Department of Applied Chemistry, College of Science, China Agricultural University, Beijing, China.
J Sep Sci. 2013 Oct;36(20):3379-86. doi: 10.1002/jssc.201300411. Epub 2013 Sep 1.
A novel design for a rapid clean-up method was developed for the analysis of pesticide residues in fruit and vegetables followed by LC-ESI-MS/MS. The acetonitrile-based sample extraction technique was used to obtain the extracts, and further clean-up was carried out by applying the streamlined procedure on a multiplug filtration clean-up column coupled with a syringe. The sorbent used for clean-up in this research is multiwalled carbon nanotubes, which was mixed with anhydrous magnesium sulfate to remove water from the extracts. This method was validated on 40 representative pesticides and apple, cabbage, and potato sample matrices spiked at two concentration levels of 10 and 100 μg/kg. It exhibited recoveries between 71 and 117% for most pesticides with RSDs < 15%. Matrix-matched calibrations were performed with the coefficients of determination >0.995 for most studied pesticides between concentration levels of 10-500 μg/L. The LOQs for 40 pesticides ranged from 2 to 50 μg/kg. The developed method was successfully applied to the determination of pesticide residues in market fruit and vegetable samples.
针对果蔬中农药残留的分析，我们开发了一种新型的快速净化方法，随后采用 LC-ESI-MS/MS 进行检测。该方法基于乙腈的样品提取技术获取提取物，然后通过在多通道过滤净化柱上应用简化的程序并结合注射器进行进一步的净化。本研究中用于净化的吸附剂是多壁碳纳米管，它与无水硫酸镁混合以去除提取物中的水分。该方法在 40 种代表性农药和苹果、白菜和土豆样品基质上进行了验证，在 10 和 100μg/kg 两个浓度水平下进行了加标。对于大多数农药，回收率在 71%至 117%之间，相对标准偏差（RSD）<15%。对于大多数研究的农药，在 10-500μg/L 的浓度水平下，基质匹配校准的决定系数（R²）>0.995。40 种农药的 LOQs 范围为 2-50μg/kg。该方法成功应用于市场果蔬样品中农药残留的测定。
