应用离子液体固相萃取材料分析氨基甲酸酯类农药

Van Duy Le, Thai The Nguyen, Hoang Phuong Tran, Anh Mai Nguyen
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摘要

本研究成功合成了固定在硅胶材料 SiO2-(CH2)3-N(Oct)3Br 上的离子液体,并通过傅立叶变换红外光谱(FT-IR)、热重分析(TGA)、扫描电子显微镜(SEM)和能量色散 X 射线光谱(EDX)对其进行了表征。该材料被用作固相萃取的固定相,用于富集水中的痕量氨基甲酸酯类农药。用 5 毫升乙腈(ACN)洗脱滤芯,用氮气吹干,然后重新溶解在 ACN:H2O(40:60,v/v)中,并在 210 和 245 纳米波长下用高效液相色谱-紫外(HPLC-UV)进行分析。在此过程中,先用 5 毫升乙腈(ACN)洗脱滤芯,然后用氮气吹干,再重新溶解于 ACN:H2O(40:60,v/v)中,最后在 210 和 245 纳米波长下进行高效液相色谱-紫外分析。条件的优化有助于氨基甲酸酯类农药的分析,自来水的定量限(LOQ)为 0.36-2.00 μg/l,河水的定量限(LOQ)为 0.4-3.5 μg/l。此外,该方法的重复性良好,相对标准偏差(RSD)小于 10%,符合官方分析合作协会(AOAC)的标准。
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Application of solid-phase extraction materials from ion liquids for the analysis of carbamate pesticide
In this study, ionic liquid immobilised onto silica gel material SiO2-(CH2)3-N(Oct)3Br was successfully synthesised and characterised by Fourier-transform infrared spectroscopy (FT-IR), thermal gravimetric analysis (TGA), scanning electron microscopy (SEM), and energy-dispersive X-ray spectroscopy (EDX). This material was applied as the stationary phase of solid-phase extraction for the enrichment of trace amounts of carbamate pesticides in water. The cartridge was eluted with 5 ml of acetonitrile (ACN), blow-dried with nitrogen gas, and re-dissolved in ACN:H2O (40:60, v/v) and analysed by high-performance liquid chromatography - ultraviolet (HPLC-UV) at 210 and 245 nm. Within this process, elution of the cartridge with 5 ml of acetonitrile (ACN) was followed by nitrogen gas blow-drying and subsequent re-dissolution in ACN:H2O (40:60, v/v), culminating in analysis by HPLC-UV at 210 and 245 nm. Optimisation of conditions facilitated the analysis of carbamate pesticides, with the limit of quantitation (LOQ)ranging from 0.36-2.00 μg/l for tap water and 0.4-3.5 μg/l for river water. Furthermore, the method exhibited favourable repeatability, with a relative standard deviation (RSD) of less than 10%, thereby meeting the Association of Official Analytical Collaboration (AOAC) standards.
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