图1 凝胶净化方法
表1定量和定性选择离子
序号 | 化合物名称 | RT/min | 定量离子 | 定性离子1 | 定性离子2 |
1 | N-亚硝基二甲胺 | 5.19 | 42 | 74 | 43 |
2 | 2-氟酚(SS) | 7.62 | 64 | 112 | 92 |
3 | 苯酚-D6(SS) | 9.11 | 99 | 71 | --- |
4 | 苯酚 | 9.13 | 94 | 66 | 40 |
5 | 双(2-氯苯酚)醚 | 9.23 | 93 | 63 | 65 |
6 | 2-氯苯酚 | 9.28 | 128 | 130 | 64 |
7 | 1,3-二氯苯 | 9.50 | 146 | 111 | 75 |
8 | 1,4-二氯苯-D4(IS1) | 9.60 | 150 | 115 | --- |
9 | 1,4-二氯苯 | 9.63 | 146 | 148 | 111 |
10 | 1,2-二氯苯 | 9.85 | 146 | 148 | 111 |
11 | 二(2-氯异丙基)醚 | 10.03 | 121 | 107 | 77 |
12 | 2-甲基苯酚 | 10.05 | 108 | 107 | 77 |
13 | N-亚硝基二正丙胺 | 10.27 | 43 | 70 | 130 |
14 | 4-甲基苯酚 | 10.30 | 107 | 108 | 77 |
15 | 六氯乙烷 | 10.37 | 117 | 109 | 201 |
16 | 硝基苯-D5(SS) | 10.51 | 82 | 128 | 54 |
17 | 硝基苯 | 10.54 | 77 | 123 | 51 |
18 | 异佛尔酮 | 10.91 | 82 | 138 | 54 |
19 | 2-硝基苯酚 | 11.04 | 139 | 65 | 81 |
20 | 2,4-二甲基苯酚 | 11.12 | 107 | 122 | 77 |
21 | 二(2-氯乙氧基)甲烷 | 11.27 | 93 | 63 | 123 |
22 | 2,4-二氯苯酚 | 11.44 | 162 | 164 | 63 |
23 | 1,2,4-三氯苯 | 11.53 | 147 | 74 | 109 |
24 | 萘-d8(IS2) | 11.62 | 136 | 108 | --- |
25 | 萘 | 11.66 | 128 | 129 | --- |
26 | 4-氯苯胺 | 11.79 | 127 | 129 | 65 |
27 | 六氯丁二烯 | 11.82 | 118 | 260 | 223 |
28 | 4-氯-3-甲基苯酚 | 12.72 | 107 | 142 | 144 |
29 | 2-甲基萘 | 12.96 | 115 | 141 | 142 |
30 | 六氯环戊二烯 | 13.28 | 130 | 235 | 239 |
31 | 2,4,6-三氯苯酚 | 13.70 | 196 | 198 | 200 |
32 | 2,4,5-三氯苯酚 | 13.81 | 196 | 198 | 200 |
33 | 2-氟联苯(SS) | 13.91 | 172 | 171 | 170 |
34 | 2-氯萘 | 14.25 | 162 | 127 | ---- |
35 | 2-硝基苯胺 | 14.70 | 138 | 65 | 92 |
36 | 邻苯二甲酸二甲酯 | 15.40 | 163 | 77 | --- |
37 | 2,6-二硝基甲苯 | 15.69 | 165 | 63 | 89 |
38 | 3-硝基苯胺 | 15.70 | 65 | 92 | 138 |
39 | 苊烯 | 15.73 | 152 | 76 | --- |
40 | 苊-d10(IS3) | 16.37 | 164 | 162 | 160 |
41 | 苊 | 16.52 | 153 | 76 | --- |
42 | 2,4-二硝基苯酚 | 17.03 | 184 | 63 | 154 |
43 | 二苯并呋喃 | 17.43 | 168 | 139 | --- |
44 | 2,4-二硝基甲苯 | 17.68 | 165 | 89 | 63 |
45 | 4-硝基苯酚 | 17.76 | 139 | 109 | 65 |
46 | 邻苯二甲酸二乙酯 | 19.20 | 149 | 177 | --- |
47 | 芴 | 19.36 | 166 | 163 | 82 |
48 | 4-氯苯基苯甲醚 | 19.58 | 204 | 141 | 77 |
