Two new noroleanane-type triterpenoid saponins from the stems of Stauntonia chinensis

Two new noroleanane-type triterpenoid saponins, 3β,20α,24-trihydroxy-29-norolean-12-en-28-oic acid 24-O-β-L-fucopyranosyl-(1→2)-[β-D-xylopyranosyl-(1→3)]-β-D-glucopyranoside (1) and 3β,20α,24-trihydroxy-29-norolean-12-en-28-oic acid 24-O-β-D-glucopyranosyl-(1→2)-[α-L-arabinopyranosyl-(1→3)]-β-D-glucopyranoside (2) were isolated from the stems of Stauntonia chinensis DC., together with three known compounds, brachyantheraoside B₂ (3), eupteleasaponin Ⅷ (4) and fargoside B (5). Their structures were elucidated by spectroscopic and chemical methods. The cytotoxic activities of compounds 1 and 2 were evaluated against five human tumor cell lines (HCT-116, HepG2, BGC-823, NCI-H1650, and A2780). Compounds 1 and 2 showed moderate cytotoxic activities toward the tested cell lines with IC₅₀ values ranging from 12.71 to 32.04 μM.     

Application of characteristic fragment filtering with ultra high performance liquid chromatography coupled with high‐resolution mass spectrometry for comprehensive identification of components in Schisandrae chinensis Fructus

An integrated strategy of characteristic fragment filtering combined with target database screening based on ultra‐high‐performance liquid chromatography coupled with high‐resolution mass spectrometry was proposed for comprehensive profiling of components in Schisandrae chinensis Fructus. The strategy consisted of following five steps: (1) Representative standards were analyzed by ultra high performance liquid chromatography coupled with linear ion trap‐Orbitrap mass spectrometer for characteristic fragments and fragmentation rules of each structure type. (2) The raw data of 70% methanol extract was collected by ultra high performance liquid chromatography quadrupole time‐of‐flight tandem mass spectrometry. (3) The chemical components database that consisted of names, chemical formulas and structures of potential components in Schisandrae chinensis Fructus was established by summarizing previous literature to screen the collected liquid chromatography with mass spectrometry data and obtain matched compounds. (4) Characteristic fragments, literature, and reference standards were used to verify the matches. (5) Characteristic fragment filtering combined with online database querying was used to deduce potential new compounds. As a result, a total of 94 compounds were identified or characterized and 16 of them were potential new compounds. The study provided a reference for comprehensive characterization of ingredients in herbal medicine and formed the foundation for pharmacodynamic study of Schisandrae chinensis Fructus.     

开口箭化学成分及抗肿瘤活性

从开口箭新鲜根茎中分离得到8个化合物, 通过理化性质分析、 质谱、 红外光谱及核磁共振波谱检测等方法鉴定了其结构, 分别为开口箭皂苷J(1)、 (25S)-26-O-β-D-吡喃葡萄糖基呋甾-1β,3β,22α,26-四羟基-3-O-β-D-吡喃葡萄糖苷(2)、 洋地黄毒苷元-3-O-α-L-吡喃岩藻糖苷(3)、 弯蕊皂苷元B(4)、 异罗斯考皂苷元(5)、 罗斯考皂苷元(6)、 香豌豆酚(7)及(+)-儿茶素(8). 其中, 化合物1为新化合物, 化合物3, 4, 7和8为首次从该属植物中分离得到. 在抗人结肠癌细胞LoVo和胃癌细胞BGC-823活性评价中, 化合物5和6表现出较强的抗肿瘤活性, 半抑制浓度(IC₅₀)值分别达到0.532和0.757 μmol/L.     

Seconoriridone A: A C16-seco-noriridal derivative with a 5/5/7 tricyclic skeleton from Belamcanda chinensis

Seconoriridone A (1), a novel C₁₆-seco-noriridal with a 5/5/7 tricyclic scaffold, was isolated from the rhizome of Belamcanda chinensis. Its structure and absolute configuration were determined by NMR spectroscopy and quantum chemical calculations. Notably, seconoriridone A featured a 2-butanonyl moiety with oxidative cleavage of the conventionally multisubstituted cyclohexane ring of iridals. Seconoriridone A was a mixture of C-14 epimers in the presence of hemiacetal. The plausible biosynthetic pathway for 1 was deduced.     

二维反相液相色谱制备五味子中的木脂素

应用自主研发的具有分离-富集模式的制备色谱工厂,建立了分离制备五味子木脂素有效部位及其单体化合物的方法。该方法首先以C₁₈（250 mm×4.6 mm,5 μm）为色谱柱,水和甲醇为流动相,分离度和保留时间为考察指标,采集4个不同梯度的色谱信息,通过XTool色谱专家系统软件模拟,确定五味子木脂素第一、二维色谱条件;然后采用线性放大的方法,以C₁₈（250 mm×30 mm,10 μm）为第一、二维分离柱,C₁₈（80 mm×30 mm,10 μm）为富集柱,水为富集稀释液,对五味子木脂素进行二维色谱分离纯化;最后第一维分离得到9个可重复组分,第二维分离得到20个高纯度化合物,其中有6个单体化合物。结果表明该法重现性良好,可以实现五味子木脂素的系统性分离,对五味子化学成分的研究具有重要意义。     

