在线氧化衍生-HPLC荧光法在药物分析中的应用
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摘要
荧光衍生法扩大了荧光法的使用范围,对物质的分析具有灵敏度高、选择性好、信息量丰富、检测限低等优点,所以此方法在药物分析中具有极为重要的作用。近年来HPLC荧光衍生法的应用也成为药物分析的主要方法之一。而氧化还原反应作为荧光衍生法中的一种,可以将某些本身不具有或只有弱荧光的药物分子转化为含较强荧光的物质。本研究应用高效液相色谱-固相反应器在线氧化技术,建立了在线氧化衍生-HPLC荧光法测定甲氨蝶呤含量的方法,并结合固相萃取技术分析了血样中甲氨蝶呤的含量；建立了三种精神类药物含量同时测定的方法,并将此方法运用于动物饲料中三种精神类药物含量的测定。
本研究论文内容共包括三章。
第1章综述
首先,对药物分析的研究现状以及现有技术进行了概括。然后,综述了近年来所发表的有关应用在药物分析方面的各种荧光测定方法。接着,对高效液相色谱荧光法的各种衍生试剂、柱前柱后衍生方法以及相关文献作了概述。最后,展望了开发新的、灵敏度高、方便快捷的测定药物含量方法的应用前景。
第2章在线氧化衍生-HPLC荧光法测定甲氨蝶呤
甲氨蝶呤自身只有微弱荧光,经氧化后可转变为最大激发波长λex=367nm,最大发射波长λem=457nm的强荧光物质,本文建立了HPLC结合醋酸纤维素固定化的二氧化铅固相反应器在线氧化荧光法测定甲氨蝶呤的新方法,对实验条件进行了优化。结果表明该方法具有线性范围宽、精密度高、检测限低、选择性好等特点。并且成功地应用于药物制剂中甲氨蝶呤含量的测定,测定结果与药典中的高效液相色谱法进行了比较,结果一致。再结合固相萃取前处理技术,成功地建立了确定人血样中甲氨蝶呤含量的新方法,并通过加标回收实验确定了方法的准确性。
第3章在线氧化衍生-HPLC荧光法同时测定三种精神类药物
氯丙嗪、盐酸硫利达嗪、氯普噻吨三种三环类化合物可在酸性介质中被二氧化铅氧化成强荧光物质。本研究利用HPLC结合固相反应器建立了同时分析三种精神类药物含量的新方法,对检测波长、流动相组成、酸度及温度等条件进行了优化。并将此方法成功地应用于测定动物饲料中三种精神类药物的含量。
Fluorescent derivatization with high sensitivity and selectivity, information-rich and low detection limit expands the range of the use of the fluorescence method, which makes it play a very important role in drug analysis. In recent years, HPLC coupled with fluorescence derivatization application has also become one of the main method of drug analysis. Redox reaction is one of the ways of fluorescent derivatization, through which the ones themselves have no or only weak fluorescence turn to strong fluorescence substance. In this thesis, we used HPLC coupled with online solid-phase oxidation reactor established the HPLC coupled with on-line oxidizing with fluorescence detection method for determination MTX in table and plasma samples, respectively. Besides, we also proposed a new method to simultaneously analyzed the three psychiatric drugs, and applied to the determination of the content of the three psychiatric drugs in animal feed.
There are three chapters in this thesis.
Chapter one:review
First, current research and existing technologies of drug analysis had been summarized. Then on the basis of the literature in recent years, a variety of fluorescence method on the applications in pharmaceutical analysis were reviewed. After that, related literatures about the derivate methods, a variety of derivatization reagents, pre-column derivatization and post-column derivatization for HPLC-fluorescence detection methods were summarized. Finally, we did the future application prospects of the development of a new, high sensitivity, convenient and fast method of analysis the content of the drugs.
Chapter two:on-line oxidation derivatization combined with HPLC-fluorescence detection for the determination of methotrexate.
Methotrexate itself with only weak fluorescence through oxidation could be transformed into strongly fluorescent substance with maximum excitation wavelength at λex=367nm, maximum emission wavelength at λem=457nm. We used the method, which was HPLC-fluorescence detection coupled with a solid-phase reactor of the immobilization of the lead oxide with cellulose acetate, to analysis the content of MTX. The experimental conditions had been studied and optimized. The results showed that this method had a wide linear range, low detection limit, high precision and good selectivity. The method was successfully applied to the determination of methotrexate in tablet. The result was consistent with the HPLC. Besides, combined with SPE, we successfully established a new method for determination of methotrexate in human blood, and the spiked recovery experiments had been determined.
Chapter three:on-line oxidation derivatization combined with HPLC-fluorescence detection for the simultaneous determination of three psychotropic drugs.
