加替沙星和磺胺嘧啶检测方法研究
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摘要
药品质量的优劣,直接关系到患者的身体健康乃至生命安全。因此,为了确保人们用药的安全、合理和有效,必须对药品质量进行全面控制。能够简便、快速地从复杂样品中可靠、灵敏地检测出痕量药物成分是当前药物分析的发展趋势。适应这一要求,光谱法因其设备简单、操作方便、准确度好、灵敏度高以及适用范围广等优点成了药物分析中最基本和最主要的研究手段之一。
本文以光谱法作为检测手段,探寻检测加替沙星、磺胺嘧啶更简单、更灵敏的方法,主要研究内容包括:
一、综述了加替沙星和磺胺嘧啶测定方法研究现状。
二、建立了利用荧光光度法测定加替沙星新方法:在pH6.0的B-R缓冲溶液中,刚果红能与钙黄绿素生成配合物,使钙黄绿素荧光猝灭,加入加替沙星后,加替沙星与刚果红可生成比钙黄绿素-刚果红更稳定的配合物,使钙黄绿素游离重现荧光。将该方法用于片剂、粉针剂和尿液中加替沙星的测定,结果与文献报道的紫外法一致。
三、用紫外光谱和同原射线计量分析法同时测定加替沙星和左氧氟沙星:铝离子和十二烷基硫酸钠(SDS)与加替沙星(GFLX)、左氧氟沙星(LVFX)均能反应形成离子缔合物,两者最大吸收波长均在292nm处,其差异仅在于两吸光强度随浓度线性增幅不同,据此建立了双组分信号响应的两条同原射线计量分析法。四、研究了在不同酸度条件下茜素红-Al3+-磺胺嘧啶体系:磺胺嘧啶能使茜素红紫外吸收峰增强,加入Al3+后,吸光度进一步增强。在pH4.50的B-R缓冲溶液体系中,体系的最大吸收波长为261nm,在一定浓度范围内,吸光度与磺胺嘧啶浓度成线性关系,据此建立了在pH4.50的体系中测定磺胺嘧啶的新方法;在pH10.00的B-R缓冲溶液体系中,体系的最大吸收波长为261nm,在一定浓度范围内,吸光度与磺胺嘧啶浓度成线性关系,据此建立了在pH10.00体系中测定磺胺嘧啶的方法。实际工作中,可根据样品测定的实际需要选择酸性或碱性条件下测定。将此两种方法用于片剂和尿液中磺胺嘧啶含量的测定,结果与文献报道的荧光法一致。
五、建立了表面活性剂增敏二甲酚橙显色测定磺胺嘧啶的方法:研究了多种表面活性剂对二甲酚橙-磺胺嘧啶显色反应体系的影响。实验表明,氯代十六烷基吡啶(CPC)和十六烷基三甲基溴化铵(CTAB)对该体系有显著的增敏作用;据此分别建立了氯代十六烷基吡啶(CPC)、十六烷基三甲基溴化铵(CTAB)增敏二甲酚橙显色测定磺胺嘧啶的方法。将这两种方法用于片剂中磺胺嘧啶含量测定,结果满意。
Pharmaceutcial quality directly affects the sufferers’life health and safety. Therefore, Pharmaceutcial quality must be controlled comprehensively in order to ensure its safty, reasonableness, validity when it is used.
Nowadays, the trend of pharmaceutcial analysis is to determine the trace pharmaceutcial ingredient of the complex samples simply and reliably. Therefore, Spectrographic method has become one of the most essential and important methods in the determination of pharmic products due to its easy apparatus, simple procedure, high selectivity and sensitivity.
The aim of this dissertation is to explore simpler, more sensitive determination methods of Gatifloxacin(GFLX) and Surfactantsa(SD), with using spectrophotometry as research means. The major contents are described as follows :
1.A somewhat through and all-around review of the application of methods in the analysis of Gatifloxacin and Surfactantsa is given in this part.
2.Established a fluorometry for the determination of GFLX:The interaction between Congo Red(CR)and Calcein in pH 6.00Britton-Robinson buffer solution. resulted in a fluorescence intensity of Calcein decreasement. Addition of GFLX into the Calcein-CR system, the fluorescence intensity was enhanced. This method has been applied for the determination of GFLX in tablet, injection and urine, and the results were very close to those obtained by the UV method reported.
3.Simultaneous determination of Gatifloxacin and Levofloxacin by spectrophotometry and measurement analysis of two lines with same one point.The Al~(3+) and Sodium Dodecyl Sulfate (SDS) could react with Gatifloxacin and Levofloxacin to form ion-association complexes, their UV absorption spectra were located at 292 nm and the difference was their linear amplification different as their Concentration. It is based on the difference a novel method for simultaneous determination of Gatifloxacin and Levofloxacin had been developed with“measurement analysis of two lines with one same point”.
4.Researched the alizarin red-Al3+-SD system in different acidity.SD can enhance a UV absorbance of ARS, addition of Al3+ into the ARS-GFLX system, the absorbance was much stronger. Then maximum absorbance at 261nm in pH 4.50 Britton-Robinson buffer solution and at 259nm in pH 10.00. So the contents were calculated according to the standard curves. In practical work,we can determine SD use appropriate method in pH 4.50 or in pH 10.00 by required. Both of methods have been applied for the determination of SD in tablet and urine, and the results were very close to those obtained by the fluorimetry method reported.
