕滅威亞砜ND91.2~12410112101±242涕滅威砜ND96.1~12410311103±223滅多威ND95.9~11199.17.899.1±1643-羥基克百威ND89.7~10395.35.395.3±115涕滅威ND80.3~96.388.16.388.1±136殘殺威ND86.7~10192.95.192.9±107克百威ND92.7~1161008.6100±178甲萘威ND87.5~11810111101±229異丙威ND74.4~96.588.68.388.6±1710甲硫威ND89.6~10395.55.695.5±11加標(biāo)濃度:0.200mg/kg1涕滅威亞砜ND81.3~11097.11197.1±222涕滅威砜ND86.7~11110312103±243滅多威ND90.8~10899.85.899.8±1243-羥基克百威ND81.3~10994.51194.5±225涕滅威ND86.0~10194.86.094.8±126殘殺威ND88.9~10796.45.996.4±127克百威ND88.9~1101008.1100±168甲萘威ND80.3~11295.81395.8±269異丙威ND89.9~10797.65.697.6±1110甲硫威ND77.7~11194.21294.2±24加標(biāo)濃度:0.005mg/kg1涕滅威亞砜ND86.6~12410315103±302涕滅威砜ND85.6~12610115101±303滅多威ND84.1~11610112101±2443-羥基克百威ND78.8~10692.79.492.7±195涕滅威ND82.3~12096.01496.0±286殘殺威ND77.7~11495.01495.0±287克百威ND78.5~12398.81798.8±348甲萘威ND69.7~11089.21689.2±329異丙威ND73.7~11190.01490.0±2810甲硫威ND55.7~10790.42190.4±421919續(xù)表樣品類型序號化合物樣品濃度(mg/kg)加標(biāo)回收率范圍P(%)P(%)SP(%)加標(biāo)回收率最終值P2SP(%)殘渣加標(biāo)濃度:0.500mg/kg1涕滅威亞砜ND90.4~1101017.0101±142涕滅威砜ND82.0~10897.29.597.2±193滅多威ND90.6~12310112101±2443-羥基克百威ND72.6~11089.71589.7±305涕滅威ND80.4~10291.38.491.3±176殘殺威ND79.3~10291.67.991.6±167克百威ND82.8~10294.47.194.4±148甲萘威ND66.1~10385.01585.0±309異丙威ND76.4~10191.11191.1±2210甲硫威ND67.5~10585.41685.4±32加標(biāo)濃度:0.200mg/kg1涕滅威亞砜ND86.6~11196.48.396.4±172涕滅威砜ND85.8~10691.88.691.8±173滅多威ND89.3~10794.77.494.7±1543-羥基克百威ND86.6~92.088.62.088.6±4.05涕滅威ND86.6~96.490.13.590.1±7.06殘殺威ND87.8~98.791.24.091.2±8.07克百威ND88.4~10192.14.592.1±9.08甲萘威ND83.5~98.289.35.389.3±119異丙威ND88.1~10090.84.690.8±9.210甲硫威ND83.1~95.689.14.789.1±9.4加標(biāo)濃度:0.005mg/kg1涕滅威亞砜ND75.3~12392.71692.7±322涕滅威砜ND81.2~10188.98.088.9±163滅多威ND88.7~11396.09.696.0±1943-羥基克百威ND80.7~12197.51697.5±325涕滅威ND78.5~11793.01593.0±306殘殺威ND74.3~10489.21089.2±207克百威ND85.3~10395.97.595.9±158甲萘威ND79.0~10288.18.188.1±169異丙威ND86.7~10995.28.595.2±1710甲硫威ND81.6~10793.09.593.0±192020續(xù)表樣品類型序號化合物樣品濃度(mg/kg)加標(biāo)回收率范圍P(%)P(%)SP(%)加標(biāo)回收率最終值P2SP(%)污泥加標(biāo)濃度:0.080mg/kg1涕滅威亞砜ND45.9~10768.71568.7±302涕滅威砜ND39.7~11575.51675.5±323滅多威0.01338.3~10164.71564.7±3043-羥基克百威ND49.7~12980.71380.7±265涕滅威ND46.9~10875.89.175.8±186殘殺威ND49.4~11776.91076.9±207克百威ND43.1~10474.61074.6±208甲萘威ND38.6~13583.42283.4±449異丙威ND45.4~13878.62078.6±4010甲硫威ND56.7~12781.31581.3±302121表B.4 體物出方法準(zhǔn)度樣品類型序號化合物樣品濃度(μg/L)加標(biāo)回收率范圍P(%)P(%)SP(%)加標(biāo)回收率最終值P2SP(%)空白浸出液加標(biāo)濃度:50.0μg/L1涕滅威亞砜ND84.8~10195.15.895.1±122涕滅威砜ND85.2~10496.28.196.2±163滅多威ND90.7~11299.58.599.5±1743-羥基克百威ND63.3~10088.11488.1±285涕滅威ND81.8~91.486.73.786.7±7.46殘殺威ND80.5~10190.26.990.2±147克百威ND83.5~11895.31295.3±248甲萘威ND69.1~11491.31591.3±309異丙威ND77.1~94.086.17.586.1±1510甲硫威ND59.1~99.484.51684.5±32加標(biāo)濃度:20.0μg/L1涕滅威亞砜ND81.3~11097.11197.1±222涕滅威砜ND86.7~11110312103±243滅多威ND90.8~10899.85.899.8±1243-羥基克百威ND81.3~10994.51194.5±225涕滅威ND86.0~10194.86.094.8±126殘殺威ND88.9~10796.45.996.4±127克百威ND88.9~1101008.1100±168甲萘威ND80.3~
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