| 摘要: |
| 目的：建立测定稻谷中苯噻草胺残留量的微波辅助-固相萃取-高效液相色谱法(MAE-SPE-HPLC)。方法：以丙酮-乙腈（体积比37）为提取剂，采用微波辅助萃取稻谷中残留的苯噻草胺，经弗罗里硅土固相萃取小柱净化后，用高效液相色谱-二极管阵列检测器检测。以乙腈-水为流动相，流速1.0 ml/min，217 nm检测。结果：苯噻草胺在0.198~9.900 μg/ml范围内呈良好的线性关系，最低检测限为0.039 6 μg/ml。稻壳添加平均回收率为90.8%，RSD为1.8%；糙米添加平均回收率为85.6%，RSD为2.5%。结论：MAE-SPE-HPLC法简便、快速，可用于稻谷中苯噻草胺残留量的测定。 |
| 关键词: 微波辅助萃取 固相萃取 高压液相色谱法 苯噻草胺 水稻 |
| DOI：10.3724/SP.J.1008.2008.00845 |
| 投稿时间：2008-03-07修订日期：2008-04-03 |
| 基金项目: |
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| High performance liquid chromatography combined with microwave-assisted extraction and solid phase extraction in determination of mefenacet residues in rice |
| WANG Tao，MI He-ming*，CHAI Yi-feng，FAN Guo-rong,miheming |
| (Department of Pharmaceutical Analysis，School of Pharmacy，Second Military Medical University，Shanghai 200433，China) |
| Abstract: |
| Objective：To establish a method by combining microwave-assisted extraction(MAE), solid phase extraction(SPE) and high performance liquid chromatography (HPLC) for determination of the mefenacet residues in rice.Methods: Acetone and acetontrile (37) were used as extraction solvent. Microwave-assisted extraction was used to extract mefenacet residues in the rice. The extracts were then cleaned up with a Florisil cartridge and then subjected to Hypersil C18 column（5 μm，4.6 mm×200 mm ）, with acetonitrilewater（5050，V/V）solution as mobile phase and with a flow rate of 1.0 ml/min; the ultraviolet detection wavelength was at 217 nm. Results: Good linear correlation for mefenacet was found within a concentration range of 0.198-9.900 μg/ml. The detection limit was 0.039 6 μg/mL for mefenacet（S/N=2）. The average recovery rate of rice hull and brown rice were 90.8% (RSD 1.8%) and 85.6% (RSD 2.5%)，respectively.Conclusion: The present method is simple and rapid; it can be used for the determination of mefenacet residues in rice. |
| Key words: microwave-assisted extraction solid phase extraction high pressure liquid chromatography mefenacet Oryza sativa |
