图1自动固相萃取仪固相萃取流程(HLB萃取柱)
图2自动固相萃取仪固相萃取流程(C18萃取盘)
图3标准品色谱图
图4加标水样色谱图(HLB萃取柱)
图5加标水样色谱图(C18萃取盘)
表1加标水样过HLB萃取柱的回收率及RSD(n = 3)
名称 | 出峰时间(min) | 回收率(%) | ||||
1 | 2 | 3 | 平均 | RSD | ||
六氯丁二烯 | 6.294 | 49.5 | 47.57 | 53.15 | 50.07 | 5.66 |
敌敌畏 | 6.517 | 77.01 | 84.34 | 88.05 | 83.13 | 6.76 |
克百威 | 7.048 | 77.97 | 71.87 | 81.21 | 77.02 | 6.16 |
溴氰菊酯 | 9.751 | 75.37 | 78.21 | 76.32 | 76.63 | 1.89 |
α-六六六 | 13.573 | 83.69 | 88.43 | 81.21 | 84.44 | 4.34 |
乐果 | 14.187 | 79.5 | 69.65 | 73.21 | 74.12 | 6.73 |
阿特拉津 | 14.669 | 87.12 | 84.4 | 90.35 | 87.29 | 3.41 |
β-六六六 | 14.772 | 86.43 | 88.28 | 91.01 | 88.57 | 2.60 |
γ-六六六 | 15.044 | 73.56 | 84.2 | 89.19 | 82.32 | 9.70 |
δ-六六六 | 16.185 | 92.51 | 93.03 | 89.56 | 91.70 | 2.04 |
百菌清 | 16.431 | 88.1 | 81.12 | 83.21 | 84.14 | 4.26 |
甲基对硫磷 | 18.268 | 80.25 | 85.37 | 88.65 | 84.76 | 4.99 |
马拉硫磷 | 20.492 | 76.32 | 81.39 | 87.91 | 81.87 | 7.10 |
毒死蜱 | 20.955 | 76.83 | 80.19 | 82.79 | 79.94 | 3.74 |
对硫磷 | 20.955 | 85.99 | 81.74 | 84.09 | 83.94 | 2.54 |
P,P-滴滴伊 | 25.220 | 70.17 | 85.22 | 81.03 | 78.81 | 9.86 |
O,P-滴滴涕 | 26.681 | 79.92 | 84.89 | 77.25 | 80.69 | 4.81 |
P,P-滴滴滴 | 26.765 | 89.09 | 85.08 | 88.84 | 87.67 | 2.56 |
P,P-滴滴涕 | 27.848 | 80.88 | 86.13 | 90.21 | 85.74 | 5.46 |
苯并(α)芘 | 33.691 | 65.36 | 60.21 | 68.89 | 64.82 | 6.73 |
表2加标水样过C18萃取盘的回收率及RSD(n = 3)
名称 | 出峰时间(min) | 回收率(%) | ||||
1 | 2 | 3 | 平均 | RSD | ||
六氯丁二烯 | 6.294 | 54.48 | 51.83 | 56.51 | 54.27 | 4.32 |
敌敌畏 | 6.517 | 84.17 | 99.24 | 98.47 | 93.96 | 9.03 |
克百威 | 7.048 | 77 | 83.57 | 77.87 | 79.48 | 4.49 |
溴氰菊酯 | 9.751 | 74.78 | 82.1 | 80.56 | 79.15 | 4.88 |
α-六六六 | 13.573 | 88.86 | 99.11 | 90.68 | 92.88 | 5.89 |
乐果 | 14.187 | 77.23 | 73.33 | 75.51 | 75.36 | 2.59 |
阿特拉津 | 14.669 | 99.97 | 95.07 | 92.56 | 95.87 | 3.93 |
β-六六六 | 14.772 | 99.19 | 90.21 | 90.05 | 93.15 | 5.62 |
γ-六六六 | 15.044 | 90.51 | 95.29 | 93.36 | 93.05 | 2.58 |
δ-六六六 | 16.185 | 107.90 | 104.60 | 99.08 | 103.86 | 4.29 |
百菌清 | 16.431 | 91.92 | 87.54 | 89.27 | 89.58 | 2.46 |
甲基对硫磷 | 18.268 | 97.24 | 95.49 | 93.89 | 95.54 | 1.75 |
马拉硫磷 | 20.492 | 89.6 | 93.36 | 98.94 | 93.97 | 5.00 |
毒死蜱 | 20.955 | 96.94 | 98.06 | 102.97 | 99.32 | 3.23 |
对硫磷 | 20.955 | 96.57 | 95.67 | 101.04 | 97.76 | 2.94 |
P,P-滴滴伊 | 25.220 | 86.74 | 87.03 | 83.85 | 85.87 | 2.05 |
O,P-滴滴涕 | 26.681 | 88.99 | 88.67 | 85.08 | 87.58 | 2.48 |
P,P-滴滴滴 | 26.765 | 89.03 | 84.08 | 93.04 | 88.72 | 5.06 |
P,P-滴滴涕 | 27.848 | 93.53 | 96.05 | 85.77 | 91.78 | 5.84 |
苯并(α)芘 | 33.691 | 93.77 | 98.10 | 91.45 | 94.44 | 3.57 |