序号 | 化合物名称 | 保留时间/min | 定量/定性离子 |
1 | 苯酚 | 8.999 | 94/66/65 |
2 | 2-氯酚 | 9.136 | 128/64/130 |
3 | 邻甲苯酚 | 9.904 | 108/107/79 |
4/5 | 间/对甲苯酚 | 10.15 | 107/108/77 |
6 | 2,硝基苯酚 | 10.862 | 139/63/109 |
7 | 2,4 二甲酚 | 10.959 | 122/107/121 |
8 | 2,4二氯酚 | 11.22 | 162/164/63 |
9 | 2,6二氯酚 | 11.589 | 162/164/63 |
10 | 4-氯-3甲酚 | 12.442 | 142/107/144 |
11 | 2.4.6三氯酚 | 13.366 | 196/168/200 |
12 | 2.4.5三氯酚 | 13.448 | 196/168/97 |
13 | 2,4二硝基苯酚 | 16.159 | 184/63/53 |
14 | 对硝基苯酚 | 16.650 | 139/65/109 |
15 | 2,3,4,5四氯酚 | 17.262 | 232/230/234 |
16 | 2,3,5,6四氯酚 | 17.363 | 232/230/234 |
17 | 2,3,4,6四氯酚 | 17.474 | 232/230/234 |
18 | 2-甲基4.6二硝基苯酚 | 18.716 | 198/105/121 |
19 | 五氯酚 | 21.21 | 268/266/264 |
20 | 地乐酚 | 22.005 | 211/165/147 |
21 | 环己基4,6二硝基酚 | 26.151 | 231/185/193 |
表1
影响因素 | 萃取温度(A) | 萃取溶剂(B) | 样品含水量(C) |
水平一 | 100℃(A1) | 二氯甲烷正己烷2+1(v/v)(B1) | >1%(300摄氏度,4小时灼烧)(C1) |
水平二 | 120℃(A2) | 乙酸乙酯二氯甲烷(B2) | 2%~5%(风干土壤)(C2) |
水平三 | —— | —— | 15%~20% 新鲜土壤(C3) |
正交实验表 | |||||||||||
实验1 | 实验2 | 实验3 | 实验4 | 实验 5 | 实验 6 | 实验7 | 实验8 | 实验9 | 实验10 | 实验11 | 实验12 |
A1B1C1 | A1B1C2 | A1B1C3 | A1B2C1 | A1B2C2 | A1B2C3 | A2B1C1 | A2B1C2 | A2B1C3 | A2B2C1 | A2B2C2 | A2B2C3 |
表2
表3
表5
序号 | 化合物 | 线性方程 | R | 检出限(mg/kg) |
1 | 苯酚 | y=374594.6x+1054191.0 | 0.9980 | 0.04 |
2 | 2-氯酚 | y=454159.9x+486424.1 | 0.9999 | 0.03 |
3 | 邻甲苯酚 | y=274504.8x+1037621.2 | 0.9971 | 0.03 |
4/5 | 间/对甲苯酚 | y=500164.2x+2202597.3 | 0.9986 | 0.02 |
6 | 2-硝基苯酚 | y=248151.2x-136398.1 | 0.9996 | 0.04 |
7 | 2,4 -二甲酚 | y=285574.2x+1002052.8 | 0.9986 | 0.02 |
8 | 2,4-二氯酚 | y=294678.0x+922262.3 | 0.9974 | 0.02 |
9 | 2,6-二氯酚 | y=295683.7x+947597.8 | 0.9973 | 0.02 |
10 | 4-氯-3-甲酚 | y=282311.1x+546868.0 | 0.9994 | 0.03 |
11 | 2,4,6三氯酚 | y=286951.6x+378680.7 | 0.9983 | 0.03 |
12 | 2,4,5三氯酚 | y=307197.4x+372523.6 | 0.9988 | 0.03 |
13 | 2,4-二硝基苯酚 | y=67400.5x-250717.8 | 0.9951 | 0.07 |
14 | 对硝基苯酚 | y=18310.6x-684985.7 | 0.9973 | 0.06 |
