四妙勇安汤中甘草苷、金丝桃苷和木犀草苷提取率的拆方分析

目的研究四妙勇安汤的配伍组合对甘草苷、金丝桃苷和木犀草苷提取率的影响。方法将四妙勇安汤拆方,采用HPLC法,SunfireTMC18色谱柱(4.6 mm×150 mm,5μm),流动相为乙腈-0.1%磷酸等梯度洗脱,流速1.0 m L/min,检测波长276 nm(甘草苷)、350 nm(金丝桃苷、木犀草苷),柱温35℃,分析各组合样品中甘草苷、金丝桃苷和木犀草苷含量并计算提取率。结果与单味药相比,配伍药味越多,甘草苷、金丝桃苷和木犀草苷的提取率越高,全方合煎后,3种成分提取率均达到最高。结论配伍可以明显提高四妙勇安汤中甘草苷、金丝桃苷和木犀草苷的提取率,从化学成分提取率角度验证了复方配伍的科学性和合理性,阐明了中药复方配伍的科学内涵。     

中药复方有效成分群在陶瓷膜分离过程中的迁移研究

目的以复方板蓝根利咽颗粒(板蓝根、玄参、桔梗、甘草等)水提液为研究对象,探讨中药复方有效成分群在不同孔径陶瓷膜分离过程中的动态迁移规律,并比较其膜滤通量、固含物去除率。方法分别以200 nm和50 nm孔径陶瓷膜对复方板蓝根利咽颗粒水提液进行分离精制,连续多次取样,优化的HPLC法为Agilent Zorbox Eclipse XDB-C18色谱柱,乙腈-0.05%磷酸水溶液梯度洗脱,检测波长采用切换波长,体积流量1 m L/min,柱温30℃,进样量10μL,同时测定复方中腺苷、(R,S)-告依春、甘草苷、哈巴俄苷、桔梗皂苷D和甘草酸铵6种有效成分,考察其动态迁移率。结果 HPLC法可以同时测定复方中6种有效成分,对于复方板蓝根利咽颗粒水提液,在200 nm陶瓷膜分离过程中,6种有效成分的动态迁移率波动范围在71%~104%,平均迁移率85%,膜滤通量衰减较小,稳定通量在426~340 L/(m2·h),固含物去除率21.0%。在50 nm陶瓷膜中,6种有效成分的动态迁移率波动范围在83%~107%,平均迁移率83%,膜滤通量衰减较大,稳定通量在258~228 L/(m2·h),固含物去除率23.9%。结论初步探讨了中药复方有效成分群在2种不同孔径陶瓷膜分离过程的动态迁移情况,为现代陶瓷膜技术在中药精制中的推广应用奠定药效物质迁移理论基础。     

参术益肠丸普通粉体和超微粉体溶出行为比较研究

目的比较参术益肠丸细粉和超微粉中主要活性成分葛根素、芍药苷和甘草苷溶出情况,为其生产工艺优化提供实验依据。方法采用高效液相色谱法分别对参术益肠丸中主要活性成分在不同溶出介质中相对累积溶出率进行定量研究。色谱条件:Agilent Eclipse XDB-C18色谱柱(150 mm×4.6 mm,5μm);流动相为乙腈-0.1%磷酸水溶液(11︰89);体积流量1.5 m L/min;检测波长230 nm;进样量10μL。结果细粉中葛根素和甘草苷在水和人工胃液中相对累积溶出率大于超微粉,而细粉中芍药苷在水和人工胃液中相对累积溶出率小于超微粉。人工肠液中超微粉和细粉的溶出行为相似。结论适度的微粉化能促进参术益肠丸有效成分的溶出,其溶出行为还受到不同溶出介质的影响,超微粉碎技术应用于参术益肠丸还需进一步研究。     

Pharmacokinetic interaction of aconitine,liquiritin and 6-gingerol in a traditional Chinese herbal formula,Sini Decoction

1.?This study aimed to investigate the pharmacokinetic interaction of the three ingredients in a traditional Chinese herbal formulation, Sini Decoction, and provide evidence for its compatibility mechanism.

2.?First, the effect of liquiritin and 6-gingerol on the pharmacokinetic parameters of aconitine was investigated in rats by using a sensitive and reliable LC–MS/MS method. Then the Caco-2 cell monolayer model and Rhodamine-123 uptake assay were used to investigate the effect of liquiritin and 6-gingerol on the absorption of aconitine and the activity of P-gp.