北五味子中一种新的莽草酸衍生物的分离纯化及其含量测定

从北五味子中提取分离得到一种新的莽草酸衍生物, 经一维、二维核磁共振波谱(1D NMR, HMQC, HMBC)等数据解析, 鉴定为莽草酸正丁酯. 并采用ZORBAX Extend C18柱, 以乙腈-0.05%磷酸为流动相进行梯度洗脱, 检测波长为215 nm, 流速1.0 mL/min, 建立了北五味子中莽草酸正丁酯含量的高效液相色谱分析方法. 结果表明, 莽草酸正丁酯在2~65 μg/mL浓度范围内线性关系良好, 相关系数r=0.9999, 平均回收率为98.25%, 相对标准偏差(RSD)为1.55%, 表明本法简单准确, 重复性好.     

高效液相色谱法测定五味子和含五味子的制剂中五味子乙素及多种活性成分时流动相体系的选择

建立了用高效液相色谱法测定五味子和含五味子的制剂中五味子乙素的流动相体系。用Shim-pack VP-ODS (250 mm×4.6 mm,5 μm)色谱柱,在柱温30 ℃、检测波长285 nm、流速1.0 mL/min的条件下,用不同的流动相组成及其不同比例研究了五味子提取液中3种木脂素(五味子乙素、安五脂素和五味子甲素)的保留时间及其分离情况,从中选择测定五味子乙素的最佳流动相体系。结果表明,在甲醇-水、甲醇-冰醋酸-水的流动相体系中,安五脂素和五味子乙素很难完全分离;而在乙腈-甲醇-水和乙腈-冰醋酸-水流动相体系中,3种木脂素可很好地分离。以乙腈-甲醇-水(体积比为17:58:25)为流动相测定五味子和护肝片中3种木脂素的含量,相对标准偏差(n4)为0.95%～5.8%,平均加标回收率为94.50%～105.6%。将该流动相体系用于供试品中3种木脂素含量的测定,分离效果好,结果令人满意。     

加速溶剂萃取法快速提取黄连中的生物碱

探讨了快速溶剂萃取法（ASE）提取黄连中生物碱的可行性,并比较了该方法与回流提取法和超声提取法的优越性。以黄连中盐酸小檗碱的提取率为指标,以高效液相色谱法（HPLC）为检测方法,用正交实验对快速溶剂萃取法从黄连中提取盐酸小檗碱的工作条件进行优化。最佳仪器参数：提取溶剂为80%乙醇＋0.5%HCl,提取温度为130℃,静态提取时间为10 min,提取次数为1次。快速溶剂萃取法可作为黄连中生物碱分析测定的前处理方法。     

A Comparison Study on Polysaccharides Extracted from Atractylodes chinensis (DC.) Koidz. Using Different Methods: Structural Characterization and Anti-SGC-7901 Effect of Combination with Apatinib

For hundreds of years, Atractylodes chinensis (DC.) Koidz. (AK) has been widely used as a treatment for spleen and stomach diseases in China. The AK polysaccharides (AKPs) have been thought to be the important bioactive components. In this stud, the impacts of different extraction methods were analyzed. The differences between AKPs extracted by hot water extraction (HWE), AKPs extracted by ultrasonic extraction (UAE), and AKPs extracted by enzyme extraction (EAE) were compared in terms of yield, total carbohydrate content, molecular weight distribution, monosaccharide composition, and synergistic activity of the AKPs with apatinib were determined. The results indicated that the yield of the polysaccharide obtained from HWE was higher than that of UAE and EAE. However, activity assays indicated that UAE-AKPs and HWE-AKPs enhanced apoptosis of human gastric cancer cells (SGC-7901) treated with apatinib and UAE-AKPs showed the strongest synergistic activities. This is also in agreement with the fact that UAE-AKPs have a smaller molecular weight, β-configuration, and higher galactose content. These findings suggested that UAE is an efficient and environmentally friendly method for producing new polysaccharides from Atractylodes chinensis (DC.) Koidz. for the development of natural synergist and for the treatment of gastric cancer.     

太空育种射干的FTIR分析

对我国首创的第4代太空育种射干与地面组射干的非晶成分从整体上进行了测定和对比分析,以期为更全面地了解太空射干品质的变化和深入研究积累资料,探索建立太空射干质量标准。结果表明两组样品的FTIR谱的主要吸收峰的峰位、峰形大致相同,但峰的强度却有明显差异。与地面组相比,太空射干在1 642 cm-1处酮类的CO伸缩振动峰增强,表明太空射干中的主要活性成分异黄酮类化合物含量明显增加,在1 318 cm-1处一水草酸钙吸收峰增加,在1 541,1 456 cm-1处分子中苯环的环伸缩振动峰、1 417 cm-1处亚甲基的C—H键弯曲振动峰以及1 051 cm-1处伯醇的C—O的伸缩振动峰都明显减弱。太空诱变育种有利于筛选出活性成分含量提高的射干新品种。预期太空射干的药效比地面组的有所增强,有待于深入研究来证实。