图1.弗罗里硅土柱净化方法
表1 有机氯定量和定性选择离子
序号 | 化合物中文名称 | 扫描 | RT | 定量离子 | 定性离子1 | 定性离子2 | 定性离子3 |
1 | а-六六六 | SIM | 9.5 | 219 | 181 | 183 | 217 |
2 | 六氯苯 | SIM | 9.6 | 284 | 286 | 282 | 288 |
3 | β-六六六 | SIM | 10.0 | 181 | 183 | 219 | 109 |
4 | 林丹 | SIM | 10.2 | 181 | 182.9 | 219 | 217 |
5 | 菲-d10 (IS) | SIM | 10.6 | 188 | 189 | 184 | 94 |
6 | 百菌清 | SIM | 10.6 | 266 | 264 | 268 | 187 |
7 | δ-六六六 | SIM | 10.8 | 181 | 219 | 183 | 217 |
8 | 七氯 | SIM | 12.0 | 272 | 274 | 100 | 270 |
9 | 敌草索 | SIM | 13.0 | 301 | 299 | 303 | 332 |
10 | 艾氏剂 | SIM | 13.0 | 263 | 265 | 261 | 66 |
11 | 环氧七氯-B | SIM | 14.1 | 353 | 354.8 | 350.8 | 81 |
12 | 环氧七氯-A | SIM | 14.2 | 353 | 354.8 | 350.8 | 81 |
13 | 反式-氯丹 | SIM | 14.8 | 373 | 375 | 377 | 371 |
14 | o,p'-DDE | SIM | 14.9 | 246 | 248 | 317.9 | 315.9 |
15 | 顺式-氯丹 | SIM | 15.2 | 373 | 375 | 377 | 371 |
16 | β-硫丹 | SIM | 15.2 | 241 | 195 | 239 | 243 |
17 | p,p'-DDE | SIM | 15.9 | 246 | 318 | 248 | 316 |
18 | 对三联苯-D14(SS) | SIM | 16.1 | 244 | 245 | 122 | 240 |
19 | 狄氏剂 | SIM | 16.1 | 79 | 264 | 263 | 277 |
20 | o,p'-DDD | SIM | 16.1 | 235 | 237 | 165 | 236 |
21 | 异狄氏剂 | SIM | 16.7 | 317 | 263 | 281 | 67 |
22 | а-硫丹 | SIM | 17.1 | 195 | 241 | 237 | 207 |
23 | p,p'-DDD | SIM | 17.3 | 235 | 237 | 165 | 236 |
24 | o,p'-DDT | SIM | 17.4 | 235 | 237 | 165 | 236 |
25 | p,p'-DDT | SIM | 18.5 | 235 | 237 | 165 | 236 |
26 | 屈-D12(IS) | SIM | 20.2 | 240 | 236 | 241 | 120 |
27 | 甲氧滴滴涕 | SIM | 20.4 | 227 | 228 | 113 | 212 |
28 | 灭蚁灵 | SIM | 22.1 | 272 | 274 | 270 | 237 |
图2 有机氯标准液总离子流谱图
图3 6个平行加标离子流重叠图
表2弗罗里硅土柱净化加标样品回收率
名称 | 回收率1,% | 平均值,% | RSD,% | |||||
1 | 2 | 3 | 4 | 5 | 6 | |||
а-六六六 | 85.2 | 82.1 | 86.3 | 81.7 | 85.7 | 83.2 | 84.03 | 2.33 |
六氯苯 | 72.2 | 75.1 | 73.6 | 70.9 | 74.3 | 72.8 | 73.15 | 2.07 |
β-六六六 | 102.8 | 109.1 | 110.4 | 108.4 | 100.6 | 107.9 | 106.53 | 3.66 |
林丹 | 80.3 | 85.7 | 85.9 | 80.8 | 83.5 | 85.5 | 83.62 | 3.03 |
百菌清 | 84.2 | 80.6 | 85.8 | 84.7 | 85.3 | 82.2 | 83.80 | 2.39 |
δ-六六六 | 93.5 | 90.6 | 91.1 | 84.1 | 85.9 | 94.1 | 89.88 | 4.51 |
七氯 | 91.6 | 90.6 | 92.7 | 85.3 | 88.7 | 82.6 | 88.58 | 4.42 |
敌草索 | 92.3 | 90.5 | 85.9 | 88.1 | 94.4 | 84.3 | 89.25 | 4.32 |
艾氏剂 | 85.4 | 80.7 | 81.6 | 86.6 | 87.9 | 83.4 | 84.27 | 3.38 |
环氧七氯-B | 92.2 | 90.1 | 87.2 | 88.9 | 85.6 | 87.4 | 88.57 | 2.66 |
环氧七氯-A | 93.9 | 92.3 | 88.7 | 85.1 | 90.6 | 87.9 | 89.75 | 3.54 |
反式-氯丹 | 92.5 | 90.3 | 85.5 | 86.9 | 91.4 | 88.4 | 89.17 | 3.03 |
o,p'-DDE | 102 | 97.7 | 103.3 | 93.3 | 102.7 | 101.2 | 100.03 | 3.84 |
顺式-氯丹 | 95.1 | 90.3 | 86.3 | 96.3 | 85.7 | 90.2 | 90.65 | 4.82 |
β-硫丹 | 90.8 | 87.8 | 84.5 | 94.5 | 93.3 | 92.6 | 90.58 | 4.18 |
p,p'-DDE | 103.2 | 98.2 | 94.5 | 103.5 | 101.7 | 102.3 | 100.57 | 3.51 |
对三联苯-D14(SS) | 98.2 | 97.8 | 96.4 | 99.2 | 97.4 | 97.1 | 97.68 | 0.99 |
狄氏剂 | 103.4 | 102.2 | 94.8 | 104.8 | 100 | 95.7 | 100.15 | 4.11 |
o,p'-DDD | 105.2 | 101.2 | 96.5 | 106.5 | 101.8 | 103.5 | 102.45 | 3.45 |
异狄氏剂 | 85 | 82.1 | 91.5 | 87.2 | 80.9 | 87.8 | 85.75 | 4.57 |
а-硫丹 | 102.4 | 100.4 | 96 | 104.8 | 101.2 | 98.8 | 100.60 | 3.00 |
p,p'-DDD | 104.3 | 103.2 | 96.7 | 106.7 | 106.1 | 101.6 | 103.10 | 3.54 |
o,p'-DDT | 107.9 | 102.8 | 99 | 109 | 105.3 | 101 | 104.17 | 3.77 |
p,p'-DDT | 110.6 | 100.6 | 96.8 | 106.8 | 103.3 | 101.1 | 103.20 | 4.74 |
甲氧滴滴涕 | 105 | 112.1 | 107.9 | 111.4 | 116.2 | 106.2 | 109.80 | 3.83 |
灭蚁灵 | 91.8 | 90.2 | 93.2 | 83.2 | 88.5 | 85.2 | 88.68 | 4.36 |