15 | 2,3,4,5四氯酚 | y=361943.0x+522455.6 | 0.9991 | 0.03 |
16 | 2,3,5,6四氯酚 | y=347889.9x-313854.3 | 0.9996 | 0.03 |
17 | 2,3,4,6四氯酚 | y=340670.4x-217155.5.1 | 0.9996 | 0.03 |
18 | 2 -甲基4.6二硝基苯酚 | y=205003.4x-859860.8 | 0.9952 | 0.06 |
19 | 五氯酚 | y=182972.3x-294480.6 | 0.9992 | 0.03 |
20 | 地乐酚 | y=303031.6x-1042031.9 | 0.9975 | 0.03 |
21 | 环己基4,6二硝基酚 | y=38979.3x+1759753.3 | 0.9952 | 0.05 |
序号 | 化合物名称 | 6组平行样回收率/% | 平均值/% | RSD/% | |||||
1 | 2 | 3 | 4 | 5 | 6 | ||||
1 | 苯酚 | 73.7 | 74.5 | 72.4 | 78.3 | 70.3 | 72.2 | 73.6 | 3.7 |
2 | 2-氯酚 | 70.5 | 76.1 | 72.2 | 79.1 | 77.6 | 71.8 | 74.5 | 4.7 |
3 | 邻甲苯酚 | 71.4 | 73.1 | 78.4 | 80.5 | 79.2 | 73.9 | 76.1 | 4.9 |
4/5 | 间/对甲苯酚 | 74.7 | 75.6 | 80.3 | 84.0 | 81.4 | 76.2 | 78.7 | 4.7 |
6 | 2-硝基苯酚 | 72.7 | 76.9 | 83.3 | 90.9 | 103.8 | 83.4 | 85.2 | 13.0 |
7 | 2,4 -二甲酚 | 74.4 | 69.9 | 71.3 | 75.3 | 71.4 | 83.4 | 74.3 | 6.6 |
8 | 2,4-二氯酚 | 70.1 | 74.3 | 80.6 | 93.2 | 87.9 | 68.4 | 79.1 | 12.6 |
9 | 2,6-二氯酚 | 79.8 | 79.0 | 78.7 | 91.0 | 87.6 | 84.3 | 83.4 | 6.1 |
10 | 4-氯-3-甲酚 | 73.8 | 75.0 | 88.5 | 98.6 | 89.7 | 82.6 | 84.7 | 11.2 |
11 | 2,4,6三氯酚 | 79.3 | 77.3 | 91.7 | 97.1 | 96.9 | 87.0 | 88.2 | 9.7 |
12 | 2,4,5三氯酚 | 77.5 | 83.6 | 101.5 | 99.4 | 103.6 | 102.6 | 94.7 | 11.8 |
13 | 2,4-二硝基苯酚 | 79.8 | 83.3 | 76.1 | 75.7 | 78.5 | 104.9 | 83.1 | 13.3 |
14 | 对硝基苯酚 | 72.3 | 72.9 | 73.3 | 80.9 | 93.8 | 105.8 | 83.2 | 16.6 |
15 | 2,3,4,5四氯酚 | 75.4 | 75.9 | 85.4 | 76.9 | 71.6 | 86.2 | 78.6 | 7.5 |
16 | 2,3,5,6四氯酚 | 82.1 | 83.2 | 88.9 | 72.4 | 79.8 | 75.4 | 80.3 | 7.3 |
17 | 2,3,4,6四氯酚 | 76.5 | 81.8 | 88.1 | 74.8 | 77.7 | 82.3 | 80.2 | 6.1 |
18 | 2 -甲基4.6二硝基苯酚 | 76.5 | 86.8 | 90.8 | 101.2 | 107.2 | 96.7 | 93.2 | 11.7 |
19 | 五氯酚 | 92.1 | 97.3 | 89.0 | 85.6 | 94.2 | 93.2 | 91.9 | 4.5 |
20 | 地乐酚 | 87.4 | 84.9 | 82.4 | 84.0 | 76.3 | 89.6 | 84.1 | 5.5 |
21 | 环己基4,6二硝基酚 | 95.5 | 92.8 | 112.7 | 102.9 | 90.8 | 112.3 | 101.2 | 9.6 |