二甲硅油分子交联的表征研究
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摘要
目的:对药用辅料二甲硅油的结构进行解析表征。方法:采用超高效液相-高分辨质谱联用方法检测,基于高分辨质谱提供的分子离子峰和碎片信息对二甲硅油的结构进行解析。利用MassHunter质谱工作站及数据分析功能对二甲硅油20、50、100、200、350、500、750、1000、12500和30000系列型号样品进行分析表征。结果:二甲硅油按照黏度不同可以分为不同的型号,随着型号的增加,黏度不断增大,通过对二甲硅油分子结构的解析发现,二甲硅油的结构中存在分子交联的现象,其分子交联的比例与其黏度成正相关。结论:二甲硅油的黏度是其重要的功能性指标,二甲硅油的黏度不仅与其聚合度有关,还与其分子交联的比例有关。
Objective: To analytically characterize the structure of pharmaceutical excipient Dimethicone.Methods: UHPLC-HRMS detection was used to analyze the structure of Dimethicone based on molecular ion peak and fragment information provided by high resolution mass spectrometry. Samples of Dimethicone 20, 50,100, 200, 350, 500, 750, 1000, 12500 and 30000 series numbers were analyzed and characterized by using the data analysis functions of MassHunter mass spectrometer. Results: Dimethicone could be classified into different types according to its viscosity. With the increase of the models, the viscosity increases continuously. There was phenomenon of molecular crosslinking in the structure of Dimethicone according to the analysis of the molecular structure of dimethicone. And the proportion of molecular crosslinking was positively correlated with its viscosity.Conclusion: The viscosity of Dimethicone is an important functionality-related characteristic. The viscosity of Dimethicone is related not only to its degree of polymerization, but also to the proportion of molecule crosslinking.
Objective: To analytically characterize the structure of pharmaceutical excipient Dimethicone.Methods: UHPLC-HRMS detection was used to analyze the structure of Dimethicone based on molecular ion peak and fragment information provided by high resolution mass spectrometry. Samples of Dimethicone 20, 50,100, 200, 350, 500, 750, 1000, 12500 and 30000 series numbers were analyzed and characterized by using the data analysis functions of MassHunter mass spectrometer. Results: Dimethicone could be classified into different types according to its viscosity. With the increase of the models, the viscosity increases continuously. There was phenomenon of molecular crosslinking in the structure of Dimethicone according to the analysis of the molecular structure of dimethicone. And the proportion of molecular crosslinking was positively correlated with its viscosity.Conclusion: The viscosity of Dimethicone is an important functionality-related characteristic. The viscosity of Dimethicone is related not only to its degree of polymerization, but also to the proportion of molecule crosslinking.
引文
[1]中华人民共和国药典:四部[S].2015:453-454.
[2]R.C.罗,P.J.舍斯基,P.J.韦勒.药用辅料手册[M].北京:化学工业出版社,2005.
[3]杨婉花,张芳华.红外光谱法测定硅酮二号凝胶中二甲硅油的含量[J].中国药师,2010,13(21):1621-1622.
[4]于宏伟,解立斌,白良魁,等.硅氧树脂变温傅里叶变换衰减全反射红外光谱研究[J].精细石油化工进展,2015,16(4):54-57.
[5]严拯宇,艾小霞,唐璐,等.红外分光光度法测定二甲硅油含量[J].中南药学,2015,13(2):180-187.
[6]C Laugel,P Rafidison,G Potard,et al.Modulated Release of Triterpenic Compounds from a O/W/O Multiple Emulsion Formulated with Dimethicones:Infrared Spectrophotometric and Differential Calorimetric Approaches[J].Journal of Controlled Release,2000,63(1-2):7-10.
[7]江秋迟,胡磊,胡建国.红外分光光度法测定硅酮二号凝胶中二甲硅油含量[J].药学实践杂志,2011,29(3):212-215
[8]杨婉花,张芳华.红外光谱法测定硅酮二号凝胶中二甲硅油含量[J].中国药师,2010,13(11):1621-1622.
[9]冯光.红外分光光度法测定二甲硅油片中二甲硅油的含量[J].药物分析杂志,2013,33(9):1621-1623.
[10]田翠翠,罗永煌,张贺,等.IR测定复方枸橼酸阿尔维林软胶囊中的西甲硅油[J].光谱实验室,2012,29(1):443-448.
[11]徐新元,陈祝康,刘倩,等.傅里叶红外测定西甲硅油滴剂中二甲硅油的含量[J].药物分析杂志,1999,19(2):126-127.
[12]张庆,张广明,刘孟妮,等.二甲硅油乳剂中二甲硅油含量测定[J].中国保健营养,2015,9(11):272-273.
[13]廉慧锋,赵笑天,王蓉珍,等.超高效液相色谱-串联质谱法同时测定玉米、花生、麦仁中的九种真菌毒素[J].食品科学,2010,20(31):360-366.
[14]陈明,王昌尧,朱剑华,等.强酸性阳离子交换树脂催化合成二甲基硅油的研究[J].有机硅材料,2013,27(1):25-28.
[15]杜斌,陈海平,徐海露,等.药用级二甲基硅油的合成研究[J].有机硅材料,2018,32(2):128-131.
[2]R.C.罗,P.J.舍斯基,P.J.韦勒.药用辅料手册[M].北京:化学工业出版社,2005.
[3]杨婉花,张芳华.红外光谱法测定硅酮二号凝胶中二甲硅油的含量[J].中国药师,2010,13(21):1621-1622.
[4]于宏伟,解立斌,白良魁,等.硅氧树脂变温傅里叶变换衰减全反射红外光谱研究[J].精细石油化工进展,2015,16(4):54-57.
[5]严拯宇,艾小霞,唐璐,等.红外分光光度法测定二甲硅油含量[J].中南药学,2015,13(2):180-187.
[6]C Laugel,P Rafidison,G Potard,et al.Modulated Release of Triterpenic Compounds from a O/W/O Multiple Emulsion Formulated with Dimethicones:Infrared Spectrophotometric and Differential Calorimetric Approaches[J].Journal of Controlled Release,2000,63(1-2):7-10.
[7]江秋迟,胡磊,胡建国.红外分光光度法测定硅酮二号凝胶中二甲硅油含量[J].药学实践杂志,2011,29(3):212-215
[8]杨婉花,张芳华.红外光谱法测定硅酮二号凝胶中二甲硅油含量[J].中国药师,2010,13(11):1621-1622.
[9]冯光.红外分光光度法测定二甲硅油片中二甲硅油的含量[J].药物分析杂志,2013,33(9):1621-1623.
[10]田翠翠,罗永煌,张贺,等.IR测定复方枸橼酸阿尔维林软胶囊中的西甲硅油[J].光谱实验室,2012,29(1):443-448.
[11]徐新元,陈祝康,刘倩,等.傅里叶红外测定西甲硅油滴剂中二甲硅油的含量[J].药物分析杂志,1999,19(2):126-127.
[12]张庆,张广明,刘孟妮,等.二甲硅油乳剂中二甲硅油含量测定[J].中国保健营养,2015,9(11):272-273.
[13]廉慧锋,赵笑天,王蓉珍,等.超高效液相色谱-串联质谱法同时测定玉米、花生、麦仁中的九种真菌毒素[J].食品科学,2010,20(31):360-366.
[14]陈明,王昌尧,朱剑华,等.强酸性阳离子交换树脂催化合成二甲基硅油的研究[J].有机硅材料,2013,27(1):25-28.
[15]杜斌,陈海平,徐海露,等.药用级二甲基硅油的合成研究[J].有机硅材料,2018,32(2):128-131.