A selective dispersive liquid-liquid micro-extraction technique for trace level pollutants enrichment of pharmaceutical residues from hospital wastewaters followed by liquid chromatographic analysis

IF 16.4 1区化学 Q1 CHEMISTRY, MULTIDISCIPLINARY

Accounts of Chemical Research Pub Date : 2023-11-29 DOI:10.4314/bcse.v38i1.3

Gadisa Wakuma, Estifanos Ele Yaya, Negash Getachew, Negussie Megersa

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Abstract

In this study a dispersive liquid-liquid micro-extraction (DLLME) method was utilized for extraction of trace pharmaceuticals in wastewater samples. Factors influencing the extraction performances were tested and accordingly 900 µL dichloroethane as the extraction solvent, 1400 µL acetonitirle as dispersive solvent, 10 min extraction time at 4000 rpm centrifugation, and pH 5 were found optimum. Acetonitrile and 0.2% formic acid in water were used as eluent. The column temperature was maintained at 25 °C and the optimum detection wavelengths of 273 nm for sulfamethoxazole and 280 nm for ciprofloxacin were used. For both the analytes, the coefficients of determinations (r2) were found to vary from 0.9989 to 0.9997, confirming good linearity in the concentration range of 0.005-100 µg mL-1 for sulfamethoxazole and 0.01-100 µg mL-1 for ciprofloxacin. The LOD and LOQ were in the range of 0.78-1.58 ng mL-1 and 2.24-5.28 ng mL-1, respectively; the RSDs were 0.41-3.21% for intra-day precision and 0.37-6.44% for inter-day precision. The concentrations of the three pharmaceuticals determined ranged from 0.76-1.53 μg mL-1 in the wastewater samples collected from Black Lion Hospital. However, ciprofloxacin and doxycycline were not detected and only low concentration of sulfamethoxazole was detected in the wastewater samples collected from Menelik II Hospital. KEY WORDS: Antibiotics, DLLME, Dispersive solvent, Hospital wastewater Bull. Chem. Soc. Ethiop. 2024, 38(1), 27-42. DOI: https://dx.doi.org/10.4314/bcse.v38i1.3

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选择性分散液-液微萃取技术用于富集医院废水中的痕量药物残留，然后进行液相色谱分析

本研究采用分散液-液微萃取（DLLME）法萃取废水样品中的痕量药物。对影响萃取性能的因素进行了测试，结果表明 900 µL 二氯乙烷为萃取溶剂，1400 µL 乙腈为分散溶剂，4000 rpm 离心 10 分钟萃取，pH 值为 5 为最佳萃取条件。洗脱液为乙腈和 0.2%甲酸水溶液。色谱柱温度保持在 25 °C，磺胺甲噁唑的最佳检测波长为 273 nm，环丙沙星的最佳检测波长为 280 nm。对于这两种分析物，测定系数（r2）在 0.9989 至 0.9997 之间，证明在 0.005-100 µg mL-1 的浓度范围内磺胺甲噁唑和 0.01-100 µg mL-1 的浓度范围内环丙沙星具有良好的线性关系。最低检测限和最低定量限分别为 0.78-1.58 ng mL-1 和 2.24-5.28 ng mL-1；日内精密度的 RSD 为 0.41-3.21%，日间精密度的 RSD 为 0.37-6.44%。在黑狮医院采集的废水样本中，三种药物的测定浓度范围为 0.76-1.53 μg mL-1。然而，在梅内利克二世医院采集的废水样本中未检测到环丙沙星和多西环素，仅检测到低浓度的磺胺甲噁唑。关键词：抗生素、DLLME、分散溶剂、医院废水 Bull.Chem.Soc.2024, 38(1), 27-42.DOI: https://dx.doi.org/10.4314/bcse.v38i1.3

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来源期刊

Accounts of Chemical Research 化学-化学综合

CiteScore

31.40

自引率

1.10%

发文量

312

审稿时长

2 months

期刊介绍： Accounts of Chemical Research presents short, concise and critical articles offering easy-to-read overviews of basic research and applications in all areas of chemistry and biochemistry. These short reviews focus on research from the author’s own laboratory and are designed to teach the reader about a research project. In addition, Accounts of Chemical Research publishes commentaries that give an informed opinion on a current research problem. Special Issues online are devoted to a single topic of unusual activity and significance. Accounts of Chemical Research replaces the traditional article abstract with an article "Conspectus." These entries synopsize the research affording the reader a closer look at the content and significance of an article. Through this provision of a more detailed description of the article contents, the Conspectus enhances the article's discoverability by search engines and the exposure for the research.