Chlorpromazine, thioridazine hydrochloride, chlorprothixene tricyclic compounds in acidic media could be oxidated to strongly fluorescent substances by lead dioxide. In this study, we used HPLC-fluorescence detection combined with solid phase reactor to establish a new method for the simultaneous analysis of the content of the three psychotropic drugs. The detection wavelength, mobile phase composition, acidity and temperature were optimized. And this method was successfully applied to determine of the content of the three psychiatric drugs in animal feed.
本研究论文内容共包括三章。
第1章综述
首先,对药物分析的研究现状以及现有技术进行了概括。然后,综述了近年来所发表的有关应用在药物分析方面的各种荧光测定方法。接着,对高效液相色谱荧光法的各种衍生试剂、柱前柱后衍生方法以及相关文献作了概述。最后,展望了开发新的、灵敏度高、方便快捷的测定药物含量方法的应用前景。
第2章在线氧化衍生-HPLC荧光法测定甲氨蝶呤
甲氨蝶呤自身只有微弱荧光,经氧化后可转变为最大激发波长λex=367nm,最大发射波长λem=457nm的强荧光物质,本文建立了HPLC结合醋酸纤维素固定化的二氧化铅固相反应器在线氧化荧光法测定甲氨蝶呤的新方法,对实验条件进行了优化。结果表明该方法具有线性范围宽、精密度高、检测限低、选择性好等特点。并且成功地应用于药物制剂中甲氨蝶呤含量的测定,测定结果与药典中的高效液相色谱法进行了比较,结果一致。再结合固相萃取前处理技术,成功地建立了确定人血样中甲氨蝶呤含量的新方法,并通过加标回收实验确定了方法的准确性。
第3章在线氧化衍生-HPLC荧光法同时测定三种精神类药物
氯丙嗪、盐酸硫利达嗪、氯普噻吨三种三环类化合物可在酸性介质中被二氧化铅氧化成强荧光物质。本研究利用HPLC结合固相反应器建立了同时分析三种精神类药物含量的新方法,对检测波长、流动相组成、酸度及温度等条件进行了优化。并将此方法成功地应用于测定动物饲料中三种精神类药物的含量。
Fluorescent derivatization with high sensitivity and selectivity, information-rich and low detection limit expands the range of the use of the fluorescence method, which makes it play a very important role in drug analysis. In recent years, HPLC coupled with fluorescence derivatization application has also become one of the main method of drug analysis. Redox reaction is one of the ways of fluorescent derivatization, through which the ones themselves have no or only weak fluorescence turn to strong fluorescence substance. In this thesis, we used HPLC coupled with online solid-phase oxidation reactor established the HPLC coupled with on-line oxidizing with fluorescence detection method for determination MTX in table and plasma samples, respectively. Besides, we also proposed a new method to simultaneously analyzed the three psychiatric drugs, and applied to the determination of the content of the three psychiatric drugs in animal feed.
There are three chapters in this thesis.
Chapter one:review
First, current research and existing technologies of drug analysis had been summarized. Then on the basis of the literature in recent years, a variety of fluorescence method on the applications in pharmaceutical analysis were reviewed. After that, related literatures about the derivate methods, a variety of derivatization reagents, pre-column derivatization and post-column derivatization for HPLC-fluorescence detection methods were summarized. Finally, we did the future application prospects of the development of a new, high sensitivity, convenient and fast method of analysis the content of the drugs.
Chapter two:on-line oxidation derivatization combined with HPLC-fluorescence detection for the determination of methotrexate.
Methotrexate itself with only weak fluorescence through oxidation could be transformed into strongly fluorescent substance with maximum excitation wavelength at λex=367nm, maximum emission wavelength at λem=457nm. We used the method, which was HPLC-fluorescence detection coupled with a solid-phase reactor of the immobilization of the lead oxide with cellulose acetate, to analysis the content of MTX. The experimental conditions had been studied and optimized. The results showed that this method had a wide linear range, low detection limit, high precision and good selectivity. The method was successfully applied to the determination of methotrexate in tablet. The result was consistent with the HPLC. Besides, combined with SPE, we successfully established a new method for determination of methotrexate in human blood, and the spiked recovery experiments had been determined.
Chapter three:on-line oxidation derivatization combined with HPLC-fluorescence detection for the simultaneous determination of three psychotropic drugs.
Chlorpromazine, thioridazine hydrochloride, chlorprothixene tricyclic compounds in acidic media could be oxidated to strongly fluorescent substances by lead dioxide. In this study, we used HPLC-fluorescence detection combined with solid phase reactor to establish a new method for the simultaneous analysis of the content of the three psychotropic drugs. The detection wavelength, mobile phase composition, acidity and temperature were optimized. And this method was successfully applied to determine of the content of the three psychiatric drugs in animal feed.
引文
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