大黄泻火散质量标准改进研究
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摘要
目的改进大黄泻火散(大黄、薄荷、炙甘草、连翘、黄芩、炒栀子仁)的质量标准。方法采用粉末显微鉴别法鉴别处方中大黄、薄荷、炙甘草、连翘、黄芩、炒栀子仁;采用薄层色谱(TLC)法鉴别处方中的炙甘草和黄芩。采用高效液相色谱(HPLC)法,流动相为甲醇-0. 1%磷酸溶液,梯度洗脱;色谱柱为Waters C_(18)柱(250 mm×4. 6 mm,5μm);流速为1. 0 m L/min;检测波长为254 nm。测定大黄中的大黄素和大黄酸;流动相为乙腈-0. 1%磷酸溶液;色谱柱为Waters C18柱(250 mm×4. 6 mm,5μm);流速为1. 0 m L/min;检测波长为205 nm。测定连翘中的连翘苷。结果粉末显微鉴别中各饮片组织特征明显;薄层色谱中特征性斑点明显,分离度好,阴性对照无干扰。大黄中大黄素和大黄酚进样量分别在51. 2~1 280. 0 ng(r=0. 999 8)和49. 8~1 250. 0 ng(r=0. 999 8)范围内与峰面积线性关系良好;平均回收率分别为95. 95%和95. 58%,RSD分别为1. 39%和1. 54%(n=9)。连翘中连翘苷进样量在54. 8~1 370. 0 ng(r=0. 999 9)范围内与峰面积线性关系良好;平均回收率为95. 84%,RSD为1. 26%(n=9)。结论鉴别方法专属性强、灵敏度高,定量测定方法简便快速,结果准确,重复性良好,可作为大黄泻火散的质量控制方法。
Objective To improve the quality standard for Dahuang Xiehuo San( Rhei Radix et Rhizoma, Menthae Haplocalycis Herba,Glycyrrhizae Radix et Rhizoma Praeparata Cum Melle, Forsythiae Fructus, Scutellariae Radix, Gardeniae Fructus Semen Tostum). Methods Rhei Radix et Rhizoma, Menthae Haplocalycis Herba, Glycyrrhizae Radix et Rhizoma Praeparata Cum Melle, Forsythiae Fructus, Scutellariae Radix, Gardeniae Fructus Fructus Tostum were identified by powder microscopic identification method. Glycyrrhizae Radix et Rhizoma Praeparata Cum Melle and Scutellariae Radix were identified by TLC method. HPLC method was adopted, the mobile phase was methanol-0. 1% phosphoric acid, gradient elution, the chromatographic column was Waters C18 column( 250 mm × 4. 6 mm,5 μm), the flow rate was 1. 0 m L/min,the detection wavelength was 254 nm,the content emodin and rhein in Rhei Radix et Rhizoma was determined. The mobile phase was acetonitrile-0. 1% phosphoric acid,the chromatographic column was Waters C18 column( 250 mm × 4. 6 mm,5 μm), the flow rate was 1. 0 m L/min,the detection wavelength was 205 nm,and the content of forsythin in Forsythiae Fructus was determined. Results In powder microscopic identification,the tissue characteristics of each decoction piece were obvious,and the characteristic spots could be detected by TLC and well separated without the interference of negative samples. The emodin and chrysophanol were linear in the ranges of 51. 2-1 280. 0 ng( r = 0. 999 8), 49. 8-1 250. 0 ng( r = 0. 999 8), the average recovery rates were95. 95% and 95. 58%, RSDs were 1. 39% and 1. 54%( n = 9). The forsythin was linear in the range of 54. 8-1 370. 0 ng( r = 0. 999 9),the average recovery rate was 95. 84%, RSD was 1. 26%( n = 9). Conclusion The method is specific,sensitive, simple, rapid,accurate and reproducible,which can be used as a quality control method for Dahuang Xiehuo San.
Objective To improve the quality standard for Dahuang Xiehuo San( Rhei Radix et Rhizoma, Menthae Haplocalycis Herba,Glycyrrhizae Radix et Rhizoma Praeparata Cum Melle, Forsythiae Fructus, Scutellariae Radix, Gardeniae Fructus Semen Tostum). Methods Rhei Radix et Rhizoma, Menthae Haplocalycis Herba, Glycyrrhizae Radix et Rhizoma Praeparata Cum Melle, Forsythiae Fructus, Scutellariae Radix, Gardeniae Fructus Fructus Tostum were identified by powder microscopic identification method. Glycyrrhizae Radix et Rhizoma Praeparata Cum Melle and Scutellariae Radix were identified by TLC method. HPLC method was adopted, the mobile phase was methanol-0. 1% phosphoric acid, gradient elution, the chromatographic column was Waters C18 column( 250 mm × 4. 6 mm,5 μm), the flow rate was 1. 0 m L/min,the detection wavelength was 254 nm,the content emodin and rhein in Rhei Radix et Rhizoma was determined. The mobile phase was acetonitrile-0. 1% phosphoric acid,the chromatographic column was Waters C18 column( 250 mm × 4. 6 mm,5 μm), the flow rate was 1. 0 m L/min,the detection wavelength was 205 nm,and the content of forsythin in Forsythiae Fructus was determined. Results In powder microscopic identification,the tissue characteristics of each decoction piece were obvious,and the characteristic spots could be detected by TLC and well separated without the interference of negative samples. The emodin and chrysophanol were linear in the ranges of 51. 2-1 280. 0 ng( r = 0. 999 8), 49. 8-1 250. 0 ng( r = 0. 999 8), the average recovery rates were95. 95% and 95. 58%, RSDs were 1. 39% and 1. 54%( n = 9). The forsythin was linear in the range of 54. 8-1 370. 0 ng( r = 0. 999 9),the average recovery rate was 95. 84%, RSD was 1. 26%( n = 9). Conclusion The method is specific,sensitive, simple, rapid,accurate and reproducible,which can be used as a quality control method for Dahuang Xiehuo San.
引文
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[2]方晴霞. RP-HPLC法测定大黄泻火滴丸中大黄素的含量[J].中国药师,2010,13(2):298.
[3]中华人民共和国卫生部药典委员会.中药粉末显微鉴别彩色图集[M].广州:广东科技出版社,1999:54,180,225,297,360.
[4]国家药典委员会.中华人民共和国药典(四部)[M].北京:中国医药科技出版社,2015:57.
[5]陆静娴,谭春梅,陈碧莲,等.明目上清丸质量标准改进[J].药物分析杂志,2016,36(11):2051-2058.
[6]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,2015:170.
[7]李向军,王超,王永,等.中药薄层色谱影响因素分析及应用[J].中国药业,2011,20(14):13.
[8]王伽伯,金城,李会芳,等.泻下类中药质量的生物控制方法及基本问题探讨[J].药学学报,2009,44(5):500.
[9]李丽.大黄炮制前后物质基础变化规律研究[D].北京:中国中医科学院中药研究所,2011.
[10]段冰艳,韩豫皖,金鉴,等.美宝胶囊中大黄素的含量测定[J].时珍国医国药杂志,2006,17(1):37-38.
[11]韩莉,张贞丽,徐丽华,等.连翘中连翘苷含量测定方法的试验研究[J].齐鲁药事,2008,27(3):153.