单四极杆气相色谱质谱联用仪-安益谱7700气质联用仪关于测定水质苯胺类化合物
方法概要——参考《HJ 822-2017水质苯胺类化合物的测定 气相色谱-质谱法》，使用气相色谱质谱联用仪检测挥发性有机物混标，根据保留时间、质谱图及特征离子对挥发性有机物标准品进行定性，外标法定量。
配置方案
序号 | 配置 | 数量 | 备注 |
1 | 1 | 包括单毛细管柱进样口、质谱主机、机械泵 | |
2 | 色谱柱Agilent HP-5MS 30m×0.25mm×0.25µm | 1 | 或其他等效色谱柱 |
3 | 高纯氦气、减压阀 | 1 | N/A |
4 | 计算机 | 1 | Win10双核4G以上内存64位系统 |
测试方法（参考）
进样模式：不分流；
进样量：1.0μL；
进样口：260℃；
色谱柱：Agilent HP-5MS 30m×0.25mm×0.25µm 恒流模式 色谱柱流量：1ml/min
柱箱升温程序：40℃（5min）5℃/min 100℃（3min）10℃/min200℃（8min）30℃/min280℃
离子源：270℃； 传输线：260℃;
溶剂延迟：10min；
SIM模式分组：
目标物离子列表
序号 | 化合物 | 保留时间（min） | 定量离子（m/z） | 辅助离子（m/z） |
1 | 苯胺-d5 | N/A | 98 | 71 70 |
2 | 苯胺 | 12.166 | 93 | 66 65 |
3 | 1，2-二氯苯-d4 | N/A | 150 | 152 115 |
4 | 2-氯苯胺 | 17.115 | 127 | 129 65 |
5 | 3-氯苯胺 | 19.753 | 127 | 129 65 |
6 | 4-氯苯胺 | 19.885 | 127 | 129 65 |
7 | 4-溴苯胺 | 22.912 | 173 | 171 65 |
8 | 2-硝基苯胺 | 25.274 | 138 | 65 92 |
9 | 2，4，6-三氯苯胺 | 25.271 | 195 | 197 199 |
10 | 3，4-二氯苯胺 | 25.680 | 161 | 163 90 |
11 | 3-硝基苯胺 | 26.567 | 65 | 92 138 |
12 | 2，4，5-三氯苯胺 | 27.402 | 195 | 197 199 |
13 | 4-氯-2-硝基苯胺 | 28.247 | 172 | 126 138 |
14 | 4-硝基苯胺 | 28.262 | 65 | 138 108 |
15 | 2-氯-4-硝基苯胺 | 29.440 | 90 | 172 142 |
16 | 2，6-二氯-4-硝基苯胺 | 29.762 | 124 | 206 176 |
17 | 菲-d10 | N/A | 188 | 189 80 |
18 | 2-溴-6-氯-4-硝基苯胺 | 30.992 | 252 | 222 250 |
19 | 2-氯-4，6-二硝基苯胺 | 32.203 | 217 | 125 90 |
20 | 2，6-二溴-4-硝基苯胺 | 32.523 | 266 | 296 90 |
21 | 2，4-二硝基苯胺 | 32.959 | 183 | 91 153 |
22 | 2-溴-4，6-二硝基苯胺 | 34.033 | 90 | 261 263 |
SIM总离子流图
水质苯胺50ppm选择离子扫描总离子流图（序号对应的化合物参照上表-目标物离子列表）
校正曲线（0.5ppm、1ppm、2ppm、3ppm、5ppm）
对5ppm的苯胺重复进样6针，比较出峰时间和峰面积
图2 浓度5ppm对照品6针结果
表2 浓度5ppm对照品6针化合物出峰时间和定量离子峰面积比较
峰 | 保留时间 | 保留时间RSD[%] | 序号 | 峰面积 | 面积平均值 | 面积RSD[%] |
2 | 12.156 | 0.06 | 1 | 148110.8 | 176587.4 | 9.17 |
12.140 | 2 | 167320.9 | ||||
12.140 | 3 | 181451.8 | ||||
12.135 | 4 | 183406.3 | ||||
12.140 | 5 | 191330.5 | ||||
12.139 | 6 | 187904.2 | ||||
4 | 17.103 | 0.03 | 1 | 150142.1 | 173558.0 | 8.12 |
17.093 | 2 | 163710.5 | ||||
17.090 | 3 | 176462.9 | ||||
17.092 | 4 | 179405.6 | ||||
17.091 | 5 | 187155.2 | ||||
17.091 | 6 | 184471.7 | ||||
5 | 19.741 | 0.05 | 1 | 131225.0 | 148162.8 | 7.15 |
19.721 | 2 | 139851.7 | ||||
19.718 | 3 | 149641.0 | ||||
19.720 | 4 | 153542.1 | ||||
19.719 | 5 | 158892.4 | ||||
19.719 | 6 | 155824.5 | ||||
6 | 19.868 | 0.28 | 1 | 118993.5 | 138841.0 | 8.12 |
19.853 | 2 | 132214.2 | ||||
19.850 | 3 | 142719.9 | ||||
19.852 | 4 | 143629.7 | ||||
19.850 | 5 | 148643.0 | ||||
19.719 | 6 | 146845.6 | ||||
7 | 22.896 | 0.02 | 1 | 77023.2 | 85629.9 | 6.99 |
22.887 | 2 | 80257.0 | ||||
22.888 | 3 | 85822.3 | ||||
22.885 | 4 | 87928.0 | ||||
22.888 | 5 | 92909.5 | ||||
22.885 | 6 | 89839.6 | ||||
8 | 25.261 | 0.02 | 1 | 41543.0 | 46375.3 | 8.03 |
