固相萃取-超高效液相色谱法检测榨菜中氯吡苯脲的研究

Study on determination of forchlorfenuron in mustard tuber by solid-phase extraction and ultra performance liquid chromatography

建立了固相萃取-超高效液相色谱法定榨菜中氯吡苯脲的方法。样品匀浆后经乙腈提取,固相萃取柱净化后,在流动相为乙腈-纯水(体积比65∶35)、紫外检测波长为260 nm的色谱条件下进行分离检测。结果表明:丙基乙二胺PSA分散固相萃取柱对样品净化效果好,氯吡苯脲在0.1~10.0μg/m L范围内线性关系良好,相关系数r=0.9993,方法检出限为0.03 mg/kg,试样在0.1~1.0 mg/kg添加水平下的平均回收率在96.3%~103.2%之间,RSD值在0.4%~2.2%之间。结论:方法准确度较好,操作简单快捷,样品净化效果好,测定低限能满足限量要求。

A method of solid-phase extraction and ultra performance liquid chromatography coupled with diode array detection was established for the determination of forchlorfenuron in mustard tuber. The sample was extracted with acetonitrile, and cleaned up with solid-phase extraction column.Forchlorfenuron was determined by ultra performance liquid chromatography at 260 nm using acetonitrile-water（65：35 ）as mobile phase.The results indicated that the PSA solid-phase extraction column was more effective than others, and the calibration curve showed good linearity when the amount of forchlorfennron was in the range of0.1-10.0 μg/mL, with correlation coefficient of 0.9993, and detecting limit of forchlorfenuron were 0.03 mg/kg, and the average recoveries ranged from 96.3% to 103.2% ,with the relative standard deviation（RSD）of 0.4% -2.2%.Conclusion：The result demonstrated that the method was simple, accurate and suitable for the identification and quantification of forchlorfenuron in mustard tuber.