当归润肠膏的制备工艺和质量标准
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摘要
本文对当归润肠膏的制备工艺和质量标准进行了研究,并考察其稳定性,为贮藏条件和保质期制定提供理论参考。采用正交试验L_9(3~4)优选最佳提取工艺;用薄层层析和高效液相色谱法对当归润肠膏的主要成分进行了定性鉴别和定量分析;采用单因素实验及经典恒温加速试验考察稳定性,预测其有效期。当归润肠膏的最佳提取工艺:加入10倍处方量药材的水(w/v)浸泡1.25 h,回流提取2 h,趁热过滤;滤渣中再加8倍水量(w/v),再回流提取1.5 h;合并滤液。按此操作平行制备3批样品,其出膏得率、浸出物含量分别为64.24%±0.99%、21.43%±0.68%,多糖、阿魏酸含量分别为(7.78±0.03)、(4.05±0.24) mg/mL。将滤液浓缩至相对密度为1.207±0.008(70℃)的清膏,加入1倍清膏量的炼蜜(w/w)得到煎膏剂。在薄层层析谱图中可检出当归、大枣、干姜和枳壳的特征斑点,煎膏剂中阿魏酸的含量为(102.7±4.4)μg/g。经强光照射(20℃、4500 lx)和高温储存(避光、60℃)10 d后,阿魏酸的含量均显著降低。未添加稳定剂的当归润肠膏预测保质期约3个月,加入0.4%的NaHSO_3、0.1%的EDTA-2Na作为稳定剂后,其预测保质期延长至1.68年,比未添加稳定剂的样品保质期延长了8倍。当归润肠膏的制备方法简单可行,质量相对稳定可控。
In this article,the preparation process and quality standards of DangguiRunchang paste(DRP)were studied,and its stability was also investigated to provide theoretical reference for storage conditions and shelf life. Orthogonal test L_9(3~4)was used to optimize the extraction process. The main components of DRP were qualitatively identified and quantitatively analyzed by Thin-layer Chromatography(TLC)and High Performance Liquid Chromatography(HPLC)method. The single factor test and the classical constant temperature accelerated test were used to investigate the stability and predict the shelf life. The optimal extraction conditions were:raw herbal materials were soaked with 10 times the amount of water(w/v)for 1.25 h,refluxed for 2 h,filtered while the extract was hot. The solid residue was extracted with 8 times the amount of water(w/v)again for 1.5 h. According to the above-mentioned method,3 batches of samples were prepared in parallel and the yield and extractive content of the extracts were 64.24%±0.99% and 21.43%±0.68%,respectively. The polysaccharide and ferulic acid contents were(7.78±0.03)and(4.05±0.24) mg/mL,respectively. The filtrates were combined and concentrated to the relative density of 1.207±0.008(70 ℃). The equal amount of refined honey(w/w)was added,mixed well to obtain the final preparation. The marker components of Radix Angelicae Sinensis,Zingibeais Rhizoma,Aurantii Frucrus and Jujubae Fructus were identified using TLC analyses. The content of ferulic acid in the DRP was(102.7±4.4) μg/g. After 10 days of exposure to strong light(20 ℃,4500 xl)and high temperature storage(protection from light,60 ℃),the content of ferulic acid significantly reduced. The DRP without stabilizers had a shelf life about 3 mouths. After added 0.4% NaHSO_3 and 0.1% EDTA-2 Na as stabilizers,its shelf life was extended to about 1.68 years,which was 8 times longer than that of the sample without stabilizers. The preparation technology of DRP was simple and feasible. The quality was relatively stable and controllable.