25.256 | 2 | 42568.5 | ||||
25.254 | 3 | 45856.6 | ||||
25.250 | 4 | 48607.4 | ||||
25.253 | 5 | 50892.0 | ||||
25.251 | 6 | 48784.4 | ||||
9 | 25.261 | 0.02 | 1 | 117467.8 | 130505.1 | 6.50 |
25.256 | 2 | 123883.7 | ||||
25.254 | 3 | 131997.7 | ||||
25.250 | 4 | 132257.7 | ||||
25.253 | 5 | 140437.1 | ||||
25.251 | 6 | 136986.5 | ||||
10 | 25.670 | 0.01 | 1 | 115692.5 | 128618.2 | 7.06 |
25.665 | 2 | 121666.4 | ||||
25.662 | 3 | 127544.9 | ||||
25.663 | 4 | 131859.9 | ||||
25.661 | 5 | 141257.6 | ||||
25.660 | 6 | 133687.9 | ||||
11 | 26.552 | 0.01 | 1 | 40973.0 | 44497.2 | 6.50 |
26.550 | 2 | 41492.3 | ||||
26.550 | 3 | 44391.5 | ||||
26.546 | 4 | 45813.5 | ||||
26.547 | 5 | 48662.0 | ||||
26.550 | 6 | 45651.0 | ||||
12 | 27.390 | 0.01 | 1 | 111774.0 | 120221.3 | 6.54 |
27.387 | 2 | 111336.7 | ||||
27.385 | 3 | 118832.1 | ||||
27.385 | 4 | 122162.4 | ||||
27.385 | 5 | 131057.2 | ||||
27.385 | 6 | 126165.6 | ||||
13 | 28.230 | 1.23 | 1 | 36431.8 | 40075.1 | 7.89 |
28.228 | 2 | 37185.7 | ||||
28.227 | 3 | 39578.9 | ||||
28.227 | 4 | 40729.0 | ||||
27.385 | 5 | 45176.3 | ||||
28.228 | 6 | 41348.7 | ||||
14 | 28.248 | 0.00 | 1 | 38670.5 | 41880.4 | 6.27 |
28.246 | 2 | 39904.8 | ||||
28.246 | 3 | 41474.7 | ||||
28.245 | 4 | 42185.2 | ||||
28.245 | 5 | 46265.7 | ||||
28.246 | 6 | 42781.7 | ||||
15 | 29.426 | 0.01 | 1 | 34074.7 | 36562.7 | 6.58 |
29.423 | 2 | 33772.7 | ||||
29.422 | 3 | 36461.5 | ||||
29.421 | 4 | 37408.5 | ||||
29.420 | 5 | 40230.4 | ||||
29.424 | 6 | 37428.4 | ||||
16 | 29.748 | 0.01 | 1 | 23929.9 | 26246.4 | 7.86 |
29.743 | 2 | 24150.4 | ||||
29.744 | 3 | 25582.5 | ||||
29.744 | 4 | 27559.7 | ||||
29.741 | 5 | 29193.0 | ||||
29.745 | 6 | 27062.8 | ||||
18 | 30.974 | 0.01 | 1 | 18111.5 | 20238.0 | 8.96 |
30.969 | 2 | 18490.4 | ||||
30.969 | 3 | 20075.3 | ||||
30.969 | 4 | 20568.7 | ||||
30.973 | 5 | 23051.4 | ||||
30.971 | 6 | 21130.7 | ||||
19 | 32.177 | 0.01 | 1 | 13106.5 | 14668.8 | 9.28 |
32.173 | 2 | 13509.8 | ||||
32.174 | 3 | 14481.1 | ||||
32.173 | 4 | 14776.5 | ||||
32.171 | 5 | 16941.4 | ||||
32.169 | 6 | 15197.3 | ||||
20 | 32.499 | 0.01 | 1 | 25871.0 | 28142.9 | 7.38 |
32.495 | 2 | 26236.2 | ||||
32.495 | 3 | 27776.5 | ||||
32.495 | 4 | 28238.8 | ||||
32.498 | 5 | 31538.6 | ||||
32.491 | 6 | 29196.0 | ||||
21 | 32.934 | 0.01 | 1 | 15215.8 | 16851.4 | 8.63 |
32.931 | 2 | 15737.3 | ||||
32.925 | 3 | 16761.1 | ||||
32.925 | 4 | 16920.1 | ||||
32.924 | 5 | 19419.3 | ||||
32.928 | 6 | 17054.8 | ||||
22 | 34.007 | 0.01 | 1 | 8281.5 | 9034.9 | 7.80 |
34.000 | 2 | 8432.8 | ||||
33.997 | 3 | 9008.3 | ||||
33.997 | 4 | 8947.9 | ||||
33.997 | 5 | 10250.9 | ||||
34.001 | 6 | 9287.9 |
