共振光散射技术在有机小分子药物分析中的应用研究
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摘要
共振光散射(Resonance Light Scattering, RLS)技术是二十世纪九十年代发展起来的新分析技术,它以仪器廉价,操作方便,快速,灵敏度高等优点引起人们的广泛关注和浓厚兴趣。目前该技术已广泛应用于金属离子、核酸、蛋白质、糖类等的研究和测定中。在药物分析中的应用也日益增多。本文采用共振光散射技术对异烟肼、对乙酰氨基酚、盐酸巴马汀等有机小分子药物的含量进行了测定。主要研究内容如下：
(1)在酸性介质中,异烟肼能将铁氰酸根离子还原成亚铁氰酸根离子,后者与硫酸锌反应生成K2Zn3[Fe(CN)6]2粒子引起体系的共振光散射信号显著增强。在345 nm处增强的散射信号强度ΔIRLS与异烟肼的浓度在0.01～1.0μg/mL范围内呈线性关系,据此建立了一种检测异烟肼含量的共振光散射(RLS)分析方法。线性回归方程为ΔIRLS=136.1+4239 c(c,μg/mL),相关系数(r)为0.9984,检测限(3σ)为3.8 ng/mL。该方法已成功用于异烟肼片剂及血清样品的测定。此外,文中还结合吸收光谱,动态光散射,扫描电子显微镜等表征手段对反应机理和RLS信号强度增强的原因进行了探讨。
(2)在酸性介质中,对乙酰氨基酚将铁氰酸根离子还原成亚铁氰酸根离子,后者与硫酸锌反应生成K2Zn3[Fe(CN)6]2粒子引起体系的共振光散射信号显著增强,且345nm处增强的散射信号强度ΔIRLS与对乙酰氨基酚的浓度在0.01～1.0μg/mL范围内呈良好线性关系。其线性回归方程为ΔIRLS=-15.01+4214 c(c,μg/mL),相关系数(r)为0.9992。据此建立了一种检测对乙酰氨基酚含量的共振光散射分析方法。该方法具有较高的灵敏度,检测限(3σ)为7.4ng/mL。用于对乙酰氨基酚片剂的测定,RSD≤2.8%。
(3)在酸性条件下,盐酸巴马汀与I3-反应形成离子缔合物,导致体系的共振光散射信号显著增强,且增强的散射信号与盐酸巴马汀的浓度在0.02～3.2μg/mL范围呈良好的线性关系,据此提出了一种测定盐酸巴马汀的共振光散射分析方法。该方法具有较高的灵敏度,其检测限(3σ)为1.3ng/mL。已成功用于黄藤素制剂的测定。
Resonance Light Scattering (RLS) technique is a new analytical technology developed in recent ten years. It has attracted considerable attentions and interestings for its cheap instrument, simple operation, rapid analysis speed and high sensitivity. At present, RLS technique has been applied to the study and the determination of metallic ions, nucleic acids, proteins and saccharide. Furthermore, this technique has been more and more used to determination of some pharmaceuticals. In this dissertation, RLS technique has been applied to the analysis of organic small molecule medicines, such as isoniazid, paracetamol and palmation chloride. The main contents are as follows:
(1) In acidic medium, a novel resonance light scattering (RLS) analytical method of isoniazid is developed based on RLS signal enhancement due to the interaction of Zn2+ and ferrocyanide ion derived from ferricyanide ion by isoniazid. The enhanced RLS intensity at 345 nm is proportional to the content of isoniazid in a range of 0.01 1.0μg/mL. The linear regression equation isΔIRLS=136.1+4239 c (c,μg/mL). The correlation coefficient r is 0.9984. The limit of detection is 3.8 ng/mL. This method has been successfully applied to the determination of isoniazid in pharmaceutical and serum samples. In this work, the reaction mechanism and the reasons of scattering enhanced have been also investigated by using absorption spectra, dynamic light scattering and SEM.
(2) In acidic medium, ferricyanide ion was reduced to ferrocyanide ion by paracetamol (PCT). In addition, the formed ferrocyanide ion reacted with Zn2+to form K2Zn3[Fe(CN)6]2 particles, which enhanced the resonance light scattering (RLS) intensity greatly. The enhanced RLS intensity at 345 nm is proportional to the content of paracetamol in a range of 0.01～1.0μg/mL. The linear regression equation isΔIRLS=-15.01+4214 c (c,μg/mL). The correlation coefficients r is 0.9992. The limit of detection is 7.4 ng/mL. Based on these results, a novel resonance light scattering analytical method of paracetamol was established. This method has been successfully applied to the determination of paracetamol in tablets, the RSD≤2.8%.
