Nakajima Takayuki, Tomizawa Sanae, Kamijo Kyoko, Yamamoto Kazuoki, Takada Tomomi, Kokaji Yoshie, Shiradoh Hiroko, Ohsawa Yoshihiro, Oyama Ayane, Noguchi Maiko, Yokoyama Tomoko
Tokyo Metropolitan Institute of Public Health.
Shokuhin Eiseigaku Zasshi. 2024;65(5):118-125. doi: 10.3358/shokueishi.65.118.
Nicotinic acetylcholine receptors (nAChRs) are neurotransmitter receptors found in the nervous system of many organisms, including humans. Neonicotinoid pesticides act as nAChRs modulators that affect neurotransmission. Due to toxicity effects, their use has been restricted. However, a new class of modulators (nAChRMs) have been developed, but analytical methods for the detection of residues of these new pesticides in agricultural crops have not been established. Therefore, this study aimed to develop and validate an accurate determination method for novel nAChRMs, such as sulfoxaflor, flupyradifurone, flupyrimin, and triflumezopyrim in brown rice using liquid chromatography with tandem mass spectrometry (LC-MS/MS). The method was applied to commercially available brown rice samples from Tokyo, Japan. Target analytes were extracted with acetonitrile, cleaned with GC/PSA, and then cleaned again with MonoSpin PBA. In accordance with the method validation guidelines for residual pesticides in foods, the performance characteristics were evaluated, with trueness ranging from 86.3% to 98.2%, repeatability of less than 6.5% relative standard deviation (RSD), and within-laboratory reproducibility of less than 6.5% RSD. These results indicate that the developed method can be applied to residue surveillance of target analytes using solvent standard calibration curves. By applying the developed method to 53 brown rice samples commercially available in Tokyo, sulfoxaflor residues were found in two samples at concentrations of 3.7 and 21.9 ng/g. This is the first report of the detection of sulfoxaflor residues in domestic agricultural products.
烟碱型乙酰胆碱受体（nAChRs）是在包括人类在内的许多生物体的神经系统中发现的神经递质受体。新烟碱类农药作为影响神经传递的nAChRs调节剂。由于其毒性作用，它们的使用已受到限制。然而，已开发出一类新的调节剂（nAChRMs），但尚未建立用于检测农作物中这些新型农药残留的分析方法。因此，本研究旨在开发并验证一种使用液相色谱-串联质谱法（LC-MS/MS）准确测定糙米中新型nAChRMs（如氟吡呋喃酮、氟吡菌胺和三氟苯嘧啶）的方法。该方法应用于来自日本东京的市售糙米样品。目标分析物用乙腈萃取，用GC/PSA净化，然后再用MonoSpin PBA净化。按照食品中残留农药的方法验证指南对性能特征进行了评估，准确度范围为86.3%至98.2%，相对标准偏差（RSD）的重复性小于6.5%，实验室内再现性小于6.5%RSD。这些结果表明，所开发的方法可应用于使用溶剂标准校准曲线对目标分析物进行残留监测。通过将所开发的方法应用于东京市售的53个糙米样品，在两个样品中发现了氟吡呋喃酮残留，浓度分别为3.7和21.9 ng/g。这是国内农产品中氟吡呋喃酮残留检测的首次报道。
