丹参茎叶药材的质量标准研究  

Quality standard for stems and leaves of Salvia miltiorrhiza

作　　者：沙秀秀 戴新新 宿树兰[1] 严辉[1] 郭盛[1] 钱大玮[1] 唐志书[2] 段金廒[1] 

机构地区：[1]南京中医药大学江苏省中药资源产业化过程协同创新中心/中药资源产业化与方剂创新药物国家地方联合工程研究中心,南京210023 [2]陕西中医药大学陕西省中药资源产业化协同创新中心,咸阳712046

出　　处：《药物分析杂志》2016年第6期1094-1100,共7页Chinese Journal of Pharmaceutical Analysis

基　　金：江苏高校中药资源产业化过程协同创新中心建设专项(2013年度);江苏省"333高层次人才工程"第一层次培养对象资助项目(2013年度);江苏省高校中药学优势学科Ⅱ期建设项目(ysxk-2014)

摘　　要：目的:丹参花期至初秋地上嫩茎叶部位是制药或制茶的原料,研究制定其质量标准,使其资源化价值不断提升和拓展。方法:运用薄层色谱法分别对芦丁、异槲皮苷、迷迭香酸和丹酚酸B进行定性鉴别,其条件:以醋酸丁酯-甲酸-水(10∶2∶3)为展开剂,紫外灯(365 nm)下检视;参照中国药典2015年版附录相关方法对丹参茎叶药材的总灰分和酸不溶性灰分进行测定;运用高效液相色谱法分别对丹参素、原儿茶醛、咖啡酸、芦丁、异槲皮苷、迷迭香酸、紫草酸和丹酚酸B进行定量测定,其条件:色谱柱为Grace Apollo C_(18)(4.6 mm×250 mm,5μm),流动相为乙腈(A)-0.1%甲酸水(B),梯度洗脱(0~5 min,10% A;5~10 min,10% A→12% A;10~20 min,12% A→14% A;20~25 min,14% A→20% A;25~60 min,20% A→30% A;60~65 min,30% A→40% A);流速1 mL·min^(-1),检测波长280 nm和256 nm。结果:薄层色谱鉴别芦丁、异槲皮苷、迷迭香酸和丹酚酸B,色谱斑点清晰,分离度良好;10批样品中总灰分测定结果为7.14%~9.86%,酸不溶性灰分为0.06%~0.38%;HPLC色谱分析结果表明,丹参素、原儿茶醛、咖啡酸、芦丁、异槲皮苷、迷迭香酸、紫草酸和丹酚酸B进样质量分别在0.163~3.26、0.118~2.36、0.117~2.34、0.158~3.16、0.252~5.04、0.100~2.00、0.132~2.64和0.131~2.62μg范围内与峰面积呈良好的线性关系(R^2=0.999 4~1.000 0),且分离度良好,平均加样回收率分别为102.1%、95.53%、100.8%、99.63%、97.48%、101.4%、98.44%和102.6%;10批样品各指标成分的含量分别在0.05%~0.11%、0.01%~0.02%、0.07%~0.23%、0.04%~0.35%、0.07%~0.20%、1.17%~4.25%、0.03%~0.16%和1.68%~5.10%之间。结论:建立的定性和定量方法可用于客观评价丹参茎叶及其产品的品质评价与质量控制,为制定丹参茎叶药材质量标准和开发利用丹参茎叶资源提供了可靠的方法和科学依据。Objective： To establish the quality standard, so as to improve and expand the value of the stems and leaves of Salvia miltiorrhiza collected from the period of flowering to early autumn. Methods： The quality standards were established based on 10 batches of stems and leaves of Salvia miltiorrhiza from nationwide. TLC was adopted to analyze the rutin, isoquercitrin, rosmarinic acid and salvianolic acid B. The silica gel G was adopted as the coating substance and butyl acetate-formic acid-water（ 10 ： 2 ： 3 ） as the mobile phase. The total ash and acid- insoluble ash were determined according to the method that included in the appendix of Chinese pharmacopoeia （ 2015 ）. HPLC was used for quantitative determination of danshensu, protocateehuic aldehyde, caffeic acid, rutin, isoquereitrin, rosmarinic acid, lithospermic acid and salvianolie acid B. The HPLC was performed using Grace Apollo C18 （4.6 mm x 250 mm, 5 p, m ）column with gradient elution of acetonitrile-water with 0. 1% formic acid as the mobile phase （0-5 rain, 10%A; 5-10 rain, 10%A→ 12%A; 10-20 min, 12%A - 14%A; 20-25 rain, 14%A → 20%A ; 25-60 min, 20%A → 30%A ; 60-65 min, 30%A → 40%A ）. The flow rate was 1.0 mL· min^-1, and the UV detection was at 280 nm and 256 nm. Results： TLC was added and its spots of the rutin, isoquereitrin, rosmarinic acid and salvianolic acid B were fairly and simply identical. The content of the total ash and the acidinsoluble ash were 7.14%-9.86% and 0. 06%-0. 38% in 10 batches of the stems and leaves of Salvia miltiorrhiza. The concentration of salvianolic acids and flavonoids showed an excellent linear regressions with the determination coefficients （ R2 ） ranging from 0. 999 4 to 1. 000 0, and the calibration ranges adequately covered variations in the amounts of compounds. The precision, repeatability, and stability RSD values of the 8 compounds were all below 3.34%. The overall recoveries lay between 95.53% and 102.6% for the 8 reference compounds, with RSDs less than 3.09%. The content

关 键 词：丹参 茎叶 丹参素 原儿茶醛 咖啡酸 芦丁 异槲皮苷 迷迭香酸 紫草酸 丹酚酸B TLC定性鉴别 灰分检查 HPLC含量测定 中药材资源开发 

分 类 号：R917[医药卫生—药物分析学]