取*****混标1.0mL,过GCB/PSA柱(500mg/6mL,厂家: )用乙腈+甲苯=3+1洗脱,分段收集第一次5mL,第二次5mL,第三次5mL;然后于35℃氮吹,定容1mL。 | ||||||
5mL | 5mL | 5mL | ||||
化合物名称 | 保留时间 (分) | 浓度 | 浓度 | 浓度 | 原液浓度 | 回收率(%) |
1、甲胺磷 | 8.106 | 916.1 | 321.5 | 0.0 | 2500.0 | 49.5 |
2、敌敌畏 | 8.31 | 1046.3 | 85.4 | 0.0 | 2500.0 | 45.3 |
3、氧乐果 | 12.788 | 412.9 | 5.2 | 0.0 | 1018.9 | 41.0 |
4、甲拌磷 | 14.637 | 114.1 | 14.5 | 0.0 | 499.4 | 25.8 |
5、α-666 | 14.79 | 442.1 | 55.4 | 0.0 | 999.6 | 49.8 |
6、六氯苯 | 0 | 0.0 | 0.0 | 6.6 | 499.5 | 1.3 |
7、乐果 | 15.338 | 730.7 | 66.2 | 0.0 | 2462.9 | 32.4 |
8、β-666 | 15.903 | 516.3 | 67.5 | 0.0 | 1001.4 | 58.3 |
9、γ-666(林丹) | 16.145 | 457.3 | 75.4 | 5.8 | 999.6 | 53.9 |
10、五氯硝基苯 | 16.38 | 141.0 | 154.4 | 7.9 | 999.2 | 30.4 |
11、二嗪磷(二嗪农) | 17.107 | 256.7 | 34.5 | 0.0 | 999.4 | 29.1 |
12、δ-666 | 17.266 | 540.2 | 67.7 | 0.0 | 998.3 | 60.9 |
13、甲基毒死蜱 | 19.407 | 279.7 | 58.2 | 0.5 | 1000.0 | 33.8 |
14、甲基对硫磷 | 19.391 | 170.4 | 19.1 | 0.0 | 500.0 | 37.9 |
15、七氯 | 19.657 | 163.8 | 40.0 | 0.0 | 500.0 | 40.8 |
16、杀螟硫磷 | 21.018 | 462.2 | 56.0 | 0.0 | 1495.7 | 34.6 |
17、甲基嘧啶磷 | 21.268 | 285.2 | 32.9 | 0.0 | 998.9 | 31.8 |
18、艾氏剂 | 21.586 | 398.5 | 139.7 | 0.0 | 1000.0 | 53.8 |
19、马拉硫磷 | 21.829 | 260.5 | 22.3 | 0.0 | 1000.0 | 28.3 |
20、倍硫磷 | 22.209 | 322.4 | 33.1 | 0.0 | 1000.0 | 35.5 |
21、对硫磷 | 22.379 | 143.2 | 16.1 | 0.0 | 500.0 | 31.8 |
22、三氯杀螨醇 | 22.329 | 715.1 | 117.0 | 0.0 | 1482.7 | 56.1 |
23、毒死蜱 | 22.359 | 339.5 | 60.0 | 0.0 | 1000.0 | 40.0 |
24、水胺硫磷 | 22.759 | 220.4 | 17.2 | 0.0 | 500.0 | 47.5 |
25、噻虫嗪 | 23.342 | 995.4 | 101.4 | 0.0 | 2504.9 | 43.8 |
26、甲基异柳磷 | 24.083 | 123.1 | 14.1 | 0.0 | 499.3 | 27.5 |
27、环氧七氯 | 24.126 | 420.3 | 70.1 | 0.0 | 999.9 | 49.0 |
28、喹硫磷 | 25.2 | 240.2 | 32.3 | 0.0 | 1000.0 | 27.2 |
29、氟虫腈 | 25.366 | 317.8 | 32.3 | 0.0 | 1000.3 | 35.0 |
30、腐霉利 | 25.577 | 500.1 | 54.0 | 0.0 | 1000.0 | 55.4 |
31、反-氯丹 | 25.7 | 455.0 | 97.3 | 1.0 | 1000.0 | 55.3 |
32、噻螨酮 | 25.717 | 775.4 | 107.2 | 0.0 | 2500.0 | 35.3 |
33、α-硫丹 | 26.467 | 1132.2 | 255.4 | 0.0 | 2500.0 | 55.5 |
34、α-氯丹 | 26.751 | 457.5 | 93.8 | 1.0 | 1000.0 | 55.2 |
35、狄氏剂 | 28.296 | 400.8 | 79.8 | 0.0 | 999.5 | 48.1 |
36、PP/-DDE | 28.581 | 468.5 | 129.7 | 1.2 | 999.9 | 59.9 |
37、噻嗪酮 | 29.497 | 553.6 | 66.1 | 0.0 | 1500.0 | 41.3 |
