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

中文关键词:  在线净化/固相萃取  高效液相色谱法  柑橘  多菌灵

英文关键词:on-line clean-up and solid phase extraction  high performance liquid chromatography  citrus  carbendazim ¬

中文摘要:

      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1~20 μg/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0.1 μg/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。

英文摘要:

      Objective To establish a method for determination of carbendazim in citrus by high performance 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 enrichment 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 fitted as follows: Y=0.0921X-0.0016 with a correlation coefficient of 0.9995. The detection limit was 0.1 μg/L. Average recovery at various levels were 86.5%~96.7% with RSD 2.34%~3.21% (n=6). Conclusion The established method is simple, rapid, accurate and credible, and can be applied in rapid determination of trace carbendazim in citrus with satisfactory results.