测定天然和栽培缬草根金属元素的微波和干灰化消解-FAAS法

采用微波消化法和马弗炉干灰法处理天然和栽培缬草根样品，火焰原子吸收光谱法连续测定样品中金属元素，分别检出12种和11种元素，其中Zn、Cu、Fe、Co、Mn、Ni、Cr为生命必需微量元素；两种样品各用两种消化法处理，测得金属元素及含量有差异，干灰法操作简单，但消化温度高、时间长、易挥发、元素容易损失，使检测值偏低；而微波消化法简便、省时、损失减少；两种消化法的加标回收率分别为95％-100％和96％-105％。     

Natural Xanthine Oxidase Inhibitor 5-O-Caffeoylshikimic Acid Ameliorates Kidney Injury Caused by Hyperuricemia in Mice

Xanthine oxidase (XOD) inhibition has long been considered an effective anti-hyperuricemia strategy. To identify effective natural XOD inhibitors with little side effects, we performed a XOD inhibitory assay-coupled isolation of compounds from Smilacis Glabrae Rhizoma (SGR), a traditional Chinese medicine frequently prescribed as anti-hyperuricemia agent for centuries. Through the in vitro XOD inhibitory assay, we obtained a novel XOD inhibitor, 5-O-caffeoylshikimic acid (#1, 5OCSA) with IC₅₀ of 13.96 μM, as well as two known XOD inhibitors, quercetin (#3) and astilbin (#6). Meanwhile, we performed in silico molecular docking and found 5OCSA could interact with the active sites of XOD (PDB ID: 3NVY) with a binding energy of −8.6 kcal/mol, suggesting 5OCSA inhibits XOD by binding with its active site. To evaluate the in vivo effects on XOD, we generated a hyperuricemia mice model by intraperitoneal injection of potassium oxonate (300 mg/kg) and oral gavage of hypoxanthine (500 mg/kg) for 7 days. 5OCSA could inhibit both hepatic and serum XOD in vivo, together with an improvement of histological and multiple serological parameters in kidney injury and HUA. Collectively, our results suggested that 5OCSA may be developed into a safe and effective XOD inhibitor based on in vitro, in silico and in vivo evidence.     

Capillary electrophoresis determination of six bioactive constituents in San-huang-hsieh-hsin-tang

A capillary electrophoretic method for simultaneous determination of six bioactive ingredients (berberine, palmatine, baicalin, sennoside B, emodin, and sennoside A) in the Chinse herbal formula San-huang-hsieh-hsin-tang was established. A carrier composed of aqueous buffer solution (50 mM sodium cholate, 15 mM sodium dihydrogen phosphate, and 4.25 mM sodium borate)-acetonitrile (3:2) was found to be the most suitable electrolyte for this separation. Contents of these constituents in a non-pretreated methanol-water extract of San-huang-hsieh-hsin-tang sample could be easily determined within 20 min. The effects of borate, cholate, and organic modifier (acetonitrile) concentration of the carrier on the migration behavior of the solutes were also studied.     

川芎浓缩颗粒挥发性成分分析

采用气相色谱－质谱法对川芎浓缩颗粒挥发性成分进行分离鉴定。从水蒸气蒸馏法工艺制备的浓缩颗粒（样品I）中分离鉴定了12个成分,主要为亚油酸、棕榈酸;从超临界CO2流体萃取工艺制备的浓缩颗粒（样品Ⅱ）中分离鉴定了32个成分,主要为藁本内酯、亚油酸。用面积归一化测定了样品Ⅰ、Ⅱ中成分的相对百分含量。     

