Zheng Hao-Bo, Ding Jun, Zheng Shu-Jian, Yu Qiong-Wei, Yuan Bi-Feng, Feng Yu-Qi
Key Laboratory of Analytical Chemistry for Biology and Medicine (Ministry of Education), Department of Chemistry, Wuhan University, Wuhan 430072, China.
Chinese Academy of Sciences, Key Laboratory of Plant Germplasm Enhancement & Specialty A, Wuhan Botanical Garden, Wuhan 430074, China.
J Chromatogr A. 2015 Jun 12;1398:1-10. doi: 10.1016/j.chroma.2015.04.021. Epub 2015 Apr 18.
A "one-step" quick, easy, cheap, effective, rugged and safe (QuEChERS) method was proposed for pesticide residue analysis in freshly squeezed juice of fruits and vegetables. In this method, a new magnetic adsorbent prepared by simple physical blending was adopt, which could endow the sample mixture with magnetic separability. To achieve the best performance of the modified QuEChERS towards target analytes, the amounts of adsorbents were investigated. Under the optimized conditions, a simple, rapid and sensitive method for the determination of 11 pesticide residues in freshly squeezed juice was established by coupling modified QuEChERS to gas chromatography/mass spectrometry analysis. The limits of quantification of the proposed method for 11 pesticides ranged from 2.0 to 49.6ng/g. Good linearities (R value ≥0.9993) were achieved at different concentration ranges, and acceptable method reproducibility was obtained by evaluating intra- and inter-day precisions with the relative standard deviations being less than 8.5% and 13.5%, respectively. The recoveries were in the range of 70.3-114.1% at different concentrations for real samples. Compared with the traditional QuEChERS methods, extraction/partitioning and purification were integrated into one step in the proposed method, which thus was time-saving (within 3.5min) with keeping good clean-up performance.
提出了一种“一步法”快速、简便、廉价、高效、耐用且安全的（QuEChERS）方法用于水果和蔬菜鲜榨汁中农药残留分析。该方法采用通过简单物理混合制备的新型磁性吸附剂，其可赋予样品混合物磁分离性。为实现改良的QuEChERS对目标分析物的最佳性能，研究了吸附剂的用量。在优化条件下，通过将改良的QuEChERS与气相色谱/质谱分析联用，建立了一种简单、快速且灵敏的测定鲜榨汁中11种农药残留的方法。该方法对11种农药的定量限为2.0至49.6 ng/g。在不同浓度范围内均具有良好的线性（R值≥0.9993），通过评估日内和日间精密度获得了可接受的方法重现性，相对标准偏差分别小于8.5%和13.5%。实际样品在不同浓度下的回收率为70.3 - 114.1%。与传统的QuEChERS方法相比，该方法将萃取/分配和净化整合为一步，因此省时（3.5分钟内）且具有良好的净化性能。
