Rahman Md Musfiqur, Abd El-Aty A M, Kabir Md Humayun, Chung Hyung Suk, Lee Han Sol, Hacımüftüoğlu Fazil, Jeong Ji Hoon, Chang Byung-Joon, Shin Ho-Chul, Shim Jae-Han
Natural Products Chemistry Lab., College of Agriculture and Life Sciences, Chonnam National University, 300 Yongbong-dong, Buk-gu, Gwangju 500-757, Republic of Korea.
Department of Pharmacology, Faculty of Veterinary Medicine, Cairo University, 12211-Giza, Egypt; Department of Veterinary Pharmacology and Toxicology, College of Veterinary Medicine, Konkuk University, Seoul 143-701, Republic of Korea.
Food Chem. 2018 Jan 15;239:1235-1243. doi: 10.1016/j.foodchem.2017.07.073. Epub 2017 Jul 18.
A simple and effective method was developed for analyzing dinotefuran and its three metabolites (MNG, UF, and DN) in plum using liquid chromatography-tandem mass spectrometry (LC-MS/MS). Due to the polarity and high water miscibility, dinotefuran and some of its metabolites (especially DN) have some limitations to be extracted with acetonitrile and salt following the "QuEChERS" sample preparation methodology. Alternatively, the samples were extracted with methanol, and purified with dispersive-solid phase extraction procedure (d-SPE) using primary secondary amine (PSA) and C sorbents after filtration, and mass up. Due to the suppression effect originated from plum matrix, matrix-matched calibration curves, which provided good linearity with coefficient of determination (R)≥0.998, were used for quantification of all analytes. Blank plum samples fortified with 2 spiking levels (10×LOQ and 50×LOQ) yielded satisfactory recoveries for all tested analytes in the range of 83.01 to 110.18% with relative standard deviation (RSD)≤8.91. The method was successfully applied to field-incurred plum samples and dinotefuran and all metabolites were positively detected and quantified. In conclusion, we suggest that the method can be expanded to polar compounds having solvent and partitioning problems in any of the versions of QuEChERS.
建立了一种简单有效的方法，用于采用液相色谱 - 串联质谱法（LC-MS/MS）分析李子中的呋虫胺及其三种代谢物（MNG、UF和DN）。由于呋虫胺及其一些代谢物（尤其是DN）具有极性且与水的混溶性高，按照“QuEChERS”样品制备方法用乙腈和盐进行提取存在一些局限性。因此，样品先用甲醇提取，过滤后用伯仲胺（PSA）和C吸附剂通过分散固相萃取程序（d-SPE）进行净化，然后浓缩。由于李子基质产生的抑制效应，采用基质匹配校准曲线进行所有分析物的定量，校准曲线具有良好的线性，决定系数（R）≥0.998。添加了2个加标水平（10×LOQ和50×LOQ）的空白李子样品对所有测试分析物的回收率在83.01%至110.18%范围内，相对标准偏差（RSD）≤8.91，结果令人满意。该方法成功应用于田间采集的李子样品，呋虫胺及其所有代谢物均被阳性检测和定量。总之，我们建议该方法可扩展到在任何版本的QuEChERS中存在溶剂和分配问题的极性化合物。
