山玉兰叶化学成分研究

目的对山玉兰Magnolia delavayi叶的化学成分进行研究。方法采用MCI、硅胶、Sephadex LH-20、HPLC等多种色谱技术进行分离纯化,根据波谱数据鉴定化合物的结构。结果从山玉兰叶95%乙醇提取物中分离得到14个化合物,分别鉴定为(2E)-3,7,11-trimethyl-2,10-dodecadien-l,6,7-triol(1)、(2E,6E)-3,7,11-trimethyl-2,6-dodecadien-l,10,11-triol(2)、黑麦草内酯(3)、松脂醇(4)、丁香脂素(5)、梣皮树脂醇(6)、桉脂素(7)、连翘脂素(8)、松柏醛(9)、3,4,5-三甲氧基肉桂醇(10)、3-吲哚甲醛(11)、3-吲哚乙醇(12)、3,4-二甲氧基苯甲酸(13)、3,4-二甲氧基苯酚(14)。结论所有化合物均为首次从该植物中分离得到,并且首次报道化合物1的1H-和13C-NMR数据。     

基于大鼠离体外翻肠囊模型考察杜仲提取物在正常和自发性高血压状态下的肠吸收特性差异

目的:研究杜仲提取物在正常大鼠和自发性高血压大鼠的肠吸收特性差异。方法:采用大鼠外翻肠囊模型,收集10.0 g·L-1杜仲提取物给药后不同时间点的肠囊液,通过UPLC-MS/MS检测肠吸收液样品中京尼平苷酸、原儿茶酸、新绿原酸、绿原酸、隐绿原酸、松脂醇二葡萄糖苷、松脂醇单葡萄糖苷7个成分的含量,计算累积吸收量和吸收速率常数,比较正常大鼠和自发性高血压大鼠肠吸收液中杜仲提取物各指标成分的吸收情况。结果:杜仲提取物中7种成分的肠吸收均为线性吸收(R2均0.99),主要吸收部位在小肠,正常状态下以十二指肠的吸收最好。原儿茶酸和松脂醇二葡萄糖苷在高血压状态下的空肠有更好吸收,提示病理状态可能会改变药物吸收的特定部位。7个指标成分在SHR模型的肠吸收与正常大鼠相比均表现出了不同程度的差异。京尼平苷酸在自发性高血压大鼠各肠段的吸收弱于正常大鼠,但以松脂醇二葡萄糖苷为代表的其他成分都没有表现出一致的吸收趋势。结论:自发性高血压会影响杜仲提取物的肠吸收,从肠黏膜通透性降低和吸收部位后移的角度无法完全解释这些差异,可能还与肠道中存在的酶和转运蛋白等相关,具体作用机制有待进一步的深入研究。     

连花清瘟胶囊化学成分研究(I)

目的研究连花清瘟胶囊化学成分。方法采用硅胶、凝胶柱色谱、液相色谱等多种色谱方法对其进行分离和纯化,根据理化性质及波谱数据进行结构鉴定。结果从连花清瘟胶囊孔树脂70%乙醇部位分离得到20个化合物,分别鉴定为芦荟大黄素(1)、连翘脂素(2)、cepharanone B(3)、松脂醇(4)、表松脂醇(5)、松脂素单甲醚(6)、胡椒内酰胺A(7)、反式对羟基肉桂酸乙酯(8)、刺芒柄花素(9)、异甘草素(10)、柚皮素(11)、山柰酚(12)、ω-羟基大黄素(13)、大黄酸(14)、大黄素甲醚-8-O-β-D-吡喃葡萄糖苷(15)、4,5-dioxodehydroasimilobine(16)、kaempferol-3-O-α-L-ramnopyranosyl-4″-O-E-(4-hydroxy)-cinnamoyl(17)、大黄酚-1-O-β-D-吡喃葡萄糖苷(18)、大黄酚-8-O-β-D-吡喃葡萄糖苷(19)、大黄素-8-O-β-D-吡喃葡萄糖苷(20)。结论化合物2