丹参茎叶酚酮有效部位的提取纯化工艺研究

目的对丹参茎叶酚酮有效部位提取纯化工艺进行优选。方法采用超高效液相色谱仪检测,以丹参茎叶中酚酸类(丹参素、原儿茶酸、原儿茶醛、咖啡酸、丹酚酸B、迷迭香酸、紫草酸)及黄酮类成分(芦丁、异槲皮苷、山柰酚-3-O-芸香糖苷、紫云英苷)二者提取量、总提取量及浸膏得率为评价指标,通过单因素及正交试验考察提取方法、提取溶剂、料液比、提取时间及提取次数对丹参茎叶提取工艺的影响;采用大孔吸附树脂纯化丹参茎叶提取物并对纯化工艺参数进行考察,确定最佳纯化工艺。结果以50%乙醇8倍量回流提取3次,每次提取1.0 h为最佳提取工艺;以AB-8型大孔吸附树脂纯化,1.0 g/m L药液上样,上样量为每10克干树脂上样1.5 g干燥提取物,40%乙醇洗脱,洗脱用量3 BV为最佳纯化工艺,酚酸类及黄酮类成分总纯度可达到41.83%。结论优选的提取工艺稳定可行,适用于丹参茎叶酚酮有效部位的提取纯化,可为丹参茎叶的进一步开发提供参考。     

HPLC-DAD同时测定丹参中原儿茶醛、丹酚酸B、隐丹参酮、丹参酮IIA四种成分的含量

目的:研究丹参指纹图谱全貌并同时测定不同种植地区、不同采摘批次丹参药材中的活性成分原儿茶醛、丹酚酸B、隐丹参酮及丹参酮IIA的含量,研究新的丹参质量控制指标。方法:本文针对不同批次丹参采用高效液相色谱及紫外-可见光二极管阵列检测器联用技术(HPLC-DAD),以乙腈-水(含0.026%磷酸)为流动相进行梯度洗脱,检测波长270nm,柱温24℃。结果:10个批次丹参提取液中,原儿茶醛浓度在0.375~6μg.mL-1,丹酚酸B浓度在65~390μg.mL-1,隐丹参酮浓度在2.2~22μg.mL-1,丹参酮IIA浓度在2.5~25μg.mL-1范围内呈良好的线性关系。原儿茶醛的含量为0.00124%~0.00205%,丹酚酸B的含量为7.26%~9.94%,隐丹参酮的含量为0.190%~0.568%,丹参酮IIA含量为0.512%~1.252%。结论:应用HPLC-DAD法同时对丹参中原儿茶醛、丹酚酸B、隐丹参酮及丹参酮IIA的测定结果准确可靠,可同时将它们作为丹参的质量控制指标。     

HPLC法测定滑膜炎颗粒中原儿茶醛的含量

目的建立滑膜炎颗粒剂中原儿茶醛的含量测定方法质量。方法采用高效液相色谱法对方中原儿茶醛进行含量测定。结果高效液相色谱法测定结果表明原儿茶醛在0．1005～1．005μg范围内呈线性关系，平均加样回收率为99．22％；RSD为0．72％。结论本法简便，重现性好、结果可靠，可作为控制滑膜炎颗粒剂的质量方法。     

HPLC同时测定通脉颗粒中丹参素、原儿茶醛、丹酚酸B、阿魏酸和葛根素的含量

目的 建立通脉颗粒中丹参素、原儿茶醛、丹酚酸B、阿魏酸和葛根素的HPLC测定方法。方法 采用Welch Ultimate XD-C₁₈色谱柱（4.6 mm×250 mm,5 μm）,以乙腈-0.1%三氟乙酸为流动相,梯度洗脱,双波长检测（282,305 nm）,柱温35℃,流速1.0 mL·min^-1。结果 丹参素、丹酚酸B、原儿茶醛、葛根素和阿魏酸的线性范围分别为3.117~62.33 μg·mL^-1（r=0.998 7）,4.044~80.88 μg·mL^-1（r=0.9985）,1.280~25.60 μg·mL^-1（r=0.997 9）,7.964~159.3 μg·mL^-1（r=0.992 8）,1.980~39.60 μg·mL^-1（r=0.999 1）;平均回收率分别为101.6%（RSD=1.62%）,99.7%（RSD=1.76%）,97.4%（RSD=1.19%）,99.9%（RSD=1.52%）,102.2%（RSD=1.56%）。结论 该方法操作简便、快速,结果准确,可用于通脉颗粒的质量控制。     

Effect of protocatechualdehyde,a metabolite of the novel antirheumatic agent ACP,on chondrocyte metabolism

We investigated PAL (protocatechualdehyde), one of the metabolites of ACP (3,4-diacetoxy benzylidene diacetate) which is a candidate novel antirheumatic agent. Specifically, we studied the effect and mechanism of action of PAL on chondrocyte metabolism using a primary culture of chondrocytes from rabbit articular cartilage. Proteoglycan (PG) depletion in the chondrocyte matrix was induced by the addition of human recombinant interleukin-1α (hrlL-1α) or phorbol myristate acetate (PMA). PAL (10–100 μM) significantly reduced the induced PG depletion and [³⁵S]-PG release in the chondrocyte matrix. The matrix metalloproteinase (MMPs) inhibitor, 1,10-phenanthroline, and protein kinase C (PKC) inhibitor, H-7, also blocked PG depletion and [³⁵S]-PG release. Furthermore, H-7 reduced the production of MMPs induced by hrlL-1α in the culture media of chondrocytes. These results indicate that hrlL-1α causes MMPs production by the activation of PKC, which is followed by [³⁵S]-PG release in the chondrocyte matrix. While PAL also resulted in significant inhibition of MMPs production, which might be mediated by PKC activation, it had no direct influence on PKC activity. These results suggest that PAL affects chondrocyte metabolism by the inhibition of MMPs production. ©1993 Wiley-Liss, Inc.     

