由于某种原因，我要用葡聚糖凝胶柱层析来分离无机盐和环糊精，我用自动部分收集器收集，想绘制一个分离图谱，无机盐氯化钠我用硝酸银定量加550nm透光率法，环糊精我想用紫外末端吸收法，但是环糊精的紫外扫描图谱显示其末端吸收也不是很强，这样灵敏度太低。
请问还有什么别的方法来基本定量测定环糊精？
或者怎样显色环糊精然后紫外定量？
！～～
上HPLC。
Assay
Examine by liquid chromatography (2.2.29).
Test solution (a)
Dissolve 0.25 g of the substance to be examined in water R with heating, cool and dilute to 25.0 ml with the same solvent.
Test solution (b)
Dilute 5.0 ml of test solution (a) to 50.0 ml with water R.
Reference solution (a)
Dissolve 25.0 mg of alfadex CRS, 25.0 mg of gammacyclodextrin CRS and 50.0 mg of betadex CRS in water R and dilute to 50.0 ml with the same solvent.
Reference solution (b)
Dilute 5.0 ml of reference solution (a) to 50.0 ml with water R.
Reference solution (c)
Dissolve 25.0 mg of betadex CRS in water R and dilute to 25.0 ml with the same solvent.
The chromatographic procedure may be carried out using:
a stainless steel column 0.25 m long and 4.6 mm in internal diameter packed with octadecylsilyl silica gel for chromatography R (10 mm),
as mobile phase at a flow rate of 1.5 ml/min a mixture of 10 volumes of methanol R and 90 volumes of water R,
as detector a differential refractometer,
a 50 ml loop injector.
Equilibrate the column with the mobile phase at a flow rate of 1.5 ml/min for about 3 h. Inject each solution. Record the chromatograms for 1.5 times the retention time of betadex. Adjust the sensitivity of the detector so that the height of the peak corresponding to gammacyclodextrin, in the chromatogram obtained with reference solution (a), is 55 per cent to 75 per cent of the full scale of the recorder. The retention time of betadex is about 10 min, the relative retention time of gammacyclodextrin is about 0.3 and that of alfadex is about 0.45. The test is not valid unless the resolution between the peaks corresponding to gammacyclodextrin and alfadex is not less than 1.5, and the relative standard deviation of the area of the peak corresponding to betadex is less than 2.0 per cent. If necessary, adjust the concentration of methanol in the mobile phase to achieve the required resolution. Calculate the percentage content of 7 from the area of the principal peak in each of the chromatograms obtained with test solution (b) and reference solution (c) and the declared content of betadex CRS.
！～～
differential refractometer
这个东西我没有啊
不知道有没有环糊精 （没有还原端的的葡萄糖聚合物）的显色反应，这样用紫外比较方便和快捷
不过您的回答提醒了我，我查下各国药典先
没有示差折光检测器要搞糖类化合物就很麻烦了，可以查查衍生化以后用UV测的方法。
显色反应估计是没戏，除非浓度足够高。
实在不行还有NMR，就是贵，不合算。
没有示差折光检测器要搞糖类化合物就很麻烦了，可以查查衍生化以后用UV测的方法。
显色反应估计是没戏，除非浓度足够高。
实在不行还有NMR，就是贵，不合算。
看了N多文献后，找到了一个用于cyclodextrin的间接紫外法
原理是一些紫外吸收物质在被环糊精包合后其紫外波谱会发生红移，可以以只含紫外吸收物质的为Blank，以含与背景同样浓度紫外吸收物质的环糊精样品溶液为Sample，则紫外响应A(Sample)-A(Blank)即对应环糊精浓度。
此间接紫外法（indirect UV photometric detection）可用于紫外分析，HPLC，毛细管电泳等，其检测限也比较理想。
下图为毛细管电泳图，流动相中含一定浓度的可被环糊精包合红移的紫外吸收物质。
欢迎高手讨论使环糊精可以用紫外检测的其他的手段
江苏金湖县绿洲医药辅料有限公司致力于环糊精及其衍生物的研究与生产，并为客户提供环糊精系列产品在医药、食品、日化、纺织等领域的应用技术。
我们为您提供的2-羟丙基-β-环糊精质量符合欧洲药典（第四版增补版），已得到国内外客户的广泛认可。我们的科研步伐始终与世界同步，确保为您提供高品质的产品与细致的文献和技术服务。
网址:www.cyclochem.cn
email:cyclochem@126.com
tel:0512-57037155
qq:813376275
请问还有什么别的方法来基本定量测定环糊精？
或者怎样显色环糊精然后紫外定量？
！～～
上HPLC。
Assay
Examine by liquid chromatography (2.2.29).
