表1 梯度洗脱条件
时间(min) | A(%) | B(%) |
0 | 80 | 20 |
1 | 80 | 20 |
3 | 50 | 50 |
7 | 25 | 75 |
7.1 | 5 | 95 |
10 | 5 | 95 |
10.1 | 80 | 20 |
16 | 80 | 20 |
表2 质谱仪离子源参数
Source/Gas | |
Collision Gas(CAD) | 6 |
Curtain Gas(CUR) | 15 |
Ion Source Gas 1(GS 1) | 50 |
Ion Source Gas 2(GS 2) | 50 |
Ion Spray Voltage(IS) | 5500 |
Temperature(TEM) | 600 |
Interface Heater(ihe) | On |
表3 4种硝基呋喃待测物母离子和子离子参数表
物质名称 | 保留时间(min) | 监测离子对 | DP | EP | CE | CXP |
SEM | 8.10 | 209.1/166.1 | 51 | 10 | 17 | 10 |
209.1/192.1 | 51 | 10 | 17 | 10 | ||
AHD | 8.30 | 249.2/134.1 | 61 | 10 | 20 | 10 |
249.2/104.1 | 66 | 10 | 31 | 10 | ||
AOZ | 8.89 | 236.2/134.1 | 61 | 10 | 20 | 10 |
236.2/104.1 | 56 | 10 | 31 | 10 | ||
AMOZ | 3.12 | 335.3/291.2 | 46 | 10 | 19 | 10 |
335.5/128.1 | 46 | 10 | 19 | 10 |
图1 4种硝基呋喃代谢物总离子
图2 SEM(209/166)质谱图 | 图3 AOZ(236/134)质谱图 |
图4 AHD(249/134)质谱图 | 图5 AMOZ(335/291)质谱图 |
表4 猪肉中0.5ppb加标回收实验结果
名称 | 1# | 2# | 3# | 平均回收率 | RSD |
AMOZ | 109.43% | 97.84% | 109.75% | 105.67% | 6.42% |
SEM | 91.81% | 88.91% | 88.22% | 89.65% | 2.12% |
AHD | 80.68% | 82.11% | 77.25% | 80.01% | 3.12% |
AOZ | 83.94% | 80.70% | 80.85% | 81.83 | 0.02% |
产品名称 | 规格/包装 | 订货号 | 定价(元) |
Cleanert® PEP-2 | 60mg/3mL,50支/包 | PE0603-2 | 1035.00 |
Venusil® MP C18 | 2.1×150mm,5um,100Å;1支 | VA951502-0 | 3200.00 |