中药白芍的HPLC含量测定及指纹图谱研究

建立白芍商品药材指纹图谱,并测定芍药苷含量评价药材质量。采用高效液相色谱分析,HypersilODS C18柱(4.6mm×250mm,5μm),乙腈-0.08%磷酸溶液梯度洗脱,柱温30℃。测定了市售17批白芍药材的HPLC指纹图谱,建立了白芍药材的总共有模式,计算得到各批药材的相似度,其中8批药材的相似度介于0.902—0.985。以相似度0.90为界,大于0.90认定为合格药材,小于0.90为不合格药材。本评价方法的结果与根据药典标准的划分结果一致,但更直观,可操作性更强,尤其对白芍药材中硫化物进行有效监控,还可对熏硫药材的质量控制起到示范作用。     

徐长卿中药中丹皮酚含量的测定

采用紫外分光光度法测定了徐长卿中药中丹皮酚的含量。丹皮酚在1—8μg/mL具有良好的线性关系,徐长卿中丹皮酚含量为0.9676%,平均加标回收率为101.21%。该方法简便、快捷、准确、重现性好,可作为检测徐长卿中丹皮酚含量的一种好方法。     

Exploring the In Vivo Existence Forms (23 Original Constituents and 147 Metabolites) of Astragali Radix Total Flavonoids and Their Distributions in Rats Using HPLC-DAD-ESI-IT-TOF-MSn

Astragali Radix total flavonoids (ARTF) is one of the main bioactive components of Astragali Radix (AR), and has many pharmacological effects. However, its metabolism and effective forms remains unclear. The HPLC-DAD-ESI-IT-TOF-MSⁿ technique was used to screen and tentatively identify the in vivo original constituents and metabolites of ARTF and to clarify their distribution in rats after oral administration. In addition, modern chromatographic methods were used to isolate the main metabolites from rat urine and NMR spectroscopy was used to elucidate their structures. As a result, 170 compounds (23 original constituents and 147 metabolites) were tentatively identified as forms existing in vivo, 13 of which have the same pharmacological effect with ARTF. Among 170 compounds, three were newly detected original constituents in vivo and 89 were new metabolites of ARTF, from which 12 metabolites were regarded as new compounds. Nineteen original constituents and 65 metabolites were detected in 10 organs. Four metabolites were isolated and identified from rat urine, including a new compound (calycoisn-3’-O-glucuronide methyl ester), a firstly-isolated metabolite (astraisoflavan-7-O-glucoside-2’-O-glucuronide), and two known metabolites (daidzein-7-O-sulfate and calycosin-3’-O-glucuronide). The original constituents and metabolites existing in vivo may be material basis for ARTF efficacy, and these findings are helpful for further clarifying the effective forms of ARTF.     

Anti-hypertensive effects of Radix Rehmanniae and its active ingredients

Abstract

Radix Rehmanniae (RR) is the root tuber of Rehmannia glutinosa Libosch. Herein, the methanol extracts of dried RR (DRR) and processed RR (PRR) were partitioned to obtain ethyl acetate, aqueous, and n-butanol layers. The angiotensin-I converting enzyme (ACE) inhibition test indicated that the ethyl acetate extracts of DRR (DRRE) and PRR (PRRE) show better inhibitory activity. Therefore, changes in blood pressure were tested over 24?h in spontaneously hypertensive rats, with DRR showing good anti-hypertensive activity. DRRE was further subjected to column chromatography; 28 fractions were separated and tested for ACE inhibition. Ultimately, six compounds were identified by spectral analysis, and literature comparison. Specifically, ursolic acid and oleanolic acid showed better ACE inhibition than the other compounds. This study confirmed that DRR has anti-hypertensive activity. In future, DRR’s potential as a health food should be further assessed.     

Simultaneous determination of main phytoecdysones and triterpenoids in radix achyranthis bidentatae by high-performance liquid chromatography with diode array-evaporative light scattering detectors and mass spectrometry

A liquid chromatographic method was developed for simultaneous determination of two main types of bioactive compounds: four phytoecdysones and eight triterpenoids in Radix Achyranthis Bidentatae (RAB), i.e., polypodine B (1), ecdysterone (2), 25-R inokosterone (3), 25-S inokosterone (4), ginsenoside Ro (5), chikusetsusaponin IVa (6), zingibroside R₁ (7), chikusetsusaponin IVa ethyl ester (8), 28-deglucosyl-chikusetsusaponin IVa (9), PJS-1 (10), 28-deglucosyl-chikusetsusaponin IVa butyl ester (11), and oleanolic acid (12). Optimum separations were obtained with a Zorbax C18 column, using a gradient elution with 0.08% aqueous formic acid (containing 5% isopropyl alcohol) and acetonitrile as mobile phase. Phytoecdysones were detected by diode array detector (DAD) at 242 nm, whereas triterpenoids were monitored by evaporative light scattering detector (ELSD) connected in series with DAD, temperature for the drift tube was 110 °C and the nitrogen flow rate was 3.2 L min⁻¹. The identity of the analytes was confirmed using retention times, ultraviolet absorbance and mass spectral data in comparison with reference compounds. The method was validated for acceptable precision (intra- and inter-day variation ≤ 4.87%), accuracy (recovery ≥ 88.9%) and sensitivity (LOD ≤ 0.43 μg mL⁻¹ (DAD) and 26.0 μg mL⁻¹ (ELSD), LOQ ≤ 0.97 μg mL⁻¹ (DAD) and 46.5 μg mL⁻¹ (ELSD), respectively). This rapid and reliable method was applied for the analysis of four cultivated and ten commercial samples. The results demonstrated that the method is suitable for routine analysis and quality control of RAB.     

黄芩中微量元素的模糊数学处理及正品黄芩的识别

采用模糊数学方法处理中药黄芩的微量元素数据，对１０个不同产地的黄芩样品进行了分类，获得了满意的结果。     

生地熟地中矿物元素的测定与分析

用原子吸收光谱法,对生地熟地中镁、铜、锌、铁、锰、镉、钴7种矿物元素进行了测定,发现生地与熟地中Fe的含量都很高,熟地的补血作用可能与Fe元素的存在形态发生变化有关,使更多的Fe^3＋与血浆转铁蛋白结合。另外,AAS法具有良好的准确度和精确度,测定结果准确、可靠。测定结果可为以后生地、熟地中矿物元素与药效间的关系以及新药的开发、研制等奠定一定的理论基础。     

白芷的提取工艺

探讨多因素实验条件对白芷的提取工艺参数的影响,以欧前胡素和异欧前胡素的含量为指标,以乙醇浓度、乙醇用量、提取时间、提取次数为因素进行单因素试验。结果表明,白芷的最佳提取工艺参数为:以8倍量80%乙醇提取3次,每次lh。     

基于全二维气相色谱-四极杆飞行时间质谱高通量检测独活挥发油化学成分

利用全二维气相色谱-四极杆飞行时间质谱(GC×GC-QTOF MS)建立了一种适用于独活挥发油化学成分的高通量检测方法,样品经水蒸气蒸馏提取后,直接采用全二维气相色谱进行分离,并根据谱库匹配、保留指数及精确质量数进行定性确认.结果表明,共分离鉴定了独活挥发油中207种化学成分,其中正向、反向匹配因子大于800的化合物占...     

广东土牛膝超临界流体萃取物的 GC-MS分析

采用GC－MS技术,对广东土牛膝的超临界流体萃取物中的化学成分进行了分析。气相色谱分离出77种组分,鉴定出其中32种化合物,主要为萜类物质（大部分为倍半萜）、有机酸及其酯类、酚类等化合物。