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机构地区:[1]发光与实时分析化学教育部重点实验室、西南大学化学化工学院,重庆400715 [2]重庆市万州区环境监测站,重庆404020
出 处:《光谱学与光谱分析》2014年第6期1589-1593,共5页Spectroscopy and Spectral Analysis
基 金:国家自然科学基金项目(20877063);重庆市科委重点实验室专项经费项目资助
摘 要:在pH 为4.6的 HAc-NaAc介质中,盐酸巴马汀与桑色素通过静电引力发生反应,得到具有疏水性的离子缔合物,致使体系在308 nm处的共振光散射信号显著增强。研究表明,体系增强的共振光散射信号强度与盐酸巴马汀的浓度在0.08~1.0μmol·L^-1之间具有良好的线性关系,检测限为8.0 nmol·L^-1。由此建立了用于盐酸巴马汀检测的共振光散射分析方法。研究了体系的散射光谱和吸收光谱,通过扫描电镜和动态光散射考察离子缔合物的聚集情况并研究了体系的反应机理,研究了酸度及离子强度对体系的影响,最终实验选择pH 4.6的 HAc-NaAc缓冲,不加NaCl控制体系离子强度的情况下信号最佳。探讨了体系的稳定性,结果显示本反应体系反应迅速,5 min内散射强度即可达到最大值并至少能稳定120 min。考察了可能存在的共存物质的影响,结果发现常见的金属离子,无机阴离子,部分糖类及氨基酸不影响对盐酸巴马汀的检测。该方法具有简单,快速,灵敏度高的优点。该法成功用于实际药片和胶囊中盐酸巴马汀含量的测定,RSD≤3.3%。A novel resonance light scattering method for the determination of PaH was developed based on the interaction of Pal-matine hydrochloride (PaH)with Morin in pH 4. 6 HAc-NaAc buffer medium,and this interaction can result in largely enhanced resonance light scattering (RLS)signal characterized by a peak at 308. 0 nm.It was found that the enhanced RLS signals intensi-ty (IRLS)at 308. 0 nm is proportional to the concentration of PaH.The limit of detection is 8. 0 nmol·L^-1 and the linear range is from 0. 08 to 1. 0 mol·L^-1 .In this study,the mechanism of this reaction was investigated by scanning electron microscope (SEM),dynamic light scattering (DLS)and UV absorption spectrum.The SEM images and DLS graph show that ion-associa-tion complex aggregated after the addition of PaH .The experimental condition optimization results indicate that when the buffer medium is pH 4. 6 HAc-NaAc without adding NaCl,the system has a good response for PaH.The authors investigated the sta-bility of this system.The results indicate that this reaction system has a rapid response and the IRLS can reach the maximum within 5 min and remain stable at least for 120 min.The tolerance of coexisting foreign substances in the system was also stud-ied.The research results show that the common metal ions,inorganic anions,a part of carbohydrate and amino acids have negli-gible effects on the analysis of PaH .This proposed method has some advantages including simplicity,rapidity and sensitivity.It also has been applied to the detection of PaH in tablet and capsule samples with RSD≤3. 3%.
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