高效毛细管电泳法同时测定丹参饮片中5种酚酸类成分

 目的 建立高效毛细管电泳法同时测定丹参饮片中迷迭香酸、原儿茶醛、丹参素、丹酚酸B、丹酚酸A含量的方法,同时考察丹参药材适宜干燥温度。方法 10 mmol·L^-1硼酸-12 mmol·L^-1磷酸二氢钠-10 mmol·L^-1SDS为电泳介质,未涂渍标准熔融石英毛细管(75 μm×64.5 cm,有效长度56 cm)为分离通道,分离电压为18 kV,检测波长为206 nm,毛细管温度为20 ℃,压力进样:5 kPa×6 s。结果 5种指标成分的浓度与峰面积的线性关系良好(r>0.999 0);干燥温度以100 ℃为宜。结论 该方法简单、准确,重复性较好,可用于丹参饮片的质量评价和控制。     

RP-HPLC法测定软肝颗粒中原儿茶醛的含量

目的采用反相高效液相色谱法测定软肝颗粒中原儿茶醛的含量。方法采用十八烷基硅烷键合硅胶柱;流动相:甲醇—1%醋酸溶液(12∶88),检测波长为279nm;流速为1.0mL.min-1。结果原儿茶醛线性范围0.0552~0.2208μg,平均回收率为99.9%,RSD=0.5%。结论方法简便,结果准确,能有效控制软肝颗粒的质量。     

反相高效液相色谱法测定舒乳消痛口服液中原儿茶酸和原儿茶醛的含量

目的:建立舒乳消痛口服液中原儿茶酸、原儿茶醛的高效液相色谱测定方法.方法:采用Shim-pack CLC-ODS柱,流动相:甲醇-水-冰醋酸(40:96:0.25),检测波长:280 nm.结果:原儿茶酸线性范围为20.0～100.0 mg·L-1,平均加样回收率98.97%;RSD为1.24%(n=5).原儿茶醛线性范围为6.0～30.0 mg·L-1,平均加样回收率为96.75%;RSD为0.94%(n=5).结论:实验方法简便,结果准确,可用于该制剂的质量控制.     

Synthesis of [uniformly ring‐14C]‐labelled 4‐hydroxybenzaldehyde,vanillin, and protocatechualdehyde

[Uniformly ring‐¹⁴C]‐labelled 4‐hydroxybenzaldehyde, vanillin, and protocatechualdehyde were synthesized from [¹⁴C]‐labelled phenol, guaiacol, and catechol with methyl dichloromethyl sulfide (CH₃SCHCl₂) under Friedel–Crafts alkylation conditions in dichloromethane at ?78°C for 5 min (in the case of phenol and guaiacol) or at ?20°C for 1 min (in the case of catechol), by rapid addition of SnCl₄ to mixtures of the phenolic compound and CH₃SCHCl₂, followed by hydrolysis with HCl. Regioselective formylation (para to the –OH group) was achieved. The conversion rates were 96, 81, and 88% for 4‐hydroxybenzaldehyde, vanillin, and protocatechualdehyde, respectively, and the yields of the recovered products after work‐up amounted to 88, 75, and 83%, respectively. In the case of guaiacol, 17% of isovanillin was obtained as by‐product. It was found that the presence of water or ethyl acetate in the reaction mixture, at a molar ratio of 60:1 (water:guaiacol) or 120:1 (ethyl acetate:guaiacol), had little influence on the yields under the reaction conditions. Factors influencing the yields are discussed in the study. Copyright © 2004 John Wiley & Sons, Ltd.     

丹七片HPLC指纹图谱

目的:采用高效液相色谱法建立丹七片的指纹图谱。方法:资生堂CAPCELL PARK C18色谱柱(4.6 mm×250mm,5μm),流动相乙腈-0.06%磷酸溶液(梯度洗脱),检测波长210 nm,柱温30℃,流速为1.0 mL·min-1。采用"中药色谱指纹图谱相似度评价系统(2004A)"对10批丹七片指纹图谱进行分析。结果:10批丹七片的HPLC指纹图谱有15个共有峰,确认了其中7个色谱峰的成分分别为丹参素钠、原儿茶醛、迷迭香酸、紫草酸、人参皂苷Rg1、丹酚酸B和人参皂苷Rb1,相似度>0.990。结论:该法操作简便,精密度、重复性和稳定性良好,为丹七片的质量控制提供了有效手段。