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流动注射化学发光法测定江水中乙草胺和灭多威的酸性高锰酸钾-罗丹明 B 反应体系。

Flow injection chemiluminescence determination of acetochlor and cartap-HCl in freshwater samples using an acidic KMnO -rhodamine-B reaction system.

机构信息

Department of Chemistry, University of Balochistan, Sariab Road, Quetta, Pakistan.

Department of Chemical Engineering and Analytical Chemistry, University of Barcelona, Marti i Franques 1-11, Barcelona, Spain.

出版信息

Luminescence. 2023 May;38(5):647-661. doi: 10.1002/bio.4493. Epub 2023 Apr 10.

Abstract

A flow injection (FI) methodology using the acidic potassium permanganate (KMnO )-rhodamine-B (Rh-B) reaction with chemiluminescence (CL) detection was established to determine acetochlor and cartap-HCl pesticides in freshwater samples. Experimental parameters were optimized, and Chelex-100 cationic exchanger mini column and solid-phase extraction (SPE) were used as phase separation techniques. Linear calibration curves were observed for the standard solutions of acetochlor and cartap-HCl over the ranges 0.005-2.0 mg L [y = 1155.8x + 57.551, R  = 0.9999 (n = 8)] and 0.005-1.0 mg L [y = 979.76x + 14.491, R  = 0.9998 (n = 8)] with LODs and LOQs of 7.5 × 10 and 8.0 × 10  mg L (3σ blank) and 2.5 × 10 and 2.7 × 10  mg L (10σ blank), respectively, with an injection throughput of 140 h . These methods were used to estimate acetochlor and cartap-HCl with or without the SPE procedure, respectively, in spiked freshwater samples. Results obtained were not significantly different at a 95% confidence level to those of other reported methods. Recoveries for acetochlor and cartap-HCl were obtained over the ranges 93-112% (RSD = 1.9-3.6%) and 98-109% (RSD = 1.7-3.8%), respectively. The most probable CL reaction mechanism was explored.

摘要

建立了一种利用酸性高锰酸钾(KMnO )-罗丹明 B(Rh-B)反应与化学发光(CL)检测的流动注射(FI)方法,用于测定淡水样品中的乙草胺和杀虫脒盐酸盐农药。优化了实验参数,并使用 Chelex-100 阳离子交换剂微型柱和固相萃取(SPE)作为相分离技术。乙草胺和杀虫脒盐酸盐标准溶液在 0.005-2.0 mg/L 范围内呈线性校准曲线 [y=1155.8x+57.551,R 2 =0.9999(n=8)] 和 0.005-1.0 mg/L [y=979.76x+14.491,R 2 =0.9998(n=8)],检出限和定量限分别为 7.5×10 和 8.0×10 毫克/升(3σ空白)和 2.5×10 和 2.7×10 毫克/升(10σ空白),进样通量为 140 小时。这些方法分别用于估计未经 SPE 程序和经 SPE 程序处理的加标淡水样品中的乙草胺和杀虫脒盐酸盐。在 95%置信水平下,所得结果与其他报道的方法无显著差异。乙草胺和杀虫脒盐酸盐的回收率分别为 93-112%(RSD=1.9-3.6%)和 98-109%(RSD=1.7-3.8%)。探讨了最可能的 CL 反应机制。

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