磺丁基醚-β-环糊精单一取代组分的分离纯化及取代度的测定
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摘要
目的:建立磺丁基醚-β-环糊精(SBE7-β-CD)单一取代组分分离、纯化及取代度测定的方法。方法:采用DEAE Sephadex A-25柱进行分离,得到单一取代组分。采用Sephadex G-25柱层析对单一取代组分进行脱盐纯化。分别采用核磁共振氢谱(~1H-NMR)和质谱(MS)法测定各单取代组分的取代度。结果:共得到6种单取代组分,其取代度依次为3,4,5,6,7,8。~1H-NMR和MS所测结果一致。结论:本试验成功分离、纯化了6种SBE_7-β-CD的单取代组分,为SBE_7-β-CD的质量控制奠定了基础。
Objective: To establish a method for separation,purification and determination of substitution degree of the mono-substitution ingredients in sulfobutyl ether-β-cyclodextrin (SBE_7-β-CD). Methods: The SBE_7-β-CD mixture was fractionated by DEAE Sephadex A-25,and then the mono-substitution ingredients in SBE7-β-CD were desalted by Sephadex G-25. The substitution degree of each mono-substitution ingredient was determined by ~1H nuclear magnetic resonance(~1H-NMR) and mass spectrography (MS). Results: Totally 6 mono-substitution ingredients of SBE_7-β-CD were obtained with the substitution degree of 3,4,5,6,7 and 8,respectively. The results of substitution degree from ~1H-NMR were agreed with those from MS. Conclusion: The experiment isolated and purified 6 mono-substitution ingredients in SBE_7-β-CD,which establishes basis for the feature description of SBE_7-β-CD.
Objective: To establish a method for separation,purification and determination of substitution degree of the mono-substitution ingredients in sulfobutyl ether-β-cyclodextrin (SBE_7-β-CD). Methods: The SBE_7-β-CD mixture was fractionated by DEAE Sephadex A-25,and then the mono-substitution ingredients in SBE7-β-CD were desalted by Sephadex G-25. The substitution degree of each mono-substitution ingredient was determined by ~1H nuclear magnetic resonance(~1H-NMR) and mass spectrography (MS). Results: Totally 6 mono-substitution ingredients of SBE_7-β-CD were obtained with the substitution degree of 3,4,5,6,7 and 8,respectively. The results of substitution degree from ~1H-NMR were agreed with those from MS. Conclusion: The experiment isolated and purified 6 mono-substitution ingredients in SBE_7-β-CD,which establishes basis for the feature description of SBE_7-β-CD.
引文
1曹雅培,王静,曹德英.药用辅料磺丁基醚-β-环糊精在不同制剂中的应用进展[J].中国药房,2012,23(1):79-82
2胡裕迪,赵雁,陶涛.磺丁基醚-β-环糊精的增溶机制及在难溶性药物制剂中的应用[J].中国医药工业出版社,2018,49(3):292-300
3谢佳蓉,涂家生,孙春萌.盐酸非索非那定磺丁基醚-β-环糊精包合物鼻用温敏凝胶的制备及黏附效果评价[J].中国药房,2016,27(28):3961-3963
4冯彩霞,修宪,田伟,等.伏立康唑磺丁基醚-β-环糊精包合物制备工艺优化[J].中国医院药学杂志,2017,37(15):1431-1434
5邓凤,贾运涛,田睿,等.染料木素磺丁基醚-β-环糊精包合物的研制[J].中国医院药学杂志,2015,35(18):1646-1650
6蒋娟,陈萌萌,王淼,等.泊沙康唑-磺丁基-β-环糊精包合物的制备[J].沈阳药科大学学报,2016,33(7):519-524
7孙宏晟,王建华.甲氧苄啶-磺丁基醚-β-环糊精包合物的制备、表征及分子模拟[J].中国医院药学杂志,2017,52(13):1159-1166
8李英杰,王宁,高立娣,等.磺丁基-β-环糊精氧化锆复合材料电色谱整体柱的制备及应用[J].分析试验室,2016,35(12):1428-1431
9杨学敏,杨波,廖霞俐,等.不同取代度磺丁基醚-β-环糊精的合成工艺研究[J].化学世界,2013,54(2):110-113
10李闻新,周娜,律涛,等.LC-MS/MS法测定药用辅料磺丁基醚-β-环糊精中2个杂质[J].药物分析杂志,2018,38(3):495-499
11李闻新,周娜,律涛,等.LC-MS/MS法测定药用辅料磺丁基醚-β-环糊精中2个杂质[J].药物分析杂志,2018,38(3):495-499
12李闻新,新型药用辅料磺丁基醚-β-环糊精的质量控制方法研究[D].石家庄:河北医科大学硕士学位论文,2013
13姜锡娟,李闻新,杜玉民,等.磺丁基醚-β-环糊精的高效毛细管电泳-间接UV法分析[J].中国医药工业杂志,2012,43(3):201-203