49 | 4-硝基苯胺 | 19.91 | 65 | 138 | 108 |
50 | 4,6-二硝基-2-甲基苯酚 | 20.02 | 198 | 51 | 105 |
51 | 偶氮苯 | 20.54 | 77 | 182 | 51 |
52 | 2,4,6-三溴苯酚(SS) | 20.90 | 332 | 62 | 143 |
53 | 4-溴二苯基醚 | 21.63 | 250 | 141 | 77 |
54 | 六氯苯 | 22.72 | 284 | 286 | 282 |
55 | 五氯苯酚 | 24.36 | 266 | 184 | --- |
56 | 菲-d10(IS4) | 25.48 | 188 | 80 | --- |
57 | 菲 | 25.65 | 178 | 176 | 179 |
58 | 蒽 | 26.01 | 178 | 176 | 179 |
59 | 咔唑 | 27.60 | 167 | 166 | 139 |
60 | 邻苯二甲酸二正丁酯 | 31.12 | 149 | 150 | 76 |
61 | 荧蒽 | 34.43 | 202 | 200 | 203 |
62 | 芘 | 36.03 | 202 | 200 | 201 |
63 | 4,4’-三联苯-D14(SS) | 38.10 | 244 | 245 | 243 |
64 | 邻苯二甲酸丁基苄基酯 | 42.60 | 149 | 91 | 206 |
65 | 苯并(α)蒽 | 45.46 | 228 | 226 | 229 |
66 | ?-d12(IS5) | 45.50 | 240 | 236 | 241 |
67 | 屈 | 45.70 | 228 | 226 | 229 |
68 | 邻苯二甲酸二(2-二乙基己基)酯 | 47.48 | 149 | 167 | 57 |
69 | 邻苯二甲酸二正辛酯 | 52.34 | 149 | 279 | --- |
70 | 苯并(b)荧蒽 | 53.14 | 252 | 126 | 250 |
71 | 苯并(k)荧蒽 | 53.35 | 252 | 126 | 250 |
72 | 苯并(α)芘 | 55.22 | 252 | 250 | 253 |
73 | 苝-d12(IS6) | 55.61 | 264 | 260 | 263 |
74 | 茚并(1,2,3-cd)芘 | 61.94 | 276 | 138 | 274 |
75 | 二苯并(ah)蒽 | 62.26 | 278 | 139 | 276 |
76 | 苯并(ghi)苝 | 63.31 | 276 | 138 | 274 |
图2 76种半挥发性有机污染物总离子流谱图
图3 土壤样品加标色谱图
表2 加标样品回收率
物质名称 | 回收率(%) | 平均值(%) | RSD (%) | |||||
1 | 2 | 3 | 4 | 5 | 6 | |||
N-亚硝基二甲胺 | 48.2 | 48.8 | 49.3 | 51.8 | 47.8 | 55.6 | 50.3 | 5.9 |
2-氟酚(SS) | 53.9 | 60.8 | 51.4 | 54.1 | 58.2 | 54.6 | 55.5 | 6.1 |
苯酚-D6(SS) | 52.8 | 54.0 | 54.2 | 51.0 | 56.5 | 50.4 | 53.2 | 4.2 |
苯酚 | 54.5 | 59.0 | 64.6 | 62.8 | 59.2 | 65.8 | 61.0 | 6.9 |
双(2-氯苯酚)醚 | 53.1 | 65.0 | 58.7 | 60.3 | 55.9 | 57.6 | 58.4 | 6.9 |
2-氯苯酚 | 56.1 | 64.1 | 53.4 | 54.5 | 58.1 | 62.6 | 58.1 | 7.5 |
1,3-二氯苯 | 54.0 | 53.4 | 57.5 | 60.8 | 53.9 | 55.1 | 55.8 | 5.1 |
1,4-二氯苯 | 59.3 | 57.7 | 51.9 | 52.8 | 48.0 | 47.8 | 52.9 | 9.1 |
1,2-二氯苯 | 50.9 | 49.2 | 44.4 | 51.6 | 51.7 | 45.3 | 48.9 | 6.6 |
二(2-氯异丙基)醚 | 58.3 | 51.1 | 59.7 | 71.8 | 59.9 | 59.0 | 60.0 | 11.1 |
