Department of Agro-food Safety and Crop Protection, National Institute of Agricultural Sciences, Rural Development Administration, Wanju-gun, Jeollabuk-do, Republic of Korea.
J Sep Sci. 2019 Jul;42(14):2379-2389. doi: 10.1002/jssc.201900066. Epub 2019 Jun 12.
A multi-residue method has been developed and validated to determine 46 pesticides in spinach using liquid chromatography tandem mass spectrometry. The method is based on modified quick, easy, cheap, effective, rugged, and safe sample preparation, where high-surface-area graphitized carbon black was used first as sorbent material in the dispersive solid-phase extraction. The method was compared with the quick, easy, cheap, effective, rugged, and safe method. The morphology, surface area, pore size, and pore volume of the sorbent was determined. The results obtained show that the sorbent consists of high surface area (233 m /g) and large pore volume (1.5 cm /g). The calibration curve correlation coefficient (R ) of the method was at least 0.99. The average recoveries ranged from 74 to 116%, and limits of detection and quantification from 0.0001 to 0.002 mg/kg and from 0.0002 to 0.005 mg/kg, respectively. Using the method, the pesticides exhibited low matrix effect (< 20%), except for nicosulfuron (29.86%), methomyl (26.77%), and flufenoxuron (24.65%). The method showed better potential to remove pigments than the quick, easy, cheap, effective, rugged, and safe method. It is demonstrated that the proposed method could be useful alternative for sample preparation of spinach and other matrices in future.
建立并验证了一种使用液相色谱串联质谱法检测菠菜中 46 种农药残留的多残留方法。该方法基于改良的 QuEChERS 方法,首先使用高比表面积石墨化炭黑作为分散固相萃取的吸附剂材料。该方法与 QuEChERS 方法进行了比较。对吸附剂的形貌、比表面积、孔径和孔体积进行了测定。结果表明,该吸附剂的比表面积(233 m /g)高,孔体积(1.5 cm /g)大。方法的校准曲线相关系数(R )至少为 0.99。平均回收率为 74%至 116%,检出限和定量限分别为 0.0001 至 0.002 mg/kg 和 0.0002 至 0.005 mg/kg。使用该方法,除了硝磺草酮(29.86%)、灭多威(26.77%)和氟虫脲(24.65%)外,其他农药的基质效应均<20%。该方法在去除色素方面比 QuEChERS 方法更具潜力。结果表明,该方法可作为未来菠菜及其他基质样品前处理的有效替代方法。