3.?The C_max of aconitine increased significantly (p?liquiritin (20?mg/kg), and to 17.43?±?0.96?ng/mL with 6-gingerol (20?mg/kg). When aconitine was co-administered with liquiritin and 6-gingerol, the C_max and AUC_(0–t) of aconitine increased approximately twofold, and while t_1/2 only increased 1.2-fold. The Caco-2 cell monolayer model and Rhodamine-123 uptake assay indicated that both liquiritin and 6-gingerol could increase the absorption of aconitine by inhibiting the activity of P-gp.

4.?These results indicated that both liquiritin and 6-gingerol could promote the absorption of aconitine and increase its drug concentration in blood by inhibiting the activity of P-gp, and it could also provide evidence for compatibility mechanism of the traditional Chinese herbal formula, Sini Decoction.     

HPLC-DAD法测定银屑优化颗粒中芍药苷、甘草苷、落新妇苷、迷迭香酸和甘草酸

目的建立同时测定银屑优化颗粒中芍药苷、甘草苷、落新妇苷、迷迭香酸和甘草酸5种成分的HPLC-DAD测定方法。方法采用高效液相色谱波长切换法。Lichrospher C18色谱柱(250 mm×4.6 mm,5μm);流动相为乙腈–0.1%磷酸溶液,梯度洗脱;检测波长在230、254、290 nm切换;体积流量为1 mL/min;柱温为30℃;进样体积10μL。结果 5种成分的线性关系良好。芍药苷在69.12~691.20 ng线性关系良好,平均加样回收率为97.45%,RSD值为1.54%;甘草苷在39.02~390.20 ng线性关系良好,平均加样回收率为97.10%,RSD值为1.90%;落新妇苷在30.03~300.30 ng线性关系良好,平均加样回收率为99.98%,RSD值为1.22%;迷迭香酸在7.82~78.20 ng线性关系良好,平均加样回收率为100.83%,RSD值为1.36%;甘草酸在31.09~310.90 ng线性关系良好,平均加样回收率为97.52%,RSD值为1.49%。结论本方法具有方法简便、快速、准确等特点,可同时测定银屑优化颗粒中5种活性成分。     

UPLC测定银翘散中的多指标性成分

目的: 建立UPLC同时测定银翘散中绿原酸、甘草苷、橙皮苷、牛蒡子苷、连翘苷含量的方法. 方法: 采用UPLC系统,ACQUITY UPLC BEH Shield RP18色谱柱(2.1 mm×50 mm,1.7 μm),甲醇-0.15%甲酸溶液梯度洗脱,流速0.25 mL·min^-1,检测波长279 nm,柱温40 ℃,同时测量5种活性成分的含量. 结果: 绿原酸、连翘苷、牛蒡子苷、橙皮苷、甘草苷分别在0.018 76~0.043 77,0.002 37~0.011 85,0.011 21~0.056 06,0.001 34~0.006 71,0.001 71~0.012 38 μg线性关系良好(r≥0.999 1),平均回收率分别为97.12%(RSD 0.9%),101.40%(RSD 2.1%),100.61%(RSD 1.6%),100.79%(RSD 0.7%),101.04% (RSD 1.7%). 结论: 该方法简便、快速、专属性强,可用于银翘散的质量控制.     

高效液相色谱法同时测定加味藿香正气软胶囊中橙皮苷、厚朴酚、和厚朴酚和甘草苷的含量

目的：建立高效液相色谱法同时测定加味藿香正气软胶囊中橙皮苷、厚朴酚、和厚朴酚和甘草苷的方法。方法：采用Kromasil C18色谱柱（250 mm×4.6 mm,5 μm）,以水-甲醇为流动相梯度洗脱,流速1.0 mL·min-1,检测波长287 nm。结果：橙皮苷、厚朴酚、和厚朴酚、甘草苷分别在4.47-178.70 μg·mL-1、3.42-136.96 μg·mL-1、3.49-139.48 μg·mL-1、3.92-157.20 μg·mL-1 范围内与峰面积呈良好线性关系（r=0.999 9）,平均回收率分别为99.48%、99.05%、99.57%、99.79%。结论：该方法准确、灵敏、专属性强,为加味藿香正气软胶囊质量标准提高奠定了基础。     

