刘明利,张霞,姜廷福.涡旋辅助分散液液微萃取-石墨炉原子吸收光谱法测定铜的方法研究[J].中国海洋药物,2026,(1):-. |
涡旋辅助分散液液微萃取-石墨炉原子吸收光谱法测定铜的方法研究 |
Study on the method of determination of copper by graphite furnace atomic absorption spectrometry with dispersive liquid-liquid microextraction assisted by vortex |
投稿时间:2024-10-13 修订日期:2024-11-21 |
DOI: |
中文关键词: 海洋药用生物 分散液液微萃取 石墨炉原子吸收 铜 |
English Keywords:marine medicinal organisms dispersive liquid-liquid microextraction graphite furnace atomic absorption copper |
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中文摘要: |
目的 优化基于低共熔溶剂(DES)的涡旋辅助分散液液微萃取(DLLME)联用石墨炉原子吸收光谱法(GFAAS)用于测定的铜的方法,并测定海洋药用生物、水样、尿样中铜含量。方法 以甲基三辛基溴化铵为氢键受体,癸酸为氢键供体,按摩尔比3∶1混合制备DES。在适宜磷酸盐浓度下,目标样品中的铜在pH=5时与吡咯烷二硫代甲酸铵形成螯合物并被富集到萃取相,用原子吸收光谱仪测定。研究了pH、DES用量、螯合剂浓度、涡旋时间等因素对萃取效率的影响。结果 在最佳条件下,该方法线性范围良好(相关系数r=0.998 5),检出限为0.02 μg/L,重现性(RSD)为7.75%。用该方法测定海洋药物中的铜含量为2.98~23.50 mg/kg。测定收集水样及尿样中的铜含量分别为12.28~21.50、22.25~29.21 μg/L。结论 本研究设计并优化了基于DES的涡旋辅助分散液液微萃取联用原子吸收光谱法测定铜含量的方法,具有高效、便捷、灵敏的特点,可应用于海洋药用生物、水样及尿样中铜含量的测定。 |
English Summary: |
Objective To optimize the method of vortex assisted dispersive liquid-liquid microextraction (DLLME) combined with graphite furnace atomic absorption spectrometry (GFAAS) for the determination of copper in marine medicinal organisms, water samples and urine samples based on deep eutectic solvents (DES). Methods DES was prepared by mixing methytrioctylammonium bromide as hydrogen bond acceptor and decanoic acid as hydrogen bond donor at a molar ratio of 3∶1. At the appropriate phosphate concentration, copper in the target sample formed a chelate with ammonium pyrrolidinedithiocarbamate (APDC) at pH=5 and was enriched into the extraction phase, which was determined by atomic absorption spectrometry. The effects of pH, DES volume, vortex time, and concentration of chelating agent on the extraction efficiency were investigated. Results Under the optimal conditions, the linear range was good (r=0.998 5), the detection limit was 0.02 μg/L, and the relative standard deviations (RSD) was 7.75%. Copper in marine medicinal organisms was determined by this method, and the content was 2.98?23.50 mg/kg. The concentrations of copper in water and urine samples were 12.28?21.50 μg/L and 22.25?29.21 μg/L. Conclusion The method of vortex assisted DLLME-GFAAS based on DES was designed and optimized. It has the characteristics of high efficiency, convenience and sensitivity, and can be applied to the determination of copper in marine medicinal organisms, water and urine samples. |
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