枳实制白术的炮制工艺优选及HPLC特征图谱分析
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摘要
目的:探讨枳实制白术的最佳炮制工艺,建立其HPLC特征图谱。方法:采用"脾虚泄泻"免疫力低下动物模型和大鼠饮水量来评价枳实制白术的健脾祛燥作用;通过对比不同配比枳实制白术饮片的健脾祛燥作用,筛选枳实与白术的最佳配比;采用正交试验,以辛弗林和白术内酯Ⅲ的含量为评价指标,优选枳实制白术的炮制工艺,并建立其特征图谱。结果:10%枳实制白术组的效果最佳。枳实制白术饮片炮制过程中,影响辛弗林及白术内酯Ⅲ的主次因素依次为烘制温度>炒制温度>炒制时间,最佳炮制工艺为取生白术饮片100 g,加入枳实汁50 mL(生药质量浓度0.2 g·mL~(-1)),浸泡24 h,不时翻动,直至汁尽药透,于110℃炒制6 min,取出,于40℃烘箱干燥。枳实制白术有5个共有峰,均能达到较好分离,该分析方法具有良好的精密度、重复性和稳定性,符合特征图谱相关要求。结论:药汁制是中药炮制的重要组成部分,枳实制白术的健脾祛燥作用充分体现了这一炮制特色——增效,纠正偏性。建立的HPLC特征图谱方法准确、可靠,为枳实制白术的质量控制提供了参考。
Objective: To optimize processing technology of Atractylodis Macrocephalae Rhizoma processed with Aurantii Fructus Immaturus and establish its HPLC fingerprint. Method: The invigorating spleen and dispelling dryness of Atractylodis Macrocephalae Rhizoma processed with Aurantii Fructus Immaturus was investigated by model rats with splenasthenic diarrhea, and then the best ratio of Atractylodis Macrocephalae Rhizoma and Aurantii Fructus Immaturus was screened. Taking overall desirability of contents of synephrine and atractylenolide Ⅲ as index,orthogonal test was employed to optimize processing technology,and HPLC fingerprint of this processed product was established. Result: The best ratio of Atractylodis Macrocephalae Rhizoma to Aurantii Fructus Immaturus was 9 ∶ 1. The factors influenced contents of synephrine and atractylenolide Ⅲ were followed by baking temperature > frying temperature > frying time,optimum processing technology of this processed product was as follows: added Aurantii Fructus Immaturus juice 50 mL(crude drug concentration of 0. 2 g·mL~(-1)) into 100 g of Atractylodis Macrocephalae Rhizoma pieces,soaked 24 hours,fried 6 min at 110 ℃,dried at 40 ℃ in a oven. Five common peaks were selected in Atractylodis Macrocephalae Rhizoma processed with Aurantii Fructus Immaturus. Among the obtained fingerprint,all of the detected peaks were separated effectively.The accuracy,repeatability and stability of this method were satisfied. Conclusion: The invigorating spleen and dispelling dryness of Atractylodis Macrocephalae Rhizoma processed with Aurantii Fructus Immaturus can reflect the processing characteristics of increasing efficiency and correcting bias. The established HPLC fingerprint can provide reference for the quality control of this processed product.
Objective: To optimize processing technology of Atractylodis Macrocephalae Rhizoma processed with Aurantii Fructus Immaturus and establish its HPLC fingerprint. Method: The invigorating spleen and dispelling dryness of Atractylodis Macrocephalae Rhizoma processed with Aurantii Fructus Immaturus was investigated by model rats with splenasthenic diarrhea, and then the best ratio of Atractylodis Macrocephalae Rhizoma and Aurantii Fructus Immaturus was screened. Taking overall desirability of contents of synephrine and atractylenolide Ⅲ as index,orthogonal test was employed to optimize processing technology,and HPLC fingerprint of this processed product was established. Result: The best ratio of Atractylodis Macrocephalae Rhizoma to Aurantii Fructus Immaturus was 9 ∶ 1. The factors influenced contents of synephrine and atractylenolide Ⅲ were followed by baking temperature > frying temperature > frying time,optimum processing technology of this processed product was as follows: added Aurantii Fructus Immaturus juice 50 mL(crude drug concentration of 0. 2 g·mL~(-1)) into 100 g of Atractylodis Macrocephalae Rhizoma pieces,soaked 24 hours,fried 6 min at 110 ℃,dried at 40 ℃ in a oven. Five common peaks were selected in Atractylodis Macrocephalae Rhizoma processed with Aurantii Fructus Immaturus. Among the obtained fingerprint,all of the detected peaks were separated effectively.The accuracy,repeatability and stability of this method were satisfied. Conclusion: The invigorating spleen and dispelling dryness of Atractylodis Macrocephalae Rhizoma processed with Aurantii Fructus Immaturus can reflect the processing characteristics of increasing efficiency and correcting bias. The established HPLC fingerprint can provide reference for the quality control of this processed product.
引文
[1]徐楚江,万德光,杨明.传统药汁制法的探讨[J].中国中药杂志,1989,14(3):22-25.
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[3]崔妮,史辑,景海漪,等.中药炮制药汁制法历史沿革及研究进展[J].药学实践杂志,2014,32(3):167-198.
