Camellia nut shell was collected, dried at room temperature and ground to get fine powder. The powder was extracted three times with 95% EtOH, combined, evaporated, and then freeze dried. The crude powder was dissolved in H 2 O and then sequentially fractionated with n-hexane, CH 2 Cl 2 , EtOAc and n-BuOH. A part of EtOAc fraction was chromatographed on a silica gel and on a Sephadex LH-20 columns using MeOH, aqueous MeOH, EtOAc-n-hexane and EtOH-n-hexane to isolate gallotannins. Three gallotannins, 1,2-di-O-galloyl-β-D-glucopyranoside (2), 1,2,6-tri-Ogalloyl-β-D-glucopyranoside (3) and 1,2,3,6-tetra-O-galloyl-β-D-glucopyranoside (4), including gallic acid (1), were isolated and elucidated by NMR and Mass spectroscopies. Although nothing new, these gallotannins were first reported from the nut shell extractives of camellia tree (Camellia oleifera C. Abel). This study was to investigate the chemical constituents, especially hydrolysable tannins, of nut shell extractives of Camellia oleifera and to provide basic information for the future chemical utilization of this species.
Herein, we present a method for the quantitative analysis of broflanilide residues in water, soil, and rice samples from a paddy field in Jiangxi Province, China. The quick, easy, cheap, effective, rugged, and safe (QuEChERS) method was optimized for the extraction and purification of broflanilide residues. Residual broflanilide concentrations in different matrices were then determined by high-performance liquid chromatography (HPLC). The calibration curve of broflanilide showed good linearity in all matrices for concentrations between 0.005 and 1 mg·L−1, with a correlation coefficient greater than 0.99. The matrix effect varied from −69% to −54%, indicating matrix suppression. The average recoveries ranged between 85.82% and 97.46%, with relative standard deviations of 3.29%–8.15%. The limits of detection ranged from 0.16 to 1.67 μg·kg−1, and the limits of quantification were in the range of 0.54 to 5.48 μg·kg−1. Dissipation dynamic tests indicated broflanilide half-lives of 0.46–2.46, 2.09–5.34, and 1.31–3.32 days in soil, water, and rice straw, respectively. Broflanilide was dissipated more rapidly in water than in soil and rice straw. More than 90% of broflanilide residues dissipated within 14 days. The final residues of broflanilide in rice were all below LOQ at harvest.
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