Test solution (a)
Dissolve 0.25 g of the substance to be examined in water R with heating, cool and dilute to 25.0 ml with the same solvent.
Test solution (b)
Dilute 5.0 ml of test solution (a) to 50.0 ml with water R.
Reference solution (a)
Dissolve 25.0 mg of alfadex CRS, 25.0 mg of gammacyclodextrin CRS and 50.0 mg of betadex CRS in water R and dilute to 50.0 ml with the same solvent.
Reference solution (b)
Dilute 5.0 ml of reference solution (a) to 50.0 ml with water R.
Reference solution (c)
Dissolve 25.0 mg of betadex CRS in water R and dilute to 25.0 ml with the same solvent.
The chromatographic procedure may be carried out using:
a stainless steel column 0.25 m long and 4.6 mm in internal diameter packed with octadecylsilyl silica gel for chromatography R (10 mm),
as mobile phase at a flow rate of 1.5 ml/min a mixture of 10 volumes of methanol R and 90 volumes of water R,
as detector a differential refractometer,
a 50 ml loop injector.
Equilibrate the column with the mobile phase at a flow rate of 1.5 ml/min for about 3 h. Inject each solution. Record the chromatograms for 1.5 times the retention time of betadex. Adjust the sensitivity of the detector so that the height of the peak corresponding to gammacyclodextrin, in the chromatogram obtained with reference solution (a), is 55 per cent to 75 per cent of the full scale of the recorder. The retention time of betadex is about 10 min, the relative retention time of gammacyclodextrin is about 0.3 and that of alfadex is about 0.45. The test is not valid unless the resolution between the peaks corresponding to gammacyclodextrin and alfadex is not less than 1.5, and the relative standard deviation of the area of the peak corresponding to betadex is less than 2.0 per cent. If necessary, adjust the concentration of methanol in the mobile phase to achieve the required resolution. Calculate the percentage content of 7 from the area of the principal peak in each of the chromatograms obtained with test solution (b) and reference solution (c) and the declared content of betadex CRS.
！～～
differential refractometer
这个东西我没有啊
不知道有没有环糊精 （没有还原端的的葡萄糖聚合物）的显色反应，这样用紫外比较方便和快捷
不过您的回答提醒了我，我查下各国药典先
没有示差折光检测器要搞糖类化合物就很麻烦了，可以查查衍生化以后用UV测的方法。
显色反应估计是没戏，除非浓度足够高。
实在不行还有NMR，就是贵，不合算。
没有示差折光检测器要搞糖类化合物就很麻烦了，可以查查衍生化以后用UV测的方法。
显色反应估计是没戏，除非浓度足够高。
实在不行还有NMR，就是贵，不合算。
看了N多文献后，找到了一个用于cyclodextrin的间接紫外法
原理是一些紫外吸收物质在被环糊精包合后其紫外波谱会发生红移，可以以只含紫外吸收物质的为Blank，以含与背景同样浓度紫外吸收物质的环糊精样品溶液为Sample，则紫外响应A(Sample)-A(Blank)即对应环糊精浓度。
此间接紫外法（indirect UV photometric detection）可用于紫外分析，HPLC，毛细管电泳等，其检测限也比较理想。
下图为毛细管电泳图，流动相中含一定浓度的可被环糊精包合红移的紫外吸收物质。
欢迎高手讨论使环糊精可以用紫外检测的其他的手段
江苏金湖县绿洲医药辅料有限公司致力于环糊精及其衍生物的研究与生产，并为客户提供环糊精系列产品在医药、食品、日化、纺织等领域的应用技术。
我们为您提供的2-羟丙基-β-环糊精质量符合欧洲药典（第四版增补版），已得到国内外客户的广泛认可。我们的科研步伐始终与世界同步，确保为您提供高品质的产品与细致的文献和技术服务。
网址:www.cyclochem.cn
email:cyclochem@126.com
tel:0512-57037155
qq:813376275