1磷、倍硫磷、水胺硫磷、甲基異柳磷、殺撲磷、馬拉硫磷、地蟲硫磷、速滅磷、磷胺、倍硫磷、水胺硫磷、甲基異柳磷、殺撲磷、丙溴磷、蠅毒磷、殺螟硫磷、甲基對硫磷、亞胺硫磷、馬拉硫磷、地蟲硫磷、速滅磷、磷胺、治螟試樣用乙腈提取，固相萃取柱凈化，氣相色譜-質(zhì)譜聯(lián)用儀檢測，外標(biāo)法定量。2磷、甲基異柳磷、殺撲磷、丙溴磷、蠅毒磷、硫磷、速滅磷、磷胺、治螟磷、久效磷、對硫5.3.1標(biāo)準(zhǔn)儲備液（100.0μg/mL）：準(zhǔn)確吸取各有機(jī)磷農(nóng)藥標(biāo)準(zhǔn)品1.0mL，分5.3.2標(biāo)準(zhǔn)中間液（2.0μg/mL）：吸取各農(nóng)藥標(biāo)準(zhǔn)儲備液1.0mL于50mL棕色容量瓶中，用丙酮定容5.3.3標(biāo)準(zhǔn)工作液：分別準(zhǔn)確吸取不同體積標(biāo)準(zhǔn)中間液，用空白基質(zhì)配制成濃度為20.0ng/mL、3速通過氨基固相萃取柱。用5mL去離子水洗滌SPE柱以去除強極性干擾物質(zhì)，隨后用真空或氮氣干凈試管中，用3.0mL相同溶劑再洗脫并合并洗脫液。40℃水浴中氮氣吹干至近干。加入2mL乙a）色譜柱：Rtx-5MS柱(30m×0.25mmj）溶劑延遲：5min；k）多反應(yīng)監(jiān)測：每種農(nóng)藥分別選擇一對定量離子、一對定性離子。每組所有需要檢測離子對按照選擇的離子均出現(xiàn)。同時所選擇離子的豐度比），>50%響應(yīng)值均應(yīng)在儀器檢測的線性范圍內(nèi)。標(biāo)準(zhǔn)使用液與試液等體積規(guī)定的條件進(jìn)行測定，如果試液中與標(biāo)準(zhǔn)溶X──試樣中各有機(jī)磷農(nóng)藥的含量，單位為毫克每千克（mg/kg);c──從標(biāo)準(zhǔn)曲線得到的有機(jī)磷農(nóng)藥濃度，單位m──試樣溶液所代表試樣的質(zhì)量，單位為克（g?──樣品稀釋倍數(shù)。磷、甲基異柳磷、殺撲磷、丙溴磷、蠅毒磷、硫磷、速滅磷、磷胺、治螟磷、久效磷、對硫Profenofosfonofos (x10,000) 2.02.0141.00>79.001.51.00.5l\"\(x10,000) 3.0 3.0 4.0 2.0 1.06.06.57.07.58.08.5(x10,000)2.0(x10,000)2.01.51.00.594.00>64.004.009.510.010.511.011.512.0(x10,000)5.0156.00>110.00 110.00>79.004.03.05.0156.00>110.00 110.00>79.004.03.02.012.513.013.514.014.515.03.02.01.03.02.01.0200.00158.00>158.00>97.006.05.04.06.05.04.03.02.01.00>134.00(x10,000)1.00260.00>75.00231.00>129.000.750.500.2514.014.515.015.516.016.5(x10,000) 257.00>162.001.5257.00>119.00 1.0 0.5——-(x10,000)278.00>109.003.0278.00>169.00 2.0 l1.02002052002057.55.02.5(x1,000)7.55.02.5230.0>136.000020.020.521.021.522.022.51.251.000.751.251.000.750.500.25>121.00>121.1021.021.522.022.523.023.51.501.251.501.251.000.750.500.25145.0>85.000>58.00 338.90>268.90 338.90>268.901.5336.90>266.90 1.00.50.5 362.00>109.002.0362.00>226.00 1.5 362.00>109.002.0362.00>226.00 1.5 0.51.0(x10,000)2.52.01.51.00.5277.00>260.00277.00>109.102.52.01.51.00.5277.00>260.00277.00>109.1019.520.020.521.021.522.0(x10,000)2.5263.00>109.00 125.00>47.002.01.51.00.52.5263.00>109.00 125.00>47.002.01.51.018.519.019.520.020.521.0(x100,000)1.25160.00>77.00 0.751.00160.00>133.001.25160.00>77.00 0.75 0.50 0.50 0.2528.028.529.029.530.030.5(x10,000) 173.10>99.00 173.10>99.00 173.10>127.00 Il5.04.03.02.01.0 Il地蟲硫磷1.000.750.500.2541.000.750.500.2547.10>109.1026.00>137.1016.517.017.518.018.519.0(x10,000) 4.0 il3.0 il2.0hlli1.0lli00(x10,000)5.0127.00>109.005.0 192.00>127.00 4.0 3.02.01.09.09.510.010.511.011.5127.10>109.10127.10>95.104.03.02.01.0(x10,000)127.10>109.10127.10>95.104.03.02.01.0(x10,000)3.0 2.0 2.01.018.018.519.019.520.020.52.0(x10,000)322.00>202.001.5322.00>174.00 2.0(x10,000)322.00>202.001.5322.00>174.00 1.00.5Il14.014.515.015.516.016.5 291.10>109.00 291.10>109.002.0139.00>109.00 1.0 1.5 1.0 0.50.51.000.750.500.251.000.750.500.25182.00>1182.00>111.0038.002.01.51.00.572.01.51.00.57人304.10>179.1016.016.517.017.518.018.5>47.00125.0>47.00125.0>79.0001.501.251.000.750.5000.25