源于中药选择性效应的新型免疫抑制疗法

近年来免疫学的发展日新月异,但与其他系统药物相比,免疫系统药物的发展十分落后。低选择性是现有免疫抑制剂的重要缺陷,这使得需要长期用药的自身免疫性疾病常因药物的严重副作用而使治疗无法持续。因此,免疫系统药物的研制必须另辟蹊径。本文在阐述免疫抑制剂发展现状的基础上,通过本课题组关于中药及其成分的研究结果,提出了选择性抑制活化T细胞的免疫抑制新模式,从作用特点、作用机理、代谢产物以及与现有免疫抑制剂的比较等角度论证了选择性免疫抑制的可行性,从而为免疫性疾病的治疗以及新型免疫抑制剂的研制提供新的思路。     

高效液相色谱法同时测定中药材虎掌南星的核苷类成分

建立了高效液相色谱同时测定中药材虎掌南星中核苷类活性成分(腺嘌呤、次黄嘌呤、黄嘌呤、尿苷、胸腺嘧啶、腺苷、鸟苷)含量的方法。以Lichrospher C18色谱柱(150 mm×4.6 mm, 5 μm)分离,以乙腈-水(含0.1%甲酸)为流动相,梯度洗脱,在254 nm下检测,腺嘌呤、次黄嘌呤、黄嘌呤、尿苷及鸟苷分别在1.6～50 mg/L范围内、胸腺嘧啶和腺苷分别在1.2～40 mg/L范围内的线性关系良好,相关系数均大于0.9995,加标回收率为98.9%～101.2%,相对标准偏差均小于3%。方法学考察结果显示符合含量测定要求,并应用于不同产地虎掌南星的测定。该方法操作简便、快速,结果可靠,重现性好,可作为虎掌南星质量评价的参考依据。     

毛细管电泳电化学检测法测定胡黄连中香草酸和阿魏酸的含量

采用毛细管电泳电化学检测法测定了胡黄连中香草酸和阿魏酸的含量 ;研究了电极电位、运行缓冲液的浓度和酸度、电泳电压及进样时间等对电泳的影响 ,得到了最优化的测定条件 ;以直径为300μm的碳圆盘电极为检测电极 ,工作电极电位为0.8V(vs.SCE) ,在50mmol/L硼砂(pH8.4)运行缓冲液中 ,上述两组分在8min内完全分离 ;香草酸和阿魏酸线性范围分别为5×10-4～1×10-6 mol/L和1×10-3～1×10-6 mol/L ,检出限分别为4.2×10 -7和3.0×10 -7mol/L ;7次平行进样的相对标准偏差(RSD)为2.2 %和2.8 % ,回收率(n=3)分别为99%和103 % ,该法灵敏可靠 ,结果令人满意。     

中药药对的化学成分研究川芎-赤芍挥发油的GC/MS分析

中药药对是复方的最小组成单位,具有中药配伍的基本特点. 药对化学是复方化学的核心内容. 联用色谱和化学计量学方法为中药复杂体系的分离与分辨提供了强有力的工具. 采用GC-MS法分离测定中药药对川芎-赤芍、 单味药川芎和赤芍的挥发油成分,并对其中的重叠色谱峰采用化学计量学解析方法(CRM)进行分辨,得到药对和各单味药的纯色谱曲线和质谱图,药对川芎-赤芍、 单味药川芎和赤芍分别分辨出82,78和57个色谱峰,通过质谱库对分辨的纯组分进行定性,分别得到61,52和33个定性结果,占总含量的90.18%,95.14%和95.82%.     

白术挥发性成分的超临界流体萃取及其分析

采用超临界流体萃取白术挥发油成分,对萃取条件进行优化,并用气相色谱、气相色谱－质谱分析鉴定出超临界流体萃了的挥发油中22个化合物。最佳的超临界流体萃取条件为压力22.0MPa,温度60℃,0.5mL乙醇作改性,先静态萃取10min(CO2用量2.0mL),再动态萃取40min(CO2流速为0.3mL/min)。将超临界流体萃取与水蒸气蒸馏进行对比,水蒸气蒸馏5h的油收率仅为超临界流体萃取1h油收率的10.32%,证明超临界流体萃取替代传统萃取的必要性。