38、β-硫丹 | 30.522 | 1177.8 | 111.4 | 0.0 | 2500.0 | 51.6 |
39、PP/-DDD | 31.645 | 403.0 | 50.3 | 0.0 | 976.8 | 46.4 |
40、OP/-DDT | 31.805 | 383.8 | 67.5 | 0.0 | 1002.8 | 45.0 |
41、硫丹硫酸盐 | 33.671 | 422.1 | 42.8 | 0.0 | 1002.9 | 46.4 |
42、PP/-DDT | 34.22 | 337.2 | 48.2 | 0.0 | 1000.0 | 38.5 |
44、联苯菊酯 | 37.61 | 273.3 | 36.7 | 0.0 | 998.1 | 31.1 |
45、甲氰菊酯 | 37.787 | 436.7 | 27.9 | 0.0 | 1500.0 | 31.0 |
46、氯氟氰菊酯(三氟氯氰菊酯)-1 | 39.236 | 139.1 | 16.3 | 0.0 | 1000.0 | 15.5 |
47、氯氟氰菊酯(三氟氯氰菊酯)-2 | 39.564 | 274.3 | 27.2 | 0.0 | 1000.0 | 30.1 |
48、氯菊酯-1 | 40.606 | 264.8 | 43.1 | 0.0 | 1500.0 | 20.5 |
49、氯菊酯-2 | 40.807 | 403.3 | 41.0 | 0.0 | 1500.0 | 29.6 |
50、哒螨灵(哒螨酮) | 40.725 | 196.8 | 24.6 | 0.0 | 1000.0 | 22.1 |
51、氟氯氰菊酯-1 | 41.332 | 255.1 | 168.2 | 0.0 | 996.9 | 42.5 |
52、氟氯氰菊酯-2 | 41.616 | 161.9 | 15.6 | 0.0 | 500.0 | 35.5 |
53、氟氯氰菊酯-3 | 41.713 | 89.7 | 25.8 | 0.0 | 500.0 | 23.1 |
54、氟氯氰菊酯-4 | 41.713 | 89.7 | 25.8 | 0.0 | 500.0 | 23.1 |
55、氯氰菊酯-1 | 41.883 | 200.2 | 42.1 | 0.0 | 468.0 | 51.8 |
56、氯氰菊酯-2 | 42.012 | 123.7 | 17.0 | 0.0 | 453.1 | 31.1 |
57、氯氰菊酯-3 | 42.109 | 143.0 | 19.6 | 0.0 | 454.3 | 35.8 |
58、氯氰菊酯-4 | 42.174 | 164.0 | 9.4 | 0.0 | 528.6 | 32.8 |
59、氟氰戊菊酯-1 | 42.182 | 355.0 | 40.9 | 0.0 | 1469.3 | 26.9 |
60、氟氰戊菊酯-2 | 42.425 | 366.5 | 61.4 | 0.0 | 1500.0 | 28.5 |
61、氰戊菊酯-1 | 43.013 | 512.1 | 48.2 | 0.0 | 2500.0 | 22.4 |
62、氰戊菊酯-2 | 43.255 | 515.1 | 52.2 | 0.0 | 2524.0 | 22.5 |
63、苯醚甲环唑-1 | 43.488 | 442.3 | 94.7 | 0.0 | 1000.0 | 53.7 |
64、苯醚甲环唑-2 | 43.575 | 371.8 | 66.7 | 0.0 | 1000.0 | 43.9 |
65、溴氰菊酯 | 43.938 | 683.2 | 177.4 | 0.0 | 1000.0 | 86.1 |
我是风儿
第8楼2018/04/17
同理,改用成丙酮+正己烷=1+1洗脱的话,各农药残留的项目回收率如下:
取****混标1.0mL,过GCB/PSA柱(500mg/6mL,厂家: )用丙酮+正己烷=1+1洗脱,分段收集第一次5mL,第二次5mL,第三次5mL;然后于35℃氮吹,定容1mL。
5mL 5mL 5mL
化合物名称 保留时间 (分) 浓度 浓度 浓度 原液浓度 回收率(%)
1、甲胺磷 8.106 370.1 329.1 0.0 2500.0 28.0
2、敌敌畏 8.31 9.3 5.9 0.0 2500.0 0.6
3、氧乐果 12.788 160.5 0.0 0.0 1018.9 15.7
4、甲拌磷 14.637 26.3 6.9 0.0 499.4 6.7
5、α-666 14.79 129.3 25.5 0.0 999.6 15.5
6、六氯苯 0 0.0 0.0 0.0 499.5 0.0
7、乐果 15.338 410.0 69.1 0.0 2462.9 19.5
8、β-666 15.903 396.8 49.8 1.5 1001.4 44.7
9、γ-666(林丹) 16.145 211.3 35.4 3.5 999.6 25.0
10、五氯硝基苯 16.38 0.0 141.0 15.1 999.2 15.6
11、二嗪磷(二嗪农) 17.107 115.8 17.1 0.0 999.4 13.3
12、δ-666 17.266 441.5 49.1 0.0 998.3 49.1