2-甲基苯酚 | 54.9 | 63.2 | 55.9 | 71.9 | 58.2 | 68.8 | 62.2 | 11.3 |
N-亚硝基二正丙胺 | 56.7 | 59.8 | 58.5 | 74.9 | 61.6 | 62.2 | 62.3 | 10.4 |
4-甲基苯酚 | 54.0 | 53.6 | 55.8 | 57.7 | 56.8 | 60.8 | 56.5 | 4.7 |
六氯乙烷 | 59.4 | 53.2 | 68.9 | 61.7 | 58.4 | 53.8 | 59.2 | 9.7 |
硝基苯-D5(SS) | 53.0 | 54.3 | 56.4 | 69.5 | 58.9 | 61.1 | 58.9 | 10.2 |
硝基苯 | 51.9 | 47.2 | 54.9 | 63.8 | 59.7 | 60.2 | 56.3 | 10.9 |
异佛尔酮 | 52.4 | 63.6 | 59.5 | 53.5 | 68.6 | 64.5 | 60.4 | 10.7 |
2-硝基苯酚 | 60.3 | 57.5 | 55.1 | 56.9 | 59.0 | 53.6 | 57.1 | 4.3 |
2,4-二甲基苯酚 | 57.3 | 53.1 | 45.0 | 47.6 | 57.7 | 55.6 | 52.7 | 10.0 |
二(2-氯乙氧基)甲烷 | 63.8 | 61.9 | 56.9 | 74.9 | 63.4 | 73.8 | 65.8 | 10.8 |
2,4-二氯苯酚 | 65.8 | 56.9 | 68.1 | 59.1 | 66.3 | 62.3 | 63.1 | 7.0 |
1,2,4-三氯苯 | 52.3 | 56.9 | 51.6 | 54.4 | 60.1 | 50.5 | 54.3 | 6.7 |
萘 | 53.5 | 50.7 | 58.4 | 50.2 | 58.9 | 53.6 | 54.2 | 6.8 |
4-氯苯胺 | 51.2 | 48.0 | 50.1 | 42.8 | 46.4 | 49.1 | 47.9 | 6.3 |
六氯丁二烯 | 51.4 | 49.0 | 43.9 | 50.0 | 40.1 | 46.0 | 46.7 | 9.1 |
4-氯-3-甲基苯酚 | 68.5 | 60.3 | 68.6 | 73.1 | 74.3 | 70.5 | 69.2 | 7.2 |
2-甲基萘 | 65.4 | 59.3 | 61.1 | 53.7 | 57.6 | 66.9 | 60.7 | 8.1 |
六氯环戊二烯 | 60.7 | 62.7 | 66.7 | 58.6 | 59.8 | 64.1 | 62.1 | 4.8 |
2,4,6-三氯苯酚 | 68.7 | 57.4 | 60.4 | 60.2 | 61.5 | 60.4 | 61.4 | 6.2 |
2,4,5-三氯苯酚 | 62.5 | 67.1 | 66.8 | 61.2 | 62.1 | 70.9 | 65.1 | 5.8 |
2-氟联苯(SS) | 60.4 | 53.1 | 55.8 | 56.1 | 62.9 | 61.8 | 58.4 | 6.7 |
2-氯萘 | 50.5 | 65.9 | 64.5 | 59.3 | 59.0 | 71.5 | 61.8 | 11.7 |
2-硝基苯胺 | 62.5 | 62.6 | 78.6 | 74.4 | 68.6 | 73.5 | 70.0 | 9.4 |
邻苯二甲酸二甲酯 | 72.0 | 63.1 | 71.8 | 70.8 | 73.4 | 79.6 | 71.8 | 7.4 |
2,6-二硝基甲苯 | 58.7 | 62.5 | 75.6 | 67.4 | 75.3 | 75.2 | 69.1 | 10.7 |
苊烯 | 59.0 | 53.3 | 59.5 | 54.2 | 57.3 | 65.8 | 58.2 | 7.7 |
3-硝基苯胺 | 46.3 | 52.6 | 54.6 | 47.6 | 53.5 | 53.5 | 51.4 | 6.8 |
苊 | 56.5 | 61.5 | 58.7 | 66.0 | 76.5 | 67.2 | 64.4 | 11.2 |
2,4-二硝基苯酚 | 43.1 | 38.3 | 43.0 | 42.1 | 45.8 | 45.1 | 42.9 | 6.2 |
二苯并呋喃 | 63.4 | 62.6 | 64.3 | 74.6 | 68.1 | 79.5 | 68.8 | 10.0 |
