NK‐1375 is a major metabolite of the diamide insecticide cyclaniliprole (CYCP) with toxicological significance. It is formed in various transformation pathways of CYCP, including photolysis and plant metabolism. In the present study, NK‐1375 was produced employing the liquid‐phase photolysis of CYCP followed by isolation using preparative liquid chromatography. The structure of the isolated substance was confirmed using MS and ¹H NMR spectroscopy, and its purity was measured to be 95.9% using HPLC. As its application, a residue analysis method was first developed for the simultaneous determination of CYCP and NK‐1375 in six representative plant‐origin foods using fast multi‐plug filtration cleanup and UHPLC–MS/MS. Excellent linearity (r > 0.999) was obtained over the calibration range from 0.001 to 0.1 μg mL⁻¹. The recoveries (intra‐day and inter‐day) of CYCP and NK‐1375 from different matrices ranged from 74 to 112%, with corresponding relative standard deviations less than 13%. The limits of quantitation of these two compounds were defined at 0.01 mg kg⁻¹. This study can be useful for the subsequent analytical or toxicological research on this important pesticide metabolite.

中文翻译：

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双酰胺杀虫剂环己腈的主要代谢物NK-1375的制备分离及其在使用UHPLC-MS / MS分析植物来源食品中的相关残留物中的应用

NK-1375是双酰胺杀虫剂环磷酰胺（CYCP）的主要代谢产物，具有毒理学意义。它是通过CYCP的各种转化途径形成的，包括光解和植物代谢。在本研究中，NK-1375是使用CYCP的液相光解法制备的，然后使用制备型液相色谱法进行分离。使用MS和¹ H NMR光谱法确认分离的物质的结构，并且使用HPLC测量其纯度为95.9％。在其应用中，首先开发了一种残留分析方法，该方法使用快速多塞滤过滤和UHPLC-MS / MS同时测定六种代表性植物性食品中的CYCP和NK-1375。出色的线性度（[R > 0.999）在0.001至0.1μgmL ^-1的校准范围内获得。CYCP和NK-1375在不同基质中的回收率（日内和日间）范围为74％至112％，相应的相对标准偏差小于13％。这两种化合物的定量限定义为0.01 mg kg ^-1。该研究对于该重要农药代谢物的后续分析或毒理学研究可能是有用的。