真武汤颗粒剂制备工艺研究
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摘要
目的:优选真武汤水提液最佳提取工艺及颗粒剂制备方法,为真武汤颗粒剂的开发利用提供参考。方法:采用加热回流提取方法,通过正交试验设计考察液料比、提取时间及提取次数,以芍药苷含量、苯甲酰新乌头原碱含量和出膏率为考察指标,确定真武汤最优水提取工艺。另外选用粒度合格率、水分、干燥失重、溶化性和休止角等为考察指标,通过单因素试验优选颗粒制备中的辅料配比。结果:芍药苷和苯甲酰新乌头原碱分别在5.45~32.70μg(r=0.999 6)和3.24~16.80μg(r=0.999 7)浓度范围内线性关系良好,平均回收率分别为99.62%(RSD=1.34%,n=6)和101.72%(RSD=1.74%,n=6)。最优提取工艺为:液料比1∶12,回流提取2次,每次2 h。颗粒最佳成型工艺为:辅料采用糊精与可溶性淀粉的混合物,最佳配比1∶3,所制颗粒的粒度合格率、水分、干燥失重、溶化性和休止角分别为94.12%、4.87%、0.93%、89.23%、36.18°。结论:优化的真武汤回流提取工艺稳定、可行,制备的颗粒成型性和溶化性较好。
Objective: To optimize the extraction process of the water extract of Zhenwutang and study on the preparation of granule of Zhenwu decoction to provide reference for the development and utilization of Zhenwutang granule. Methods: Heating refluxing was used,and the effects of the ratio of solid to liquid,extraction time and times were investigated by orthogonal test. As the synthetic indices of evaluation,the yield of extraction and the contents of paeoniflorin and benzoylmesaconine measured by HPLC were determined to confirm the optimal water extraction process of Zhenwutang granule. Besides,granularity pass rate,moisture,loss on drying,solubility and angle of repose of the granule were regarded as the indices to evaluate the best ratio of the excipients in the preparation of the granule by single factor test. Results: Paeoniflorin and benzoyl mesaconitine had good linearity within the range of 5. 45-32. 70 μg( r = 0. 999 6) and 3. 24-16. 80 μg( r = 0. 999 7),respectively. The average recovery was 99. 62%( RSD = 1. 34%,n = 6) and101. 72%( RSD = 1. 74%,n = 6),respectively. The optimum extraction process was as follows: the ratio of solid to liquid was 1∶ 12 with twice refluxing extraction( 2 h for each time). The optimum granule forming process was as follows: the pharmaceutical excipients were a mixture of dextrin and soluble starch with the best ratio of 1∶ 3. The granularity pass rate,moisture,loss on drying,solubility and angle of repose of the granule was 94. 12%,4. 87%,0. 93%,89. 23% and 36. 18°,respectively. Conclusion: The optimized refluxing extraction process is stable,reliable and feasible,and the prepared granule is in good formability and melting.
Objective: To optimize the extraction process of the water extract of Zhenwutang and study on the preparation of granule of Zhenwu decoction to provide reference for the development and utilization of Zhenwutang granule. Methods: Heating refluxing was used,and the effects of the ratio of solid to liquid,extraction time and times were investigated by orthogonal test. As the synthetic indices of evaluation,the yield of extraction and the contents of paeoniflorin and benzoylmesaconine measured by HPLC were determined to confirm the optimal water extraction process of Zhenwutang granule. Besides,granularity pass rate,moisture,loss on drying,solubility and angle of repose of the granule were regarded as the indices to evaluate the best ratio of the excipients in the preparation of the granule by single factor test. Results: Paeoniflorin and benzoyl mesaconitine had good linearity within the range of 5. 45-32. 70 μg( r = 0. 999 6) and 3. 24-16. 80 μg( r = 0. 999 7),respectively. The average recovery was 99. 62%( RSD = 1. 34%,n = 6) and101. 72%( RSD = 1. 74%,n = 6),respectively. The optimum extraction process was as follows: the ratio of solid to liquid was 1∶ 12 with twice refluxing extraction( 2 h for each time). The optimum granule forming process was as follows: the pharmaceutical excipients were a mixture of dextrin and soluble starch with the best ratio of 1∶ 3. The granularity pass rate,moisture,loss on drying,solubility and angle of repose of the granule was 94. 12%,4. 87%,0. 93%,89. 23% and 36. 18°,respectively. Conclusion: The optimized refluxing extraction process is stable,reliable and feasible,and the prepared granule is in good formability and melting.
引文
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14 何龙,姚尧.中药颗粒剂的研究现状及应用前景分析[J].中医中药,2010,17(9):82-83
15 潘秀英.中药颗粒剂辅料的应用与发展探析[J].化工管理,2014,(23):44
16 王宏顺,熊学敏.中药颗粒剂辅料筛选的研究[J].江西中医药,2010,41(7):65-67
17 商思伟,赵玉莲,王从武.青天颗粒剂辅料筛选研究[J].中国兽医杂志,2014,50(4):43-45
2 肖蕾,项忠景,陈宝国.真武汤治疗慢性肾病研究进展[J].亚太传统医药,2016,12(18):62-64
3 侯兆辉,侯志敏.《伤寒论》真武汤方证浅析[J].中国中医急症,2010,19(3):487
4 Wu JB,Liu B,Liang CL,et al.Zhen-wu-tang attenuates cationic bovine serum albumin-induced inflammatory response in membranous glomerulonephritis rat through inhibiting AGEs/RAGE/NF-kappa B pathway activation[J].Int Immunopharmacol,2016,33:33-41
5 吴俊标,贺雨,梁春玲,等.真武汤水提液HPLC特征图谱研究及指标成分的测定[J].中国实验方剂学杂志,2014,20(18):45-49
6 肖敏,王建芬,陆叶,等.金樱子醇提颗粒处方工艺研究[J].中国药师,2014,17(6):945-947
7 中国药典[S].2015版.三部.通则11-通则12
8 Liang CL,Wu JB,Lai JM,et al.Protection effect of Zhen-Wu-Tang on adriamycin-induced nephrotic syndrome via inhibiting oxidative lesions and inflammation damage[J].Evid Based Complement Alternat Med,2014,2014:131604
9 宋立群,周波,贠捷,等.真武汤调节肾间质纤维化大鼠NF-κB表达的研究[J].中国临床保健杂志,2014,17(1):68-70
10 李莎莎,肖雪,韩凌,等.真武汤对肾纤维化大鼠血清和肾脏组织中SOD活力、MDA含量的影响[J].中药药理与临床,2012,28(2):19-21
11 宋业旭,刘爽,贠捷,等.真武汤治疗肾病临床用药的文献研究[J].中医药学报,2015,43(2):103-106
12 宋立群,贠捷,宋业旭,等.真武汤治疗慢性肾病的研究进展[J].中医药信息,2013,30(6):132-134
13 徐英霞.中药汤剂与中药颗粒剂比较探析[J].临床医药文献杂志,2015,2(1):87-88
14 何龙,姚尧.中药颗粒剂的研究现状及应用前景分析[J].中医中药,2010,17(9):82-83
15 潘秀英.中药颗粒剂辅料的应用与发展探析[J].化工管理,2014,(23):44
16 王宏顺,熊学敏.中药颗粒剂辅料筛选的研究[J].江西中医药,2010,41(7):65-67
17 商思伟,赵玉莲,王从武.青天颗粒剂辅料筛选研究[J].中国兽医杂志,2014,50(4):43-45