高效液相色谱法测定小麦中残留除虫脲
Determination of Residual Difluobenzuron in Wheat by HPLC
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摘要: 建立一种以高效液相色谱技术为基础的测定小麦中残留除虫脲分析方法.目标农药经乙腈提取,C18柱色谱分离,以乙腈-水(体积比为60∶40)作流动相,流速为1 mL·min-1,用紫外检测器检测,波长为254 nm,外标法定量.在0.2~20 mg·L-1范围内,除虫脲标准工作溶液的色谱峰高与质量浓度呈线性关系,相关系数为0.999 9.小麦中除虫脲的加标回收率为89.4%~90.9%,相对标准偏差为2.37%~4.15%,检出限(S/N=3)为0.02 mg·kg-1.Abstract: High performance liquid chromatography (HPLC) was applied to the determination of residual difluobenzuron (DFBZ) in wheat.DFBZ was extracted from the sample with acetonitrile,and separated on the hypersil ODS C18 column (250 mm×4.6 mm,i.d.5 μm).A mixture of acetonitrile and water,in the ratio of 60+40 by volume,was used mobile phase,at a flow-rate of 1 mL·min-1.UV-detection was made at the wavelength of 254 nm.External standard was used in the determination.Linear relationship between the chromatographic peak height and mass concentration of DFBZ was obtained in the range of 0.2-20 mg·L-1,with correlation coefficient of 0.999 9 and a detection limit (S/N=3) of 0.02 mg·kg-1.Recovery and precision of the method were tested at 3 concentration levels (1.0,0.2 and 0.04 mg·kg-1),giving results of average recovery in the range from 89.4%-90.9%,and values of RSD′s (n=5) in the range of 2.37%-4.15%.