心脉通片质量标准的研究  

Study on the Quality Standard for Xinmaitong Tablets

作　　者：陈正东 乔莉[1] 周颖仪[1] 刘潇潇[1] Chen Zhengdong;Qiao Li;Zhou Yingyi;Liu Xiaoxiao(Guangdong Institute for Drug Control,Guangzhou 510663,China)

机构地区：[1]广东省药品检验所,广州510663

出　　处：《中国药师》2020年第4期750-754,共5页China Pharmacist

摘　　要：目的:建立心脉通片的定性鉴别方法和含量测定方法,以完善其质量标准。方法:采用TLC法对心脉通片中毛冬青、钩藤、夏枯草分别进行定性鉴别。采用HPLC法分别测定心脉通片中丹参素、橙黄决明素的含量:色谱柱分别为SymmetryShieldTMRP18、Thermo ODS Hypersil,流动相分别为甲醇-乙腈(30∶10)-0.5%甲酸溶液(梯度洗脱)、乙腈-0.1%磷酸溶液(25∶75),检测波长分别为280 nm、284 nm,流速均为1.0 ml·min^-1,柱温均为30℃,进样量分别为10μl、20μl。结果:TLC图谱斑点清晰,分离度好,阴性对照无干扰。丹参素钠、橙黄决明素的进样浓度线性范围分别为0.021~0.527 mg·ml^-1(r=1.000 0)、0.236~18.894μg·ml-1(r=0.999 8),平均回收率分别为98.5%(RSD=1.7%,n=6),108.8%(RSD=0.5%,n=6),精密度、稳定性、重复性试验的RSD均小于4.5%(n=6)。结论:研究建立的定性、定量方法准确可靠,能为心脉通片质量标准的提高奠定研究基础。Objective: To establish the qualitative identification and content determination methods,thus to improve the quality standard for Xinmaitong tablets. Methods: TLC was used for the qualitative identification of Radix ilecis Pubescens,Uncariaeramulus cum uncis and Prunellae spica in Xinmaitong tablets. HPLC was adopted for the content determination of danshensu and aurantio-obtusin in the preparation. The determination of danshensu was performed on a Symmetry ShieldTMRP18 column with the mobile phase consisting of methanol-acetonitrile( 30 ∶ 10)-0.5% formic acid solution with gradient elution at the flow rate of 1.0 ml·min-1,while the determination of aurantio-obtusin was performed on a Thermo ODS Hypersil column with the mobile phase consisting of acetonitrile-0.1% phosphoric acid solution( 25 ∶ 75) at the flow rate of 1.0 ml·min^-1. The detection wavelength was respectively set at 280 nm and284 nm,and the column temperature was 30 ℃ . The injection volume was 10 μl and 20 μl,respectively. Results: The TLC spots were clear with good separation and without any interference from the negative controls. The linear range of danshensu sodium and aurantioobtusin was 0.021-0.527 mg·ml^-1( r = 1.000 0) and 0.236-18.894 μg·ml^-1( r = 0.999 8),respectively. The average recovery was98.5%( RSD = 1.7%,n = 6) and 108.8%( RSD = 0.5%,n = 6),respectively. The RSDs of precision,stability and reproducibility tests were all lower than 4.5%( n = 6). Conclusion: The established identification and content determination methods are accurate and reliable,which can provide scientific reference for the quality standard improvement of Xinmaitong tablets.

关 键 词：质量标准 薄层色谱法 高效液相色谱法 毛冬青 钩藤 夏枯草 丹参素 橙黄决明素 

分 类 号：TQ460.72[医药卫生—药物分析学]