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| QuEChERS-液质联用法测定菜籽油中7种
芳氧苯氧丙酸酯类除草剂残留备工艺研究 |
| Determination of seven aryloxyphenoxypropionate herbicides residues in rapeseedoil by QuEChERS-liquid chromatography/tandem mass spectrometry |
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| DOI： |
| 中文关键词: 菜籽油 分散固相萃取 高效液相色谱质谱联用 芳氧苯氧丙酸酯类除草剂 |
| 英文关键词:rapeseed oil QuEChERS HPLC-MS/MS aryloxyphenoxypropionate herbicides |
| 基金项目: |
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| 中文摘要: |
| 建立了分散固相萃取(QuEChERS)净化方法结合液质联用(HPLC-MS/MS)检测技术同时测定菜籽油中7种芳氧苯氧丙酸酯类除草剂的方法。结果表明：最优检测条件为采用90%乙腈水溶液提取2次， Supel QuE Z-Sep+分散固相萃取净化，色谱柱为sunshell C18柱（2.6 μm×2.1 mm×100 mm），以乙腈和0.025%乙酸水溶液进行梯度洗脱，MRM模式。在最优检测条件下，除精恶唑禾草灵外6种除草剂线性范围0～100（50）μg/L，相关系数R大于0.999 5，定量限在0.25～2.5 μg/kg之间，回收率在78.3%～95.1%之间，相对标准偏差在0.9%～6.5%之间。方法具有基质效应低、处理简单、准确快速、重复性好的优点，适用于实验室高通量快速检测菜籽油样品。 |
| 英文摘要: |
| A QuEChERS- liquid chromatography/tandem mass spectrometry to determine seven aryloxyphenoxypropionate herbicides in rapeseed oil was developed. The results showed that the optimal detection conditions were obtained as follows:samples extracted by 90% acetonitrile water solution for twice, extractive purified by Supel QuE Z-Sep and dispersive solid-phase extraction, chromatography column sunshell C18(2.6 μm×2.1 mm×100 mm); mobile phase acetonitrile and 0.025% acetic acid water solution, gradient elution, MRM method. Under the optimal detection conditions, except for fenoxaprop-ethyl, the calibration curve was linear in the range of 0-100(50) μg/L and R>0.999 5, and the limit of quantitation was in the range of 0.25-2.5 μg/kg. The recovery rate and relative standard deviation were in the range of 78.3%-95.1% and 0.9%-6.5%, respectively. The method had advantages of low matrix effect, easy sample handling, accuracy, rapidness, and good reproducibility, and could be used as a high throughput and rapid detection method for rapeseed oil in lab. |
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