基于对照制剂的复方丹参片质量评价新模式探讨  

Discussion on a novel quality evaluation model for compound Danshen tablets based on reference drug

作　　者：林敬开 聂黎行[2] 姚力 白桂昌 罗轶 戴忠[2] 马双成[2] LIN Jing-kai;NIE Li-xing;YAO Li;BAI Gui-chang;LUO Yi;DAI Zhong;MA Shuang-cheng(Guangxi Institute for Food and Drug Control,Nanning 530021,China;National Institutes for Food and Drug Control,Beijing 100050,China)

机构地区：[1]广西壮族自治区食品药品检验所,南宁530021 [2]中国食品药品检定研究院,北京100050

出　　处：《药物分析杂志》2019年第10期1751-1761,共11页Chinese Journal of Pharmaceutical Analysis

基　　金：广西壮族自治区食品药品监督管理局“食品药品安全标准工作”（桂食药科2018-4）;中国食品药品检定研究院学科带头人培养基金资助项目(2017X1)

摘　　要：目的:以对照制剂为参照物,结合多组分含量测定,建立复方丹参片质量评价新模式。方法:采用YMC Hydrosphere C18色谱柱(4.6 mm×250 mm,5μm),以乙腈-0.1%磷酸水溶液为流动相进行梯度洗脱,流速1.0 mL·min^-1,柱温30℃,检测波长280 nm,同时测定复方丹参片中丹参素、原儿茶醛、迷迭香酸、丹酚酸B 4个丹参水溶性成分的含量。采用SHISEIDO CAPCELL PAK C18 MGⅡ色谱柱(4.6 mm×250 mm,5μm),以乙腈-水为流动相进行梯度洗脱,流速1.0 mL·min^-1,柱温30℃,以Alltech 3300蒸发光散射检测器检测,漂移管温度55℃,氮气流速2.0 L·min^-1,同时测定复方丹参片中三七皂苷R1、人参皂苷Rg1、人参皂苷Re、人参皂苷Rb1、人参皂苷Rd 5个三七皂苷类成分的含量。制备复方丹参片对照制剂,将其作为随行对照应用于样品中丹参水溶性成分和三七皂苷类成分的含量测定,对样品的质量进行评价。结果:丹参素、原儿茶醛、迷迭香酸、丹酚酸B、三七皂苷R1、人参皂苷Rg1、人参皂苷Re、人参皂苷Rb1、人参皂苷Rd 9个成分在一定浓度范围内与峰面积呈良好的线性关系,相关系数r不低于0.999 5;平均回收率(n=6)为97.5%~102.6%。11个厂家19批样品中,8批样品中丹参水溶性成分及三七皂苷类成分的含量分别相当于对照制剂的量均≥90.0%,占样品总批数的42.1%,11批样品中丹参水溶性成分及三七皂苷类成分的含量分别相当于对照制剂的量≥70%且<90%,占样品总批数的57.9%。不同厂家产品的质量差异较大。结论:建立的质量评价模式可反映复方丹参片的质量优劣,为建立中成药质量评价新模式提供借鉴和参考。Objective:Taking reference drug as control,to establish a new quality evaluation model for compound Danshen tablets(CDT) based on multi-component determination. Methods:Simultaneous determination of danshensu,protocatechuic,aldehyde,rosmarinic acid and salvianolic acid B was performed on a YMC Hydrosphere C18 column(4.6 mm×250 mm,5 μm) with acetonitrile-0.1% phosphoric acid as the mobile phase in gradient elution at a flow rate of 1.0 mL·min^-1. The column temperature was 30 ℃ and the detection wavelength was 280 nm. Simultaneous determination of notoginsenoside R1,ginsenoside Rg1,ginsenoside Re,ginsenoside Rb1 and ginsenoside Rd was performed on a SHISEIDO CAPCELL PAK C18 MG Ⅱ column(4.6 mm×250 mm,5 μm) with acetonitrile-water as the mobile phase in gradient elution at a flow rate of 1.0 m L·min^-1. The column temperature was 30 ℃ and an Alltech 3300 ELSD was used as detector with drift tube temperature of 55 ℃ and N2 flow rate of 2.0 L·min^-1. CDT reference drug was developed and applied as accompanying control in the determination of the contents and quality evaluation of the samples. Results:4 hydrophilic compounds from Radix Salviae Miltiorrhizae and 5 saponins from Notoginseng Radix et Rhizoma showed good linearity(r ≥0.999 5). The average recoveries(n=6) were in the range of 97.5%^-102.6%. Among 19 samples from 11 manufactures,the ratio of contents in 8 samples to those in CDT reference drug were above 90%,the ratio in 11 samples were within 70% and 90%,which accounted for 42.1% and 57.9% of all samples,respectively. These results indicated that there were large differences in the quality of CDT from difference enterprises. Conclusion:The proposed quality evaluation model can reflect the quality variation of CDT,which provides reference for establishing new quality evaluation model of Chinese traditional medicine.

关 键 词：复方丹参片 中药复方制剂 丹参 三七 冰片 对照制剂 质量评价模式 丹参水溶性成分 三七皂苷类成分 高效液相色谱 

分 类 号：R917[医药卫生—药物分析学]