在线净化/固相萃取-高效液相色谱法测定柑橘中多菌灵痕量残留量

Determination of trace carbendazim in citrus by high performance liquid chromatography with on-line clean-up and solid phase extraction

目的通过在线净化/固相萃取-高效液相色谱技术建立测定柑橘中痕量多菌灵的方法。方法 样品在固相萃取小柱Cyclone-MCX中进行净化和富集后,通过阀将固相萃取小柱切换至分析流路,使待测物从富集柱冲洗至分析柱PAⅡC18中,采用梯度洗脱方式完成多菌灵的分离和检测。结果 多菌灵在1~20μg/L范围内呈线性相关,线性方程为Y=0.0921X-0.0016,相关系数r=0.9995;检出限为0.1μg/L(S/N=3);柑橘中3个水平添加回收率(n=6)在86.5%~96.7%;6次加标回收相对标准偏差为2.34%~3.21%。结论 所建方法简便、快速、准确、重现性好,能够满足柑橘中多菌灵痕量残留量的测定。

Objective Toestablish a method for determination of carbendazim in citrus by high perfor-mance liquid chromatography with on-line clean-up and solid phase extraction.Methods After the samples were purified and enriched in the solid phase extraction column Cyclone-MCX, the solid phase extraction column switch to the analysis flow path by switching valve, then let the target analytes flush from the enrich-ment column to the analytical column PAⅡC18, accomplished separation and detection of carbendazim by using the method of gradient elution.Results The linear range was 1~20 μg/L, a linear regression equation was fit-ted as follows:Y=0.0921X-0.0016 with a correlation coefficient of 0.9995. The detection limit was 0.1μg/L. Average recovery at various levels were 86.5%~96.7% with RSD 2.34%~3.21% (n=6).Conclusion The es-tablished method is simple, rapid, accurate and credible, and can be applied in rapid determination of trace carbendazim in citrus with satisfactory results.