HPLC 法同时测定甘草及甘草头中4 种成分含量

目的：建立HPLC 法同时测定甘草饮片及甘草头中甘草苷、异甘草苷、甘草素和甘草酸的含量。方法：采用Diamonsil C18 色谱柱（250 mmx4.6 mm,5 μm）,0.1%磷酸水-乙腈梯度洗脱,流速1.0 mL·min-1,检测波长为276 nm（0~18 min）、360 nm（18~24 min）、276 nm（24~30 min）、250 nm（30~65 min）,柱温30℃。结果：在该色谱条件下,甘草苷、异甘草苷、甘草素、甘草酸的进样量分别在0.108 5~1.085、0.016 8~0.168、0.004 94~0.049 4、0.407~4.07 μg 范围内线性关系良好。加样回收率均在96.61%~100.89%,RSD 值均小于0.81%。5 个不同批次的甘草饮片中4 种成分的含量分别为0.513%、0.072 9%、0.048 4%、1.945%;2个批次甘草头中4 种成分含量分别为0.456%、0.063 6%、0.036 2%、1.630%。结论：4 种成分的响应与浓度之间呈良好的线性关系;甘草头中4 种成分的含量与甘草饮片基本相当,可作为活性成分提取的原料加以利用。     

Neuroprotective effect of liquiritin against focal cerebral ischemia/reperfusion in mice via its antioxidant and antiapoptosis properties

Our present study was conducted to investigate whether liquiritin (7-hydroxy-2-[4-[3,4,5-trihydroxy-6-(hydroxymethyl) oxan-2-yl] oxyphenyl]-chroman-4-one, 1), an active component of Glycyrrhiza uralensis Fisch., exerts a neuroprotective effect against focal cerebral ischemia/reperfusion (I/R) in male Institute of Cancer Research (ICR) mice. On the establishment of mice with middle cerebral artery occlusion (MCAO) for 2 h and reperfusion for 22 h, liquiritin at the doses of 40, 20, and 10 mg/kg was administered before MCAO once a day intragastrically for a subsequent 3 days. Neurological deficits and infarct volume were measured, respectively. The levels of malondialdehyde (MDA) and carbonyl, activities of superoxide anion (SOD), catalase (CAT) and glutathion peroxidase (GSH-Px) and reduced glutathione/oxidized disulfide (GSH/GSSG) ratio in brain were estimated spectrophotometrically. 8-Hydroxy-2′-deoxyguanosine (8-OHdG) and terminal deoxynucleotidyl transferase-mediated DuTP-biotin nick end labeling (TUNEL)-positive cells were detected by immunohistochemical analysis. Our results showed that the neurological deficits, infarct volume, and the levels of MDA and carbonyl decreased, the ratio of GSH/GSSG and the activities of SOD, CAT, and GSH-Px were compensatorily up-regulated, and 8-OHdG and TUNEL-positive cells decreased after 22 h of reperfusion in liquiritin-treated groups. These findings suggest that liquiritin might be a potential agent against cerebral I/R injury in mice by its antioxidant and antiapoptosis properties.     

神曲制备过程中配料比考察

目的：考察不同溶剂和提取方式对酸碱配伍药对中有效成分提取率的影响。方法：选择黄连-甘草药对为研究对象,以水和75%乙醇为提取溶剂,提取方式包括混合或单独煎煮与回流,考察不同溶剂和提取方式对黄连-甘草药对中有效成分提取率的影响。采用RP-HPLC测定甘草酸及甘草苷、盐酸小檗碱含量,流动相分别为乙腈（A）-0.05%磷酸溶液（B）梯度洗脱（0~8 min,19%A;8~35 min,19%~50%A;35~36 min,50%~100%A;36~40 min,100%~19%A）和乙腈-0.05 mol·L^-1磷酸二氢钾溶液（50：50）,检测波长依次为237,345 nm。结果：以盐酸小檗碱为指标,提取率排序为混合乙醇回流（100.0%）>单独乙醇回流（98.2%）>单独水煎（80.3%）>混合水煎（54.6%）;以甘草酸为指标,提取率排序为混合乙醇回流（100.7%）>单独水煎（99.8%）>单独乙醇回流（97.8%）>混合水煎（69.0%）;以甘草苷为指标,提取率排序为混合乙醇回流（98.5%）>单独乙醇回流（93.6%）>单独水煎（91.3%）>混合水煎（66.9%）。混合醇提液减压回收乙醇会产生大量沉淀,经水洗涤后,小檗碱、甘草酸、甘草苷转移率均>88%。结论：溶剂和提取方式对黄连-甘草药对中有效成分提取率影响较大,提示含酸碱药对的方剂在临床汤剂应用中更适合分开提取,而工业生产中以乙醇提取为最佳。