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Ultrasonic-Assisted Magnetic Solid-Phase Dispersive Extraction for Determination of Chlorpyrifos and Triclosan in Wastewater Samples prior to Liquid Chromatography Tandem Mass Spectrometry Detection
Chromatographia ( IF 1.7 ) Pub Date : 2020-01-06 , DOI: 10.1007/s10337-019-03848-0
Vallerie A. Muckoya , Patrick B. Njobeh , Philiswa N. Nomngongo , Jane C. Ngila

In the present study, carbon nanodots (CNDs) were successfully anchored on magnetite (Fe 3 O 4 ) under magnetic stirring and the nanocomposite prepared was assessed as a new adsorbent for ultrasonic-assisted magnetic solid-phase dispersive extraction of chlorpyrifos (CPF) and triclosan (TCS) in water samples. Detection was achieved using ultrahigh performance liquid chromatography–tandem mass spectrometry (LC–MS/MS). The prepared magnetic CNDs were characterised by transmission electron microscopy, scanning electron microscopy, Fourier transform infrared and X-ray diffraction. The investigation and optimisation of the main experimental variables having an influence on the analytical response were performed using a multivariate approach. The factors studied were sample pH, mass of adsorbent and extraction time. The selection of desorption solvent and desorption time were examined and optimised univariately. By appropriating the optimum experimental conditions, the developed method was validated for accuracy using real environmental water samples. The average percentage recoveries obtained using influent and effluent spiked wastewater samples ranged between 76–108% and 79–96% for CPF and TCS, respectively. A good linearity ( R 2 > 0.995) was established ranging between 5 and 100 µg L −1 . The limit of detection and limit of quantification were in the range of 0.024–0.081 µg L −1 and 0.057–0.192 µg L −1 , respectively. The repeatability and reproducibility expressed as % relative standard deviation were less than 4.7%. The developed method exhibited good method performance, is rapid, simple, inexpensive and environmentally friendly.

中文翻译:

在液相色谱串联质谱检测之前,超声波辅助磁性固相分散萃取测定废水样品中的毒死蜱和三氯生

在本研究中,碳纳米点 (CNDs) 在磁力搅拌下成功锚定在磁铁矿 (Fe 3 O 4 ) 上,制备的纳米复合材料被评估为用于超声辅助磁固相分散提取毒死蜱 (CPF) 和水样中的三氯生 (TCS)。使用超高效液相色谱-串联质谱 (LC-MS/MS) 实现检测。通过透射电子显微镜、扫描电子显微镜、傅里叶变换红外和X射线衍射对制备的磁性CNDs进行了表征。使用多变量方法对影响分析响应的主要实验变量进行调查和优化。研究的因素是样品 pH 值、吸附剂质量和提取时间。对解吸溶剂和解吸时间的选择进行了单变量检查和优化。通过选择最佳实验条件,使用真实环境水样验证了所开发方法的准确性。对于 CPF 和 TCS,使用进水和出水加标废水样品获得的平均回收率分别介于 76-108% 和 79-96% 之间。在 5 和 100 µg L -1 之间建立了良好的线性(R 2 > 0.995)。检测限和定量限分别在 0.024–0.081 µg L -1 和 0.057–0.192 µg L -1 的范围内。以百分比相对标准偏差表示的重复性和再现性小于 4.7%。所开发的方法表现出良好的方法性能,快速、简单、廉价且环保。
更新日期:2020-01-06
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