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1.0ml/min,217nm检测。结果:苯噻草胺在0.198~9.900μg/ml范围内呈良好的线性关系,最低检测限为0.0396μg/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。
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.
出处
《第二军医大学学报》
CAS
CSCD
北大核心
2008年第7期845-847,共3页
Academic Journal of Second Military Medical University
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
microwave-assisted extraction
solid phase extraction
high pressure liquid chromatography
mefenaeet
Oryza sativa