[4]王朝阳.《伤寒杂病论》中白术临床运用及证治规律研究[D].武汉:湖北中医药大学,2015.
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[6]于欢,钟凌云,宁希鲜,等.枳实不同炮制品挥发油GC-MS分析[J].中国实验方剂学杂志,2015,21(15):12-18.
[7]国家药典委员会.中华人民共和国药典.一部[M].北京:中国医药科技出版社,2015:103-104.
[8]张金莲,谢日健,刘明贵,等.不同炮制方法对白术中白术内酯Ⅰ,Ⅱ,Ⅲ含量的影响[J].中国实验方剂学杂志,2016,22(21):15-18.
[9]龙全江,徐雪琴,胡昀.白术的化学、药理与炮制研究进展[J].中国中医药信息杂志,2004,11(11):1033-1034.
[10]孙慧茹,杨庆有.临床运用枳术汤的升降作用经验拾零[J].陕西中医,2008,29(8):1072.
[11]李新旺,任钧国.枳实白术配伍的实验研究[J].中医研究,2002,15(6):23-25.
[12]田亚欣,王凤云,张娇,等.功能性消化不良的常用方剂及药对规律总结[J].中国实验方剂学杂志,2016,22(21):182-185.
[13]钟子劭,张海燕,张望,等.四君子汤对脾虚证胃肠动力障碍大鼠胃平滑肌Ca M-MLCK信号通路的机制探讨[J].中国实验方剂学杂志,2018,24(5):95-99.
[14]刘名波.香砂六君子汤对脾虚泄泻免疫功能和肠道微生态的影响[D].苏州:苏州大学,2015.
[15]刘蔚雯.枳实、白术促胃肠动力作用的配伍及枳术饮作用机理的研究[D].哈尔滨:黑龙江中医药大学,2007.
[16]龚鹏飞,于欢,翟莹莹,等.多指标评价米泔水漂苍术对湿盛困脾脾虚大鼠的药效作用[J].中国实验方剂学杂志,2017,23(24):36-40.
[17]刘瑶,刘伟.藿香正气散对湿困脾胃型亚健康大鼠胃肠功能的影响[J].江苏中医药,2011,43(6):89-90.
[18]祝婧,钟凌云,叶喜德,等.枳壳不同炮制品的燥性比较及其对功能性消化不良大鼠胃肠功能的影响[J].中国实验方剂学杂志,2017,23(22):20-26.
[2]王丽娜,贾天柱,刘洋.药汁制法研究概况[J].中成药,2006,28(12):1803-1805.
[3]崔妮,史辑,景海漪,等.中药炮制药汁制法历史沿革及研究进展[J].药学实践杂志,2014,32(3):167-198.
[4]王朝阳.《伤寒杂病论》中白术临床运用及证治规律研究[D].武汉:湖北中医药大学,2015.
[5]石俊英,陈随清,崔亚军,等.中药鉴定学[M].北京:中国医药科技出版社,2006:316.
[6]于欢,钟凌云,宁希鲜,等.枳实不同炮制品挥发油GC-MS分析[J].中国实验方剂学杂志,2015,21(15):12-18.
[7]国家药典委员会.中华人民共和国药典.一部[M].北京:中国医药科技出版社,2015:103-104.
[8]张金莲,谢日健,刘明贵,等.不同炮制方法对白术中白术内酯Ⅰ,Ⅱ,Ⅲ含量的影响[J].中国实验方剂学杂志,2016,22(21):15-18.
[9]龙全江,徐雪琴,胡昀.白术的化学、药理与炮制研究进展[J].中国中医药信息杂志,2004,11(11):1033-1034.
[10]孙慧茹,杨庆有.临床运用枳术汤的升降作用经验拾零[J].陕西中医,2008,29(8):1072.
[11]李新旺,任钧国.枳实白术配伍的实验研究[J].中医研究,2002,15(6):23-25.
[12]田亚欣,王凤云,张娇,等.功能性消化不良的常用方剂及药对规律总结[J].中国实验方剂学杂志,2016,22(21):182-185.
[13]钟子劭,张海燕,张望,等.四君子汤对脾虚证胃肠动力障碍大鼠胃平滑肌Ca M-MLCK信号通路的机制探讨[J].中国实验方剂学杂志,2018,24(5):95-99.
[14]刘名波.香砂六君子汤对脾虚泄泻免疫功能和肠道微生态的影响[D].苏州:苏州大学,2015.
[15]刘蔚雯.枳实、白术促胃肠动力作用的配伍及枳术饮作用机理的研究[D].哈尔滨:黑龙江中医药大学,2007.
[16]龚鹏飞,于欢,翟莹莹,等.多指标评价米泔水漂苍术对湿盛困脾脾虚大鼠的药效作用[J].中国实验方剂学杂志,2017,23(24):36-40.
[17]刘瑶,刘伟.藿香正气散对湿困脾胃型亚健康大鼠胃肠功能的影响[J].江苏中医药,2011,43(6):89-90.
[18]祝婧,钟凌云,叶喜德,等.枳壳不同炮制品的燥性比较及其对功能性消化不良大鼠胃肠功能的影响[J].中国实验方剂学杂志,2017,23(22):20-26.