栀子饮片浸出物提取方法的建立及其在栀子不同饮片质量评价中的应用
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摘要
该实验采用层递分析法,通过浸出物得率差异,及针对浸出物中主要成分的差异分析,用于评价栀子不同饮片的质量。实验中采用热浸法、冷浸法比较水与不同浓度乙醇浸出物得率与化学成分含量差异,通过加权计算,优选栀子浸出物最佳提取方法,并对方法进行应用验证。加权计算结果显示,水溶性浸出物下冷浸法优于热浸法,醇溶性浸出物下以冷浸法下75%乙醇为最优。方法验证结果显示,冷浸法下水溶性浸出物可显著区分生栀子与焦栀子统货,同一批次来源生栀子、焦栀子、栀子炭饮片(P<0. 05)。醇溶性浸出物可明显区分同一批次中焦栀子与栀子炭饮片(P<0. 05)。而含量测定结果显示,饮片成分含量测定下,各成分在栀子不用炮制品中变异系数高于浸出物方法下成分测定,且羟异栀子苷为栀子与其炮制品之间含量变化差异较为显著的成分。故建议建立栀子水溶性浸出物方法与羟异栀子苷含量测定,共同用于栀子及其炮制品饮片的质量评价,为进一步完善栀子饮片质量标准提供科学依据。
In this experiment,the gradation analysis method was used to evaluate the quality of different pieces of Gardeniae Fructus through the extraction rate difference and the difference analysis of the main components in the extract. In this experiment cold-dip and hot-dip methods were used to compare the yield of Gardeniae Fructus extract and the content of chemical constituents with water,25%,50%,75% and 95% ethanol fractions. By weighted calculation,the optimal extraction method of Gardeniae Fructus was determined,and this was verified by practical application. Results showed that for the water-soluble extract,cold dip method was better than the hot dip method; and for alcohol-soluble extract,75% ethanol under cold dip method was best. The verification results showed that water-soluble extracts under cold dip methods could be used to significantly distinguish the raw Gardeniae Fructus( GF) and processed( stir-baked) GF( GFP) collected from the market. Meanwhile,this method could be also used to distinguish the same batch of GF,GFP and carbonized GF( GFC) with significant differences,respectively( P<0. 05). Ethanol-soluble extract can be used to clearly distinguish GFP and GFC pieces in the same batch( P<0. 05). The results of content determination showed that the variation coefficient of components in GF processed products was higher than that in extracts,and the content of hydroxygeniposide was the most significant component between GF and its processed products. It is suggested that the method of water-soluble extract of GF and the determination of the content of gardoside should be combined together to evaluate the quality of GF and its heat processed products.
In this experiment,the gradation analysis method was used to evaluate the quality of different pieces of Gardeniae Fructus through the extraction rate difference and the difference analysis of the main components in the extract. In this experiment cold-dip and hot-dip methods were used to compare the yield of Gardeniae Fructus extract and the content of chemical constituents with water,25%,50%,75% and 95% ethanol fractions. By weighted calculation,the optimal extraction method of Gardeniae Fructus was determined,and this was verified by practical application. Results showed that for the water-soluble extract,cold dip method was better than the hot dip method; and for alcohol-soluble extract,75% ethanol under cold dip method was best. The verification results showed that water-soluble extracts under cold dip methods could be used to significantly distinguish the raw Gardeniae Fructus( GF) and processed( stir-baked) GF( GFP) collected from the market. Meanwhile,this method could be also used to distinguish the same batch of GF,GFP and carbonized GF( GFC) with significant differences,respectively( P<0. 05). Ethanol-soluble extract can be used to clearly distinguish GFP and GFC pieces in the same batch( P<0. 05). The results of content determination showed that the variation coefficient of components in GF processed products was higher than that in extracts,and the content of hydroxygeniposide was the most significant component between GF and its processed products. It is suggested that the method of water-soluble extract of GF and the determination of the content of gardoside should be combined together to evaluate the quality of GF and its heat processed products.
引文
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[13]肖小华,徐丽瑛,周艳艳,等.栀子苷和西红花苷Ⅰ对ANIT致小鼠肝损伤的保肝作用研究[J].时珍国医国药,2014(7):1600.
[14]石若夫,李大力,田春宇,等.栀子多糖的抗肿瘤活性研究[J].林产化学与工业,2002,22(4):67.
[15]刘国敏,郭素华,程维明.栀子的药理作用及其机制研究新进展[J].海峡药学,2008,20(11):8.
[16]李玲云.栀子饮片及其成方制剂的质量标准研究[D].郑州:河南中医药大学,2017.
[2]苏文田,谢建秋,潘心禾,等.多花黄精多糖与浸出物的时空变异规律[J].中国中药杂志,2019,44(2):270.
[3]杨洪军,黄璐琦.中药饮片用量标准研究[M].福州:福建科学技术出版社,2011:50.
[4]中国药典.一部[S].2015.
[5]孟延发,刘景会,李志孝,等.栀子多糖的分离纯化及其基本性质[J].兰州大学学报,1993,29(2):109.
[6]王伟影,毛菊华,余乐,等.市售栀子饮片的质量评价研究[J].中国现代应用药学,2017,34(5):681.
[7]刘电航,左月明,张忠立,等.栀子化学成分研究[J].中国实验方剂学杂志,2016,22(7):46.
[8]陈红,肖永庆,李丽,等.栀子化学成分研究[J].中国中药杂志,2007,32(11):1041.
[9]方尚玲,刘源才,张庆华,等.栀子苷镇痛和抗炎作用的研究[J].时珍国医国药,2008,19(6):1374.
[10]吴虹,魏伟,宋礼华.栀子总苷的抗炎镇痛作用研究[J].中国中医药信息杂志,2006,13(7):31.
[11]张学兰,孙秀梅,牛序莉,等.炮制对栀子部分成分及解热作用的影响[J].中药材,1995,18(3):136.
[12]魏春华,邵坚,罗光明.栀子生品及炮制品对CCl4致大鼠急性肝损伤保护作用的比较[J].中国实验方剂学杂志,2016,22(17):15.
[13]肖小华,徐丽瑛,周艳艳,等.栀子苷和西红花苷Ⅰ对ANIT致小鼠肝损伤的保肝作用研究[J].时珍国医国药,2014(7):1600.
[14]石若夫,李大力,田春宇,等.栀子多糖的抗肿瘤活性研究[J].林产化学与工业,2002,22(4):67.
[15]刘国敏,郭素华,程维明.栀子的药理作用及其机制研究新进展[J].海峡药学,2008,20(11):8.
[16]李玲云.栀子饮片及其成方制剂的质量标准研究[D].郑州:河南中医药大学,2017.