| 高效液相色谱-四极杆/静电场轨道阱高分辨质谱快速检测6种农产品中96种农药的残留量 |
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| 引用本文： | 吴斌,丁涛,柳菡,陈惠兰,赵增运,张睿,沈崇钰. 高效液相色谱-四极杆/静电场轨道阱高分辨质谱快速检测6种农产品中96种农药的残留量[J]. 色谱, 2012, 30(12): 1246-1252. DOI: 10.3724/SP.J.1123.2012.07014 |
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| 作者姓名： | 吴斌 丁涛 柳菡 陈惠兰 赵增运 张睿 沈崇钰 |
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| 作者单位： | 江苏出入境检验检疫局动植物与食品检测中心, 江苏 南京 210001 |
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| 摘 要： | 利用高效液相色谱-四极杆/静电场轨道阱高分辨质谱快速筛选辣椒、青花菜、脱水土豆、大豆、绿茶和大蒜中96种农药残留。样品经含0.1%醋酸的乙腈提取,分散固相萃取脱水、除色、净化后,以C18色谱柱为分析柱,甲醇和5 mmol/L醋酸铵水溶液作为流动相进行梯度洗脱分离。采用正、负离子切换同时测定96种农药残留,大大提高了检测通量。通过优化分辨率,在全扫描模式下提取目标化合物的精确质量数,有效地去除了基质干扰;采用自动触发采集二级质谱图进一步提高了定性的准确性。在1～200 μg/L范围内,96种农药的线性相关系数均大于0.99。通过实际样品的添加回收试验,回收率范围为58%～105%,相对标准偏差为8.8%～18.3%。该方法的检测低限可以达到5 μg/kg,可以作为蔬菜中多种农药残留高通量筛选和确认检测方法。
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| 关 键 词： | 高分辨质谱 高效液相色谱 静电场轨道阱 农产品 农药残留 |
| 收稿时间： | 2012-07-09 |
Fast screening ninety-six pesticides in six kinds of agricultural products by high performance liquid chromatography-quadrupole/electrostatic field orbit trap high-resolution mass spectrometry |
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| WU Bin , DING Tao , LIU Han , CHEN Huilan , ZHAO Zengyun , ZHANG Rui , SHEN Chongyu. Fast screening ninety-six pesticides in six kinds of agricultural products by high performance liquid chromatography-quadrupole/electrostatic field orbit trap high-resolution mass spectrometry[J]. Chinese journal of chromatography, 2012, 30(12): 1246-1252. DOI: 10.3724/SP.J.1123.2012.07014 |
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| Authors: | WU Bin DING Tao LIU Han CHEN Huilan ZHAO Zengyun ZHANG Rui SHEN Chongyu |
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| Affiliation: | Animal, Plant and Food Inspection Center of Jiangsu Entry-Exit Inspection and Quarantine Bureau, Nanjing 210001, China |
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| Abstract: | A high-throughput method for the determination of 96 pesticides in six kinds of agricultural products by liquid chromatography-quadrupole/electrostatic field orbit trap high-resolution mass spectrometry was developed. After extraction with 0.1% acetic acid in acetonitrile solution and concentration, dispersive solid-phase extraction was further utilized to reduce the matrix interference. The chromatographic analysis was performed on a C18 column with methanol and 5 mmol/L ammonium acetate solution as the mobile phases with a gradient elution program. The 96 pesticide residues were analyzed in switching positive and negative modes at the same time. With the optimized mass resolution, accurate mass-to-charge ratio extraction of the target pesticide compounds in full scan mode could eliminate matrix interference effectively. Two-stage threshold-triggered full mass scan mode was utilized to further improve the accuracy of qualitative analysis. The linear ranges of all the 96 pesticides were from 1 μg/L to 200 μg/L with correlation coefficients greater than 0.99. By detecting spiked samples, the detection limits were 5 μg/kg for all the residues and the recoveries were in the range of 58%~105% with the relative standard deviations (RSDs) between 8.8% and 18.3%. |
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| Keywords: | high performance liquid chromatography (HPLC) electrostatic field orbit trap high-resolution mass spectrometry pesticide residues agricultural products |
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