5.Investigated SD by its reaction with XO develop the color system in the presence of surface active agent CPC or CTAB. Study most of surface active agents, such as positive ions, negative ions and non ions. The study shows that CPC and CTAB have the most enhance function. So established two methods of determine SD.XO -SD- CPC and XO -SD- CTAB color systems have the special feature of good inrapidily seasieivity and stability. Used in the survey of the content of SD in the tablet.The results are satisfied.
本文以光谱法作为检测手段,探寻检测加替沙星、磺胺嘧啶更简单、更灵敏的方法,主要研究内容包括:
一、综述了加替沙星和磺胺嘧啶测定方法研究现状。
二、建立了利用荧光光度法测定加替沙星新方法:在pH6.0的B-R缓冲溶液中,刚果红能与钙黄绿素生成配合物,使钙黄绿素荧光猝灭,加入加替沙星后,加替沙星与刚果红可生成比钙黄绿素-刚果红更稳定的配合物,使钙黄绿素游离重现荧光。将该方法用于片剂、粉针剂和尿液中加替沙星的测定,结果与文献报道的紫外法一致。
三、用紫外光谱和同原射线计量分析法同时测定加替沙星和左氧氟沙星:铝离子和十二烷基硫酸钠(SDS)与加替沙星(GFLX)、左氧氟沙星(LVFX)均能反应形成离子缔合物,两者最大吸收波长均在292nm处,其差异仅在于两吸光强度随浓度线性增幅不同,据此建立了双组分信号响应的两条同原射线计量分析法。四、研究了在不同酸度条件下茜素红-Al3+-磺胺嘧啶体系:磺胺嘧啶能使茜素红紫外吸收峰增强,加入Al3+后,吸光度进一步增强。在pH4.50的B-R缓冲溶液体系中,体系的最大吸收波长为261nm,在一定浓度范围内,吸光度与磺胺嘧啶浓度成线性关系,据此建立了在pH4.50的体系中测定磺胺嘧啶的新方法;在pH10.00的B-R缓冲溶液体系中,体系的最大吸收波长为261nm,在一定浓度范围内,吸光度与磺胺嘧啶浓度成线性关系,据此建立了在pH10.00体系中测定磺胺嘧啶的方法。实际工作中,可根据样品测定的实际需要选择酸性或碱性条件下测定。将此两种方法用于片剂和尿液中磺胺嘧啶含量的测定,结果与文献报道的荧光法一致。
五、建立了表面活性剂增敏二甲酚橙显色测定磺胺嘧啶的方法:研究了多种表面活性剂对二甲酚橙-磺胺嘧啶显色反应体系的影响。实验表明,氯代十六烷基吡啶(CPC)和十六烷基三甲基溴化铵(CTAB)对该体系有显著的增敏作用;据此分别建立了氯代十六烷基吡啶(CPC)、十六烷基三甲基溴化铵(CTAB)增敏二甲酚橙显色测定磺胺嘧啶的方法。将这两种方法用于片剂中磺胺嘧啶含量测定,结果满意。
Pharmaceutcial quality directly affects the sufferers’life health and safety. Therefore, Pharmaceutcial quality must be controlled comprehensively in order to ensure its safty, reasonableness, validity when it is used.
Nowadays, the trend of pharmaceutcial analysis is to determine the trace pharmaceutcial ingredient of the complex samples simply and reliably. Therefore, Spectrographic method has become one of the most essential and important methods in the determination of pharmic products due to its easy apparatus, simple procedure, high selectivity and sensitivity.
The aim of this dissertation is to explore simpler, more sensitive determination methods of Gatifloxacin(GFLX) and Surfactantsa(SD), with using spectrophotometry as research means. The major contents are described as follows :
1.A somewhat through and all-around review of the application of methods in the analysis of Gatifloxacin and Surfactantsa is given in this part.
2.Established a fluorometry for the determination of GFLX:The interaction between Congo Red(CR)and Calcein in pH 6.00Britton-Robinson buffer solution. resulted in a fluorescence intensity of Calcein decreasement. Addition of GFLX into the Calcein-CR system, the fluorescence intensity was enhanced. This method has been applied for the determination of GFLX in tablet, injection and urine, and the results were very close to those obtained by the UV method reported.
3.Simultaneous determination of Gatifloxacin and Levofloxacin by spectrophotometry and measurement analysis of two lines with same one point.The Al~(3+) and Sodium Dodecyl Sulfate (SDS) could react with Gatifloxacin and Levofloxacin to form ion-association complexes, their UV absorption spectra were located at 292 nm and the difference was their linear amplification different as their Concentration. It is based on the difference a novel method for simultaneous determination of Gatifloxacin and Levofloxacin had been developed with“measurement analysis of two lines with one same point”.
4.Researched the alizarin red-Al3+-SD system in different acidity.SD can enhance a UV absorbance of ARS, addition of Al3+ into the ARS-GFLX system, the absorbance was much stronger. Then maximum absorbance at 261nm in pH 4.50 Britton-Robinson buffer solution and at 259nm in pH 10.00. So the contents were calculated according to the standard curves. In practical work,we can determine SD use appropriate method in pH 4.50 or in pH 10.00 by required. Both of methods have been applied for the determination of SD in tablet and urine, and the results were very close to those obtained by the fluorimetry method reported.
5.Investigated SD by its reaction with XO develop the color system in the presence of surface active agent CPC or CTAB. Study most of surface active agents, such as positive ions, negative ions and non ions. The study shows that CPC and CTAB have the most enhance function. So established two methods of determine SD.XO -SD- CPC and XO -SD- CTAB color systems have the special feature of good inrapidily seasieivity and stability. Used in the survey of the content of SD in the tablet.The results are satisfied.
引文
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