14 Grard S,Elfakir C,Dreux M.Sulfobutyl Ether-β-Cyclodextrin Fingerprint Using Ion Pair Reversed-Phase Chromatography[J].Chromatographia,1999,50(11/12):695-700
15 Grard S,Elfakir C,Dreux M.Analysis of sulfobutyl ether-β-cyclodextrin mixtures by ion-spray mass spectrometry and liquid chromatography-ion-spray mass spectrometry[J].J Chromatogr A,2001,925(1-2):79-87
16 Grard S,Elfakir C,Dreux M.Characterization of sulfobutyl ether-bcyclodextrins mixtures by anion-exchange chromatography using evaporative light scattering detection[J].J Chromatogr A,2000,897(1-2):185-193
17 Luna EA,Bormancini ER,Thompson DO,et al.Fractionation and characterization of 4-sulfobutyl ether derivatives of cyclomaltoheptaose(β-cyclodextrin)[J].Carbohydr Res,1997,299(3):103-110
18刘春东.磺丁基醚-β-环糊精的制备及其对阿奇霉素包合作用研究[D].重庆:重庆大学硕士学位论文,2007
19张玎玎.中国水处理化学品现状及发展趋势[J].精细与专用化学品,2014,22(7):7-10
20王晓飞,李辉,刘铭佩,等.油橄榄叶中三萜类成分的提取、分离与结构鉴定[J].中国药房,2017,28(19):2639-2641
21王贵金,杜红娜,乔莉,等.人参醇提后药渣中人参酸性多糖的分离纯化工艺研究[J].中国药房,2016,27(28):3957-3960
22陈军,钟新林,余彦海.离子色谱法测定减肥食品中左旋肉碱[J].理化检验(化学分册),2013,49(1):6-10
23余晖,孙聪聪,焦少俊,等.废酸的综合治理与资源化研究进展[J].环境监测管理与技术,2018,(2):5-10
2胡裕迪,赵雁,陶涛.磺丁基醚-β-环糊精的增溶机制及在难溶性药物制剂中的应用[J].中国医药工业出版社,2018,49(3):292-300
3谢佳蓉,涂家生,孙春萌.盐酸非索非那定磺丁基醚-β-环糊精包合物鼻用温敏凝胶的制备及黏附效果评价[J].中国药房,2016,27(28):3961-3963
4冯彩霞,修宪,田伟,等.伏立康唑磺丁基醚-β-环糊精包合物制备工艺优化[J].中国医院药学杂志,2017,37(15):1431-1434
5邓凤,贾运涛,田睿,等.染料木素磺丁基醚-β-环糊精包合物的研制[J].中国医院药学杂志,2015,35(18):1646-1650
6蒋娟,陈萌萌,王淼,等.泊沙康唑-磺丁基-β-环糊精包合物的制备[J].沈阳药科大学学报,2016,33(7):519-524
7孙宏晟,王建华.甲氧苄啶-磺丁基醚-β-环糊精包合物的制备、表征及分子模拟[J].中国医院药学杂志,2017,52(13):1159-1166
8李英杰,王宁,高立娣,等.磺丁基-β-环糊精氧化锆复合材料电色谱整体柱的制备及应用[J].分析试验室,2016,35(12):1428-1431
9杨学敏,杨波,廖霞俐,等.不同取代度磺丁基醚-β-环糊精的合成工艺研究[J].化学世界,2013,54(2):110-113
10李闻新,周娜,律涛,等.LC-MS/MS法测定药用辅料磺丁基醚-β-环糊精中2个杂质[J].药物分析杂志,2018,38(3):495-499
11李闻新,周娜,律涛,等.LC-MS/MS法测定药用辅料磺丁基醚-β-环糊精中2个杂质[J].药物分析杂志,2018,38(3):495-499
12李闻新,新型药用辅料磺丁基醚-β-环糊精的质量控制方法研究[D].石家庄:河北医科大学硕士学位论文,2013
13姜锡娟,李闻新,杜玉民,等.磺丁基醚-β-环糊精的高效毛细管电泳-间接UV法分析[J].中国医药工业杂志,2012,43(3):201-203
14 Grard S,Elfakir C,Dreux M.Sulfobutyl Ether-β-Cyclodextrin Fingerprint Using Ion Pair Reversed-Phase Chromatography[J].Chromatographia,1999,50(11/12):695-700
15 Grard S,Elfakir C,Dreux M.Analysis of sulfobutyl ether-β-cyclodextrin mixtures by ion-spray mass spectrometry and liquid chromatography-ion-spray mass spectrometry[J].J Chromatogr A,2001,925(1-2):79-87
16 Grard S,Elfakir C,Dreux M.Characterization of sulfobutyl ether-bcyclodextrins mixtures by anion-exchange chromatography using evaporative light scattering detection[J].J Chromatogr A,2000,897(1-2):185-193
17 Luna EA,Bormancini ER,Thompson DO,et al.Fractionation and characterization of 4-sulfobutyl ether derivatives of cyclomaltoheptaose(β-cyclodextrin)[J].Carbohydr Res,1997,299(3):103-110
18刘春东.磺丁基醚-β-环糊精的制备及其对阿奇霉素包合作用研究[D].重庆:重庆大学硕士学位论文,2007
19张玎玎.中国水处理化学品现状及发展趋势[J].精细与专用化学品,2014,22(7):7-10
20王晓飞,李辉,刘铭佩,等.油橄榄叶中三萜类成分的提取、分离与结构鉴定[J].中国药房,2017,28(19):2639-2641
21王贵金,杜红娜,乔莉,等.人参醇提后药渣中人参酸性多糖的分离纯化工艺研究[J].中国药房,2016,27(28):3957-3960
22陈军,钟新林,余彦海.离子色谱法测定减肥食品中左旋肉碱[J].理化检验(化学分册),2013,49(1):6-10
23余晖,孙聪聪,焦少俊,等.废酸的综合治理与资源化研究进展[J].环境监测管理与技术,2018,(2):5-10