Box-Behnken响应面法优化有机硅季铵盐包合物的制备工艺
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摘要
目的研究优化有机硅季铵盐(SQ-5700)-羟丙基-β-环糊精(HP-β-CD)包合物(SQ5700-HP-β-CD包合物)的最佳制备工艺。方法采用溶液-搅拌法包合SQ-5700,采用双向滴定法测定SQ-5700的质量分数,以包封率为评价指标,采用Box-Behnken响应面法考察壁芯比(HP-β-CD∶SQ-5700,质量比)、搅拌时间、包合温度对包合物包封率的影响,对结果进行多元线性和二项式拟合,优选SQ5700-HP-β-CD包合物最佳制备工艺;采用差示扫描量热法(DSC)和红外光谱分析(FTIR)对SQ-5700、HP-β-CD、SQ5700-HP-β-CD包合物、SQ5700与HP-β-CD的物理混合物进行鉴别。结果最佳制备工艺条件:包合温度42℃、壁芯比2.4∶1、搅拌时间31 min,SQ5700-HP-β-CD包合物的包封率为93.66%,与理论值偏差小于5%。结论经Box-Behnken响应面法优选工艺制备的SQ5700-HP-β-CD包合物,理化性质稳定,各项指标与理论值较好的吻合,模型选用合理有效,包合后可提高SQ5700在水中的稳定性。
Objective To optimize the best preparation technology of organosilicon quaternary ammonium salt(SQ5700) inclusion complex. Methods Organosilicon quaternary ammonium salt inclusion complex was prepared by solution agitation method. The content of SQ-5700 was determined by bidirectional titration. The effects of influence factors,such as ingredient proportion,inclusion time,inclusion temperature on inclusion rate,obtaining rate,and overall desirability were investigated by using Box-Behnken response surface methodology. The data were imitated by using multi-linear equation and second-order polyno-mial equation. SQ-5700,HP-β-CD,SQ5700-HP-β-CD inclusion complex,and physical mixture of SQ5700 and HP-β-CD were verified by DSC and FTIR. Results The optimal processing parameters were as follows: the inclusion temperature was 42 ℃;Hydroxypropyl-β-cyclodextrin∶SQ5700 was 2.4∶1,mixing time was 31 min. Base on the optimal parameters,the entrapment of SQ5700-HP-β-CD inclusion complex was 93.66%. The deviation of the measured values from the predicted ones was less than 5%. Conclusion The optimized SQ5700-HP-β-CD inclusion complex by Box-Behnken response surface methodology is stable in physical and chemical properties. The indexes are in good agreement with the predicted values. The model is reasonable and effective,and the stability of SQ5700 in water can be improved after inclusion.
Objective To optimize the best preparation technology of organosilicon quaternary ammonium salt(SQ5700) inclusion complex. Methods Organosilicon quaternary ammonium salt inclusion complex was prepared by solution agitation method. The content of SQ-5700 was determined by bidirectional titration. The effects of influence factors,such as ingredient proportion,inclusion time,inclusion temperature on inclusion rate,obtaining rate,and overall desirability were investigated by using Box-Behnken response surface methodology. The data were imitated by using multi-linear equation and second-order polyno-mial equation. SQ-5700,HP-β-CD,SQ5700-HP-β-CD inclusion complex,and physical mixture of SQ5700 and HP-β-CD were verified by DSC and FTIR. Results The optimal processing parameters were as follows: the inclusion temperature was 42 ℃;Hydroxypropyl-β-cyclodextrin∶SQ5700 was 2.4∶1,mixing time was 31 min. Base on the optimal parameters,the entrapment of SQ5700-HP-β-CD inclusion complex was 93.66%. The deviation of the measured values from the predicted ones was less than 5%. Conclusion The optimized SQ5700-HP-β-CD inclusion complex by Box-Behnken response surface methodology is stable in physical and chemical properties. The indexes are in good agreement with the predicted values. The model is reasonable and effective,and the stability of SQ5700 in water can be improved after inclusion.
引文
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[2] 河合博.道康宁5700抗微生物处理剂[J].印染,1996,8(3):38-42.
[3] 王冰.复合型季铵盐类抗菌剂的抑菌效果[D].大连:大连工业大学,2014.
[4] 黄良仙,肖波,杨军胜,等.有机硅季铵盐的合成及其在织物整理中的应用研究进展[J].印染助剂,2013,30(10):1-6.
[5] 于美宁.一种有机硅季铵盐及其抗菌剂制备方法:201610055614.9[P].2016-06-08.
[6] 陶涛.羟丙基倍他环糊精的特性及其药剂学应用[J].中国医药工业杂志,2002(6):46-50.
[7] 孙家艳,庞芳苹,刘墨祥.羟丙基-β-环糊精在天然药物中的应用研究进展[J].中成药,2015,37(2):388-391.
[8] 邹国省,关浩彬,秦凌浩.Box-Behnken响应面设计法优化替硝唑环糊精包合物的制备工艺[J].广东药学院学报,2009,25(5):444-448.
[9] 伍永富,吴品江,魏萍,等.Box-Behnken设计-效应面法优化木犀草素-β-环糊精包合物的制备工艺研究[J].中草药,2010,41(7):1094-1099.
[10] 张光杰,王聪,袁超,等.响应面法优化八角茴香精油羟丙基-β-环糊精包合物制备工艺[J].中国食品添加剂,2017,30(8):135-141.
[11] 王璐璐,郑稳生,陈少华,等.棓丙酯-羟丙基-β-环糊精包合物的研制[J].中国新药杂志2013,22(11):1337-1340.
[12] 贾丽丽.季铵盐的快速测定与杀菌凝胶剂的研究[D].北京:中国人民解放军军事医学科学院,2008.
[13] SZENTE L,SZEJTLI J.Cyclodextrins as food ingredients[J].Trends Food Sci Tech,2004,15(3/4):137-142.
[14] 郑雯,王远,袁田青,等.响应面试验优化羟丙基-β-环糊精包合植物甾醇的水溶性改性工艺[J].食品科学,2017,38(20):161-168.
[15] LOFTSSON T,BREWSTER M E.effects on drug permeation through biological membranes[J].JPP,2011,63(9):1119-1135.
[16] 郑欣,刘新,欧阳雪,李美燕.尼古丁羟丙基-β-环糊精包合物的制备及稳定性考察[J].中国医院药学杂志,2015,35(12):1138-1141.
[17] 何瑶,徐晓玉,陈红,等.卡前列甲酯-羟丙基-β-环糊精包合物的制备和评价[J].中国新药杂志,2018,27(6):637-643.