In this article,the preparation process and quality standards of DangguiRunchang paste(DRP)were studied,and its stability was also investigated to provide theoretical reference for storage conditions and shelf life. Orthogonal test L_9(3~4)was used to optimize the extraction process. The main components of DRP were qualitatively identified and quantitatively analyzed by Thin-layer Chromatography(TLC)and High Performance Liquid Chromatography(HPLC)method. The single factor test and the classical constant temperature accelerated test were used to investigate the stability and predict the shelf life. The optimal extraction conditions were:raw herbal materials were soaked with 10 times the amount of water(w/v)for 1.25 h,refluxed for 2 h,filtered while the extract was hot. The solid residue was extracted with 8 times the amount of water(w/v)again for 1.5 h. According to the above-mentioned method,3 batches of samples were prepared in parallel and the yield and extractive content of the extracts were 64.24%±0.99% and 21.43%±0.68%,respectively. The polysaccharide and ferulic acid contents were(7.78±0.03)and(4.05±0.24) mg/mL,respectively. The filtrates were combined and concentrated to the relative density of 1.207±0.008(70 ℃). The equal amount of refined honey(w/w)was added,mixed well to obtain the final preparation. The marker components of Radix Angelicae Sinensis,Zingibeais Rhizoma,Aurantii Frucrus and Jujubae Fructus were identified using TLC analyses. The content of ferulic acid in the DRP was(102.7±4.4) μg/g. After 10 days of exposure to strong light(20 ℃,4500 xl)and high temperature storage(protection from light,60 ℃),the content of ferulic acid significantly reduced. The DRP without stabilizers had a shelf life about 3 mouths. After added 0.4% NaHSO_3 and 0.1% EDTA-2 Na as stabilizers,its shelf life was extended to about 1.68 years,which was 8 times longer than that of the sample without stabilizers. The preparation technology of DRP was simple and feasible. The quality was relatively stable and controllable.
引文
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[21]张延华,朱永红,蒋晔.光线对复方当归注射液中阿魏酸稳定性的影响[J].武警医学院学报,2009,18(9):748-750.
[2]段士化,王伟明.浅述慢性便秘的中医治疗[J].黑龙江中医药,2013(4):35.
[3]叶飞,王巧民.慢性便秘的流行病学研究进展[J].中国临床保健杂志,2010,13(6):665-667.
[4]丁义江,丁曙晴.慢性功能性便秘的中医诊治策略.中国临床医生杂志,2007,35(3):18-19.
[5]于普林,李增金,郑宏,等.老年人便秘流行病学特点的初步分析[J].中华老年医学杂志,2001,20(2):132-134.
[6]筱君,李金合,张义.便秘的中西药物治疗现状[J].中国肛肠病杂志,2016,36(3):65-66.
[7]徐昊.浅述中药煎膏剂[J].河南中医,2012,32(1):60-61.
[8]曹永仓,梁晓东,陈涛,等.近十多年来中药当归配伍的文献研究[J].中国医院药学杂志,2016,36(3):161-163,209.
[9]赵林钢,姚毅,祁乃喜,等.补心益气煎膏生产工艺研究[J].江苏中医药,2016(12):67-69.
[10]袁诗俊,龚梦瑀,李梦林,等.大黄中抗氧化物质的提取工艺优化[J].食品工业科技,2018,39(19):147-149,155.
[11]任朝辉,冯国辉,张传博,等.姬松茸深层发酵多糖提取工艺优化及抗氧化活性[J].食品工业科技,2017,38(14):216-222.
[12]李宏妍.防己茯苓汤煎膏剂的制备工艺与质量标准研究[D].黑龙江中医药大学,2011.
[13]商澎,杨铁虹,贾敏,等.当归多糖AP-Ⅰ的提取、分析鉴定及抗肿瘤活性研究[J].西北药学杂志,2000(z1):80-81.
[14]张清勇,于宏,王庆奎,等.当归多糖的提取、分离及纯化[J].河北渔业,2016(3):1-3.
[15]王丹梅,付强,刘喜明,等.HPLC法测定复方保健品中阿魏酸的含量[J].食品工业科技,2009,30(7):320-321.
[16]国家药典委员会.中华人民共和国药典(四部)[S].2015年版,北京:中国医药科技出版社,2015.
[17]刘勐,史彦斌,管玉珠.氢溴酸高乌甲素注射液及冻干粉的稳定性[J].中国医院药学杂志,2010,30(2):111-113.
[18]陈丛英,陈菲,盛柳青.佛手油包合物凝胶的制备及其t0.9预测[J].中国医院药学杂志,2010,30(24):2127-2129.
[19]Ling FANG,Xue-feng XIAO,Chang-xiao LIU,et al.Recent advance in studies on angelica sinensis[J].Chinese Herbal Medicines,2012,4(1):12-25.
[20]张中华.HPLC法同时测定丹参当归复方制剂中丹酚酸B和阿魏酸的含量[J].实用医药杂志,2011,28(11):995-998.
[21]张延华,朱永红,蒋晔.光线对复方当归注射液中阿魏酸稳定性的影响[J].武警医学院学报,2009,18(9):748-750.