Rejczak Tomasz, Tuzimski Tomasz
Medical University of Lublin, Faculty of Pharmacy with Medical Analytics Division, Chair of Chemistry, Department of Physical Chemistry, 4A Chodźki Street, 20-093 Lublin, Poland.
Food Chem. 2017 Feb 15;217:225-233. doi: 10.1016/j.foodchem.2016.08.095. Epub 2016 Aug 26.
In this study, a quick, easy, cheap, effective, rugged and safe (QuEChERS) extraction technique was adapted to develop a simple sample treatment for multi-residue pesticide analysis in milk samples. The proposed method is based on liquid-liquid partitioning with acetonitrile followed by dispersive solid phase extraction clean-up using primary secondary amine along with zirconia-coated silica particles for extract purification. Identification and quantification of 30 pesticides was conducted via high performance liquid chromatography with diode-array detection (HPLC-DAD). Recoveries were from 70 to 100% for the vast majority of the analytes, with relative standard deviations less than 20% being observed. HPLC-DAD provided suitable linearity, precision and accuracy. For 28 of 30 analytes in the study method limit of quantification values (mLOQs) comply with the most recent European Union guidelines for the maximum residue levels (MRLs) in milk. Negligible matrix effect was observed due to efficient extract clean-up with ZrO2-based sorbents.
在本研究中，采用了一种快速、简便、廉价、高效、耐用且安全的（QuEChERS）萃取技术，以开发一种用于牛奶样品中多残留农药分析的简单样品处理方法。所提出的方法基于用乙腈进行液液分配，随后使用伯仲胺以及氧化锆包覆的硅胶颗粒进行分散固相萃取净化，以提纯提取物。通过配有二极管阵列检测的高效液相色谱法（HPLC-DAD）对30种农药进行鉴定和定量。绝大多数分析物的回收率为70%至100%，相对标准偏差小于20%。HPLC-DAD具有良好的线性、精密度和准确度。在研究方法中，30种分析物中的28种的定量限（mLOQ）值符合欧盟关于牛奶中最大残留限量（MRL）的最新指导方针。由于使用基于ZrO2的吸附剂进行了有效的提取物净化，观察到的基质效应可忽略不计。
