卡波姆、羧甲基纤维素钠自聚集作用的共振散射光谱及其应用研究
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摘要
论文概述了共振散射技术的基本概念、研究现状及应用。建立一个新的无荧光探针的共振散射技术研究卡波姆及羧甲基纤维素钠(CMC-Na)的自聚集作用,并用于卡波姆及CMC-Na的含量测定。本论文共分为三章。
     第一章本章概述了光散射概念及分类,共振光散射技术基本概念、特点、发展及其在生物大分子、药物分析、金属离子分析等方面的应用,从而提出本课题研究的意义。
     第二章本章主要用共振散射技术研究不同型号卡波姆在酸性条件下(pH=2.0)的自聚集作用。实验中考察了不同pH值、不同缓冲介质、有机溶剂的含量、稳定性、离子强度、干扰物质等的影响。优选出条件为pH=2.0磷酸盐缓冲液。用共振散射技术研究卡波姆的自聚集作用具有较好的稳定性,在一定范围内不受离子强度、干扰物质的影响。
     卡波姆940在20~120μg·mL~(-1)之间线性关系良好,相关系数r=0.9997。进一步用于卡波姆940样品的含量测定,其含量分别为0.993、1.006、1.032、0.986 mg·mL~(-1),与实际含量接近,RSD(%)分别为0.57、0.82、0.42、0.56。平均加样回收率(%)分别为100.9、98.8、100.9、100.9,RSD(%)分别为0.98、1.64、1.11、2.09。结果表明,用共振散射方法分析卡波姆940样品,方法简便、快速,灵敏度高,具有较好的准确度和重复性,并能在较大限度范围内排除干扰。该法可用于样品中卡波姆940的含量测定。
     卡波姆971P在50~300μg·mL~(-1)之间线性关系良好,相关系数r=0.9996。进一步应用于卡波姆971P样品的含量测定,其含量分别为0.980、0.956、1.000、1.012 mg·mL~(-1),与实际含量接近,RSD(%)分别为1.00、1.37、0.59、1.97。平均加样回收率(%)分别为96.2、97.3、96.8、97.4,RSD(%)分别为0.94、0.42、1.66、1.14。结果表明,用共振散射方法分析卡波姆971P样品,灵敏度较高,方法简便、快速,具有较好的准确度和重复性,并能在较大限度范围内排除干扰。该法可用于样品中卡波姆971P的含量测定。
     卡波姆974P在20~300μg·mL~(-1)之间线性关系良好,相关系数r=0.9994。进一步应用于抗生素缓释凝胶、盐酸达克罗宁凝胶中卡波姆974P的含量测定。抗生素缓释凝胶中卡波姆974P的含量分别为37.45、37.33、37.33 mg·g~(-1),RSD(%)分别为1.13、1.04、1.34。平均加样回收率(%)分别为100.6、95.0、97.2,RSD(%)分别为1.35、0.52、2.36。盐酸达克罗宁凝胶中卡波姆974P的含量分别为13.69、13.52、13.06 mg·g~(-1),RSD(%)分别为1.40、1.03、0.39。平均加样回收率(%)分别为98.0、99.1、95.6,RSD(%)分别为1.22、0.77、1.19。结果表明,用共振散射方法分析样品中的卡波姆974P,灵敏度较高,方法简便、快速,具有较好的准确度和重复性。该法可用于样品中卡波姆974P的含量测定。
     第三章本章主要用共振散射技术研究CMC-Na在酸性条件下(pH=2.0)的自聚集作用。实验中考察了不同pH值,不同缓冲介质,有机溶剂的含量,稳定性,离子强度,干扰物质等的影响。优选出条件为pH=2.0磷酸盐缓冲液。用共振散射技术研究CMC-Na的自聚集作用具有较好的稳定性,在一定范围内不受离子强度、干扰物质的影响。同时,发现其在10~200μg·mL~(-1)之间线性关系良好,相关系数r=0.9993。进一步用于羧甲基纤维素钠滴眼液、甲硝唑灌肠液及CMC-Na样品中CMC-Na的含量测定。羧甲基纤维素钠滴眼液中CMC-Na的含量分别为1.937、1.941、1.928 mg·支~(-1),RSD(%)分别为2.16、2.67、1.58。平均加样回收率(%)分别为95.3、103.7、95.0,RSD(%)分别为1.08、1.26、1.58。甲硝唑灌肠液中CMC-Na的含量分别为1.900、2.032、1.940 mg·mL~(-1),RSD(%)分别为0.36、0.97、1.27。平均加样回收率(%)分别为95.7、103.7、100.3,RSD(%)分别为0.76、1.26、0.71。CMC-Na样品中CMC-Na的含量分别为1.040、1.013、1.035 mg·mL~(-1),RSD(%)分别为0.28、0.90、0.37。平均加样回收率(%)分别为99.3、102.8、98.4,RSD(%)分别为1.62、0.84、1.20。结果表明,用共振散射技术分析样品中的CMC-Na,灵敏度高,方法简便、快速,具有较好的准确度和重复性。该法可用于样品中CMC-Na的含量测定。
The basic concept,current situation and application of resonance light scattering (RLS)were summarized. A novel free-probe study of carbomers and sodium carboxymethylcellulose (CMC-Na)was established based on their self-aggregations by RLS,and this technique was used for the assay of carbomers and CMC-Na in samples. This dissertation concretely consist of the following three chapters.