(3) In acidic medium, a novel resonance light scattering (RLS) analytical method of palmation chloride has been developed based on RLS signal enhancement due to the interaction of palmation chloride and I3-. Palmation chloride reacted with I3- to form an ion-association complex. The RLS intensity is proportional to the concentration of palmation chloride in the range of 0.02～3.2μg/mL. The limit of detection(3σ) is 1.3 ng/mL. It has been successfully applied to the determination of palmation chloride in pharmaceuticals.
(1)在酸性介质中,异烟肼能将铁氰酸根离子还原成亚铁氰酸根离子,后者与硫酸锌反应生成K2Zn3[Fe(CN)6]2粒子引起体系的共振光散射信号显著增强。在345 nm处增强的散射信号强度ΔIRLS与异烟肼的浓度在0.01～1.0μg/mL范围内呈线性关系,据此建立了一种检测异烟肼含量的共振光散射(RLS)分析方法。线性回归方程为ΔIRLS=136.1+4239 c(c,μg/mL),相关系数(r)为0.9984,检测限(3σ)为3.8 ng/mL。该方法已成功用于异烟肼片剂及血清样品的测定。此外,文中还结合吸收光谱,动态光散射,扫描电子显微镜等表征手段对反应机理和RLS信号强度增强的原因进行了探讨。
(2)在酸性介质中,对乙酰氨基酚将铁氰酸根离子还原成亚铁氰酸根离子,后者与硫酸锌反应生成K2Zn3[Fe(CN)6]2粒子引起体系的共振光散射信号显著增强,且345nm处增强的散射信号强度ΔIRLS与对乙酰氨基酚的浓度在0.01～1.0μg/mL范围内呈良好线性关系。其线性回归方程为ΔIRLS=-15.01+4214 c(c,μg/mL),相关系数(r)为0.9992。据此建立了一种检测对乙酰氨基酚含量的共振光散射分析方法。该方法具有较高的灵敏度,检测限(3σ)为7.4ng/mL。用于对乙酰氨基酚片剂的测定,RSD≤2.8%。
(3)在酸性条件下,盐酸巴马汀与I3-反应形成离子缔合物,导致体系的共振光散射信号显著增强,且增强的散射信号与盐酸巴马汀的浓度在0.02～3.2μg/mL范围呈良好的线性关系,据此提出了一种测定盐酸巴马汀的共振光散射分析方法。该方法具有较高的灵敏度,其检测限(3σ)为1.3ng/mL。已成功用于黄藤素制剂的测定。
Resonance Light Scattering (RLS) technique is a new analytical technology developed in recent ten years. It has attracted considerable attentions and interestings for its cheap instrument, simple operation, rapid analysis speed and high sensitivity. At present, RLS technique has been applied to the study and the determination of metallic ions, nucleic acids, proteins and saccharide. Furthermore, this technique has been more and more used to determination of some pharmaceuticals. In this dissertation, RLS technique has been applied to the analysis of organic small molecule medicines, such as isoniazid, paracetamol and palmation chloride. The main contents are as follows:
(1) In acidic medium, a novel resonance light scattering (RLS) analytical method of isoniazid is developed based on RLS signal enhancement due to the interaction of Zn2+ and ferrocyanide ion derived from ferricyanide ion by isoniazid. The enhanced RLS intensity at 345 nm is proportional to the content of isoniazid in a range of 0.01 1.0μg/mL. The linear regression equation isΔIRLS=136.1+4239 c (c,μg/mL). The correlation coefficient r is 0.9984. The limit of detection is 3.8 ng/mL. This method has been successfully applied to the determination of isoniazid in pharmaceutical and serum samples. In this work, the reaction mechanism and the reasons of scattering enhanced have been also investigated by using absorption spectra, dynamic light scattering and SEM.
(2) In acidic medium, ferricyanide ion was reduced to ferrocyanide ion by paracetamol (PCT). In addition, the formed ferrocyanide ion reacted with Zn2+to form K2Zn3[Fe(CN)6]2 particles, which enhanced the resonance light scattering (RLS) intensity greatly. The enhanced RLS intensity at 345 nm is proportional to the content of paracetamol in a range of 0.01～1.0μg/mL. The linear regression equation isΔIRLS=-15.01+4214 c (c,μg/mL). The correlation coefficients r is 0.9992. The limit of detection is 7.4 ng/mL. Based on these results, a novel resonance light scattering analytical method of paracetamol was established. This method has been successfully applied to the determination of paracetamol in tablets, the RSD≤2.8%.
(3) In acidic medium, a novel resonance light scattering (RLS) analytical method of palmation chloride has been developed based on RLS signal enhancement due to the interaction of palmation chloride and I3-. Palmation chloride reacted with I3- to form an ion-association complex. The RLS intensity is proportional to the concentration of palmation chloride in the range of 0.02～3.2μg/mL. The limit of detection(3σ) is 1.3 ng/mL. It has been successfully applied to the determination of palmation chloride in pharmaceuticals.
引文
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