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Development of a SBSE-HPLC method using sol-gel based germania coated twister for the analysis of 4-chloro-1-naphthol in biological and water samples
Arabian Journal of Chemistry ( IF 5.3 ) Pub Date : 2020-01-01 , DOI: 10.1016/j.arabjc.2018.11.016
Shehzada Muhammad Sajid Jillani , Saheed A. Ganiyu , Khalid Alhooshani

Abstract In this work, 4-chloro-1-naphthol is extracted from environmental and biological samples using germania-based polydimethylsiloxane hybrid organic-inorganic coated twister, followed by high-performance liquid chromatography-ultraviolet detection. The coated twisters showed a good preparation reproducibility of 1.7% (n = 3) for one batch and 3.5% (n = 3) for different batches. The coated stir bars were successfully characterized using field emission scanning electron microscope, energy dispersive X-ray spectroscopy, thermogravimetric analysis and X-ray photoelectron spectroscopy. Sample volume, extraction time, stirring rate, desorption solvent, desorption time and ionic strength were optimized for the stir bar sorptive extraction process. Under optimized experimental conditions, the method showed linearity in the range of 0.4–800 ng mL−1 with R2 = 0.9992 and limit of detection (S/N = 3) as 0.034 ng mL−1. The chromatographic method showed higher selectivity by having baseline separation between 1-naphthol and 2-naphthol (the expected interference) and 4-chloro-1-naphthol. This germania-based stir bar sorptive extraction-high performance liquid chromatographic method was successfully applied for 4-chloro-1-naphthol in wastewater, pool water, and human urine and showed relative recoveries between 87.4 and 141.3% with acceptable relative standard deviation i.e. 4–11%.

中文翻译:

使用基于溶胶-凝胶的锗涂层捻线器开发 SBSE-HPLC 方法,用于分析生物和水样品中的 4-chloro-1-naphthol

摘要 本研究采用氧化锗基聚二甲基硅氧烷杂化有机-无机包覆捻线机从环境和生物样品中提取4-氯-1-萘酚,然后进行高效液相色谱-紫外检测。涂层捻线机表现出良好的制备重现性,一批为 1.7% (n = 3),不同批次为 3.5% (n = 3)。使用场发射扫描电子显微镜、能量色散 X 射线光谱、热重分析和 X 射线光电子能谱成功地表征了涂层搅拌棒。样品体积、提取时间、搅拌速率、解吸溶剂、解吸时间和离子强度针对搅拌棒吸附提取过程进行了优化。在优化的实验条件下,该方法在0范围内表现出线性。4–800 ng mL-1,R2 = 0.9992,检测限 (S/N = 3) 为 0.034 ng mL-1。通过在 1-萘酚和 2-萘酚(预期干扰)和 4-氯-1-萘酚之间进行基线分离,该色谱方法显示出更高的选择性。这种基于锗的搅拌棒吸附萃取-高效液相色谱方法成功应用于废水、池水和人尿中的 4-氯-1-萘酚,其相对回收率在 87.4% 至 141.3% 之间,相对标准偏差可接受,即 4 –11%。
更新日期:2020-01-01
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