13、甲基毒死蜱 19.407 54.8 93.0 1.6 1000.0 14.9
14、甲基对硫磷 19.391 100.6 18.5 0.0 500.0 23.8
15、七氯 19.657 86.6 13.4 0.0 500.0 20.0
16、杀螟硫磷 21.018 297.6 49.9 0.0 1495.7 23.2
17、甲基嘧啶磷 21.268 152.3 22.2 0.5 998.9 17.5
18、艾氏剂 21.586 287.9 39.5 0.0 1000.0 32.7
19、马拉硫磷 21.829 139.0 16.3 0.0 1000.0 15.5
20、倍硫磷 22.209 169.1 34.2 0.0 1000.0 20.3
21、对硫磷 22.379 107.6 13.3 0.0 500.0 24.2
22、三氯杀螨醇 22.329 545.3 68.5 3.0 1482.7 41.6
23、毒死蜱 22.359 153.5 74.7 1.2 1000.0 22.9
24、水胺硫磷 22.759 149.7 20.6 0.0 500.0 34.0
25、噻虫嗪 23.342 554.4 182.8 0.0 2504.9 29.4
26、甲基异柳磷 24.083 83.9 12.6 0.0 499.3 19.3
27、环氧七氯 24.126 309.9 36.2 0.0 999.9 34.6
28、喹硫磷 25.2 107.0 70.8 0.0 1000.0 17.8
29、氟虫腈 25.366 218.0 27.9 0.0 1000.3 24.6
30、腐霉利 25.577 339.7 52.5 0.0 1000.0 39.2
31、反-氯丹 25.7 390.5 42.6 1.0 1000.0 43.4
32、噻螨酮 25.717 590.5 57.9 0.0 2500.0 25.9
33、α-硫丹 26.467 967.8 112.6 0.0 2500.0 43.2
34、α-氯丹 26.751 390.4 40.6 1.0 1000.0 43.2
35、狄氏剂 28.296 313.4 38.1 0.0 999.5 35.2
36、PP/-DDE 28.581 445.6 47.8 1.1 999.9 49.5
37、噻嗪酮 29.497 407.9 39.2 0.0 1500.0 29.8
38、β-硫丹 30.522 946.4 124.5 0.0 2500.0 42.8
39、PP/-DDD 31.645 327.5 30.8 0.0 976.8 36.7
40、OP/-DDT 31.805 341.3 25.6 0.0 1002.8 36.6
41、硫丹硫酸盐 33.671 316.1 39.1 0.0 1002.9 35.4
42、PP/-DDT 34.22 286.8 21.3 0.0 1000.0 30.8
44、联苯菊酯 37.61 246.4 20.0 0.5 998.1 26.7
45、甲氰菊酯 37.787 321.4 23.7 0.0 1500.0 23.0
46、氯氟氰菊酯(三氟氯氰菊酯)-1 39.236 122.6 13.3 0.0 1000.0 13.6
47、氯氟氰菊酯(三氟氯氰菊酯)-2 39.564 231.1 25.5 0.0 1000.0 25.7
48、氯菊酯-1 40.606 225.0 40.5 0.0 1500.0 17.7
49、氯菊酯-2 40.807 348.1 35.4 0.0 1500.0 25.6
50、哒螨灵(哒螨酮) 40.725 179.9 17.6 0.0 1000.0 19.8
51、氟氯氰菊酯-1 41.332 165.6 0.0 0.0 996.9 16.6
52、氟氯氰菊酯-2 41.616 462.2 0.0 0.0 500.0 92.4
53、氟氯氰菊酯-3 41.713 131.4 0.0 0.0 500.0 26.3
54、氟氯氰菊酯-4 41.713 131.4 0.0 0.0 500.0 26.3
55、氯氰菊酯-1 41.883 220.3 0.0 0.0 468.0 47.1
56、氯氰菊酯-2 42.012 155.5 0.0 0.0 453.1 34.3
57、氯氰菊酯-3 42.109 140.5 0.0 0.0 454.3 30.9
58、氯氰菊酯-4 42.174 182.7 0.0 0.0 528.6 34.6
59、氟氰戊菊酯-1 42.182 406.4 72.9 0.0 1469.3 32.6
60、氟氰戊菊酯-2 42.425 302.4 41.7 0.0 1500.0 22.9
61、氰戊菊酯-1 43.013 466.1 50.7 0.0 2500.0 20.7
62、氰戊菊酯-2 43.255 565.5 49.7 0.0 2524.0 24.4
63、苯醚甲环唑-1 43.488 245.1 185.6 0.0 1000.0 43.1
64、苯醚甲环唑-2 43.575 232.6 142.5 0.0 1000.0 37.5
65、溴氰菊酯 43.938 314.6 168.0 0.0 1000.0 48.3