     Chapter 1
     The concept and classification of light scattering and the basic concepts ,characteristics,development and applications such as biological macromolecules,drug and metal ions analysis of RLS were summarized.And then the significance of these researches was put forward.
     Chapter 2
     In this chapter,the self-aggregations of different types of carbomers were discussed by RLS in the acidic condition(pH = 2.0). The main influencing factors such as pH values, buffer medium,content of organic solvent,stability,ionic strength and interfering substances were investigated in detail. Phosphate buffer(pH = 2.0)was obtained as optimum conditions.In the study of carbomers based on their self-aggregations by RLS,good stability was obtained and no interference was presented in the detection when adding ionic and interfering substances.
     The RLS intensity was well proportional to the concentration of carbomer 940 over the wide range 20~120μg·mL~(-1) with r=0.9997 in the optimum conditions. The contents of carbomer 940 samples,which were almost identical to the actual ones,were analysed with the results as follows:0.993,1.006,1.032,0.986 mg·mL~(-1),and RSD(%)were 0.57,0.82,0.42,0.56,respectively. The average recoveries(%)were 100.9,98.8,100.9,100.9,and RSD(%)were 0.98,1.64,1.11,2.09,respectively. The results proved that the carbomer 940 samples analysed by the RLS owned the characteristics of easy operation,rapidity,sensitivity,good accuracy and repeatability,and also could eliminate the interfering substances in the large range. Based on this study,RLS can be used for the determination of carbomer 940 in the samples.
     The RLS intensity was well proportional to the concentration of carbomer 971P over the wide range 50~300μg·mL~(-1) with r=0.9996 in the optimum conditions. The contents of carbomer 971P samples,which were almost identical to the actual ones,were analysed with the results as follows:0.980,0.956,1.000,1.012 mg·mL~(-1),and RSD(%)were 1.00,1.37,0.59,1.97,respectively. The average recoveries(%)were 96.2,97.3,96.8,97.4, and RSD(%)were 0.94,0.42,1.66,1.14,respectively. The results proved that the carbomer 971P samples analysed by RLS owned the characteristics of easy operation,rapidity,sensitivity,good accuracy and repeatability,and also could eliminate the interfering substances in the large range. Based on this study,RLS can be used for the determination of carbomer 971P in the samples.
     The RLS intensity was well proportional to the concentration of carbomer 974P over the wide range 20~300μg·mL~(-1) with r=0.9994 in the optimum conditions. And the technique was used for analysing carbomer 974P in antibiotics sustained release gel and dyclonine hydrochloride gel. The contents of carbomer 974P in antibiotics sustained release gel were analysed with the results as follows:37.45,37.33,37.33 mg·mg~(-1),and RSD(%)were 1.13,1.04,1.34,respectively. The average recoveries(%)were 100.6,95.0,97.2, and RSD(%)were 1.35,0.52,2.36,respectively. The contents of carbomer 974P in dyclonine hydrochloride gel were analysed with the results as follows:13.69,13.52,13.06 mg·g~(-1),and RSD(%)were 1.40,1.03,0.39,respectively. The average recoveries(%) were 98.0,99.1,95.6,and RSD(%)were 1.22,0.77,1.19,respectively. The results proved that the carbomer 974P samples analysed by the RLS owned the characteristics of easy operation,rapidity,sensitivity,good accuracy and repeatability,and also could eliminate the interfering substances in the large range. Based on this study,RLS can be used for the determination of carbomer 974P in the samples.
     Chapter 3
     In this chapter,the self-aggregation of CMC-Na was discussed by RLS in the acidic condition(pH = 2.0). The main influencing factors such as pH values,buffer medium,content of organic solvent,stability,ionic strength and interfering substances were investigated in detail. Phosphate buffer (pH = 2.0) was obtained as optimum conditions. In the study of CMC-Na based on its self-aggregation by RLS,good stability was obtained and no interference was presented in the detection when adding ionic and interfering substances. It was found that the RLS intensity was well proportional to the concentration of CMC-Na over the wide range 10~200μg·mL~(-1) with r=0.9993 in the optimum conditions. And then the technique was used for analysing CMC-Na in CMC-Na eye drops,metronidazole clyster liquid and CMC-Na samples. The contents of CMC-Na in CMC-Na eye drops were analysed with the results as follows:1.937,1.941,1.928 mg·mL~(-1),and RSD(%)were 2.16,2.67,1.58,respectively. The average recoveries (%) were 95.3,103.7,95.0,and RSD(%)were 1.08,1.26,1.58,respectively. The contents of CMC-Na in metronidazole clyster liquid were analysed with the results as follows:1.900,2.032,1.940 mg·g~(-1),and RSD(%)were 0.36,0.97,1.27,respectively. The average recoveries(%)were 95.7,103.7,100.3,and RSD(%)were 0.76,1.26,0.71,respectively. The contents of CMC-Na in CMC-Na samples were analysed with the results as follows:1.040,1.013,1.035 mg·g~(-1),and RSD(%)were 0.28,0.90,0.37,respectively. The average recoveries(%)were 99.3,102.8,98.4,and RSD(%)were 1.62,0.84,1.20,respectively. The results proved that the CMC-Na samples analysed by RLS owned the characteristics of easy operation,rapidity,sensitivity,good accuracy and repeatability,and also could eliminate the interfering substances in the large range. Based on this study,RLS can be used for the determination of CMC-Na in the samples.
引文
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