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微波辅助-固相萃取-高效液相色谱法测定稻谷中苯噻草胺残留量
汪涛,宓鹤鸣*,柴逸峰,范国荣,宓鹤鸣
0
(第二军医大学药学院药物分析学教研室,上海 200433;第二军医大学药学院药分教研室)
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37)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:
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 (37) 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 acetonitrilewater(5050,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