参黄搽剂的质量标准研究
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摘要
目的:为参黄搽剂质量标准的建立提供参考。方法:按2015年版《中国药典》(四部)中薄层色谱法(TLC)对参黄搽剂中的苦参、黄柏、大黄、黄芩进行定性鉴别;采用高效液相色谱法(HPLC)测定参黄搽剂中苦参碱和氧化苦参碱的含量[色谱柱为Phenomenex Luna NH_2,流动相为乙腈-无水乙醇-3%磷酸水溶液(80∶10∶10,V/V/V),柱温为45℃,流速为1.0 mL/min,检测波长为220 nm,进样量为5μL]。结果:TLC结果显示,各供试品色谱与对照药材/对照品色谱相应位置上有相同颜色的对应斑点,且斑点清晰、比移值适中、分离度高,阴性对照无干扰。HPLC结果显示,苦参碱、氧化苦参碱分别在进样量为203.60~1 221.60 ng(r=0.999 4)、210.08~840.30 ng(r=0.999 7)范围内与其峰面积呈现出良好的线性关系;精密度、稳定性、重复性试验的RSD均小于3.0%(n=6);平均加样回收率分别为96.03%、100.93%,RSD分别为2.55%、2.69%(n=9)。结论:所建立方法专属性强、准确度高、重现性好,可用于参黄搽剂的质量控制。
OBJECTIVE:To provide reference for the establishment of quality standard of Shenhuang liniment. METHODS:Qualitative identification of Sophora flavescens,Phellodendron chinense,Rhei Radix Et Rhizoma and Scutellaria baicalensis in Shenhuang liniment were carried out by TLC according to the method of 2015 edition of Chinese Pharmacopeia(part Ⅳ). HPLC method was used to determine the contents of matrine and oxymatrine in Shenhuang liniment [Phenomenex Luna NH2 column,mobile phase consisting of acetonitrile-absolute ethanol-3% phosphoric acid aqueous solution(80 ∶ 10 ∶ 10,V/V/V),column temperature of 45 ℃,flow rate of 1.0 m L/min,detection wavelength of 220 nm,sample size of 5 μ L]. RESULTS:Results of TLC showed that the corresponding spots of the same color were found in the corresponding positions of the chromatograms for test samples and reference substance/substance control;and the spots were clear,retardation factor was moderate,the separation degree was high,and the negative control had no interference. Results of HPLC showed that the linear range of matrine and oxymatrine were 203.60-1 221.60 ng(r=0.999 4)and 210.08-840.30 ng(r=0.999 7),respectively. RSDs of precision,stability and reproducibility tests were all lower than 3.0%(n=6). Average recovery rates were 96.03% and 100.93%,and RSDs were 2.55%and 2.69%(n=9). CONCLUSIONS:Established method is specific,accurate and reproducible,and can be used for quality control of Shenhuang liniment.
OBJECTIVE:To provide reference for the establishment of quality standard of Shenhuang liniment. METHODS:Qualitative identification of Sophora flavescens,Phellodendron chinense,Rhei Radix Et Rhizoma and Scutellaria baicalensis in Shenhuang liniment were carried out by TLC according to the method of 2015 edition of Chinese Pharmacopeia(part Ⅳ). HPLC method was used to determine the contents of matrine and oxymatrine in Shenhuang liniment [Phenomenex Luna NH2 column,mobile phase consisting of acetonitrile-absolute ethanol-3% phosphoric acid aqueous solution(80 ∶ 10 ∶ 10,V/V/V),column temperature of 45 ℃,flow rate of 1.0 m L/min,detection wavelength of 220 nm,sample size of 5 μ L]. RESULTS:Results of TLC showed that the corresponding spots of the same color were found in the corresponding positions of the chromatograms for test samples and reference substance/substance control;and the spots were clear,retardation factor was moderate,the separation degree was high,and the negative control had no interference. Results of HPLC showed that the linear range of matrine and oxymatrine were 203.60-1 221.60 ng(r=0.999 4)and 210.08-840.30 ng(r=0.999 7),respectively. RSDs of precision,stability and reproducibility tests were all lower than 3.0%(n=6). Average recovery rates were 96.03% and 100.93%,and RSDs were 2.55%and 2.69%(n=9). CONCLUSIONS:Established method is specific,accurate and reproducible,and can be used for quality control of Shenhuang liniment.
引文
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[19]孔燕,王健.益气通脉软胶囊质量标准的研究[J].中成药,2019,41(3):516-521.
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[2]龙梅,徐玲,王欢.苦参的研究进展[J].世界最新医学信息文摘,2017,17(99):78-79.
[3]樊宏伟,卢继红,张蓉.苦参碱类生物碱的体外抑菌、抑病毒及诱生干扰素的实验研究[J].中医药信息,2000,17(4):75-76.
[4]李媛媛,阎旭,李墨林,等.氧化苦参碱体外抑菌活性的研究[J].中国微生态学杂志,2012,24(3):244-245,250.
[5]董方亮.氧化苦参碱抗慢性病毒性肝炎作用机制及临床研究概述[J].中国药师,2013,34(12):1912-1914.
[6]刘晓琼,沈宏辉,陈佳欣,等.苦参碱类生物碱联合胸腺肽抗HBV作用研究[J].中国中药杂志,2016,41(7):1275-1281.
[7]董晓巧,俞文华,张祖勇,等.氧化苦参碱对脑外伤大鼠脑组织IL-1β、TNF-α和IL-6水平的影响[J].浙江中西医结合杂志,2012,22(7):508-510,516.
[8]刘艳明,王雪芳.氧化苦参碱对缺血缺氧致兔心律失常保护作用及机制研究[J].河北医药,2015,37(9):1308-1310.
[9]陈晓峡,向小庆,叶红.苦参碱及氧化苦参碱抗肿瘤作用的研究进展[J].中国实验方剂学杂志,2013,34(11):361-364.
[10]陈晨,金玉.氧化苦参碱防治慢性肾纤维化机理的实验研究[J].陕西中医,2014,35(1):106-109.
[11]李嘉诚,吴岚,蔡同凯,等.黄柏化学成分及其药理作用研究进展[J].药学实践杂志,2018,36(5):389-391,398.
[12]于建玉,廖欣,丁厚伟,等.中药大黄药理作用研究进展及其临床应用[J].中国现代药物应用,2016,10(11):286-287.
[13]谢艳,毕军花,郭云鹏.道地黄芩与非道地黄芩的解毒作用比较研宄[J].中医药导报,2015,21(8):35-38.
[14]姜丹.黄芩道地性的遗传和化学物质基础研究[D].北京:北京中医药大学,2018.
[15]苏坤莲,凡永杰,刘原,等.冰片对心脑血管系统药理作用及其机制的研究进展[J].辽宁中医杂志,2018,45(9):2001-2003.
[16]尚坤,李敬文,常美月,等.冰片化学成分及药理作用研究[J].吉林中医药,2018,38(1):93-95.
[17]孙冬梅,林晓燕,李素梅,等.复方芪麻胶囊的质量标准研究[J].中国药房,2017,28(18):2553-2556.
[18]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,2015:57-59.
[19]孔燕,王健.益气通脉软胶囊质量标准的研究[J].中成药,2019,41(3):516-521.
[20]国家药典委员会.中华人民共和国药典:一部[S]. 2015年版.北京:中国医药科技出版社,2015:23,202,301,305.