2,4-二硝基甲苯 | 54.7 | 55.0 | 63.8 | 65.3 | 59.9 | 71.3 | 61.7 | 10.4 |
4-硝基苯酚 | 61.5 | 73.6 | 84.3 | 73.6 | 69.5 | 77.5 | 73.3 | 10.4 |
邻苯二甲酸二乙酯 | 80.5 | 78.0 | 77.2 | 80.2 | 82.3 | 73.8 | 78.7 | 3.8 |
芴 | 67.1 | 71.3 | 66.3 | 77.9 | 70.9 | 82.0 | 72.6 | 8.5 |
4-氯苯基苯甲醚 | 66.0 | 70.4 | 66.3 | 78.8 | 71.2 | 68.9 | 70.3 | 6.7 |
4-硝基苯胺 | 53.3 | 50.4 | 50.4 | 58.4 | 50.7 | 47.4 | 51.8 | 7.2 |
4,6-二硝基-2-甲基苯酚 | 58.9 | 60.0 | 68.7 | 59.3 | 73.7 | 70.9 | 65.3 | 10.1 |
偶氮苯 | 68.6 | 61.2 | 66.8 | 80.8 | 72.5 | 73.1 | 70.5 | 9.4 |
2,4,6-三溴苯酚(SS) | 70.6 | 77.9 | 77.5 | 74.2 | 71.0 | 64.0 | 72.5 | 7.2 |
4-溴二苯基醚 | 80.3 | 79.0 | 77.9 | 83.7 | 78.2 | 71.3 | 78.4 | 5.2 |
五氯苯酚 | 74.6 | 70.6 | 75.6 | 69.1 | 76.8 | 67.9 | 72.4 | 5.1 |
六氯苯 | 71.4 | 71.1 | 69.3 | 81.4 | 77.3 | 90.1 | 76.8 | 10.4 |
菲 | 88.3 | 88.8 | 84.7 | 100.6 | 89.5 | 84.0 | 89.3 | 6.7 |
蒽 | 74.1 | 77.5 | 68.7 | 82.2 | 78.2 | 92.8 | 78.9 | 10.4 |
咔唑 | 85.4 | 95.5 | 80.1 | 99.2 | 92.7 | 75.6 | 88.1 | 10.5 |
邻苯二甲酸二正丁酯 | 112.4 | 123.4 | 101.7 | 117.5 | 121.0 | 105.4 | 113.6 | 7.6 |
荧蒽 | 95.0 | 87.8 | 91.8 | 81.1 | 80.0 | 92.1 | 88.0 | 7.0 |
芘 | 74.2 | 86.0 | 72.8 | 83.9 | 87.3 | 85.0 | 81.5 | 7.8 |
4,4’-三联苯-D14(SS) | 78.7 | 78.7 | 73.7 | 70.7 | 81.4 | 79.1 | 77.1 | 5.2 |
邻苯二甲酸丁基苄基酯 | 80.5 | 95.6 | 76.4 | 79.9 | 92.4 | 96.2 | 86.8 | 10.2 |
苯并(α)蒽 | 73.5 | 88.8 | 70.7 | 86.0 | 82.3 | 77.9 | 79.9 | 8.9 |
屈 | 76.2 | 91.5 | 73.6 | 88.5 | 83.7 | 91.4 | 84.2 | 9.2 |
邻苯二甲酸二(2-二乙基己基)酯 | 111.2 | 114.4 | 116.0 | 118.3 | 108.3 | 115.0 | 113.9 | 3.1 |
邻苯二甲酸二正辛酯 | 107.6 | 111.8 | 115.0 | 104.4 | 115.7 | 108.7 | 110.5 | 4.0 |
苯并(b)荧蒽 | 75.2 | 93.4 | 85.1 | 90.6 | 88.1 | 83.1 | 85.9 | 7.5 |
苯并(k)荧蒽 | 71.2 | 93.8 | 70.5 | 88.9 | 87.2 | 79.5 | 81.9 | 11.8 |
苯并(α)芘 | 77.6 | 94.7 | 74.5 | 70.6 | 88.5 | 84.4 | 81.7 | 11.1 |
茚并(1,2,3-cd)芘 | 85.1 | 92.4 | 84.4 | 91.0 | 85.3 | 100.3 | 89.8 | 6.9 |
二苯并(ah)蒽 | 81.2 | 84.2 | 80.8 | 94.1 | 84.1 | 95.5 | 86.7 | 7.5 |
苯并(ghi)苝 | 87.6 | 85.8 | 80.3 | 85.6 | 73.6 | 78.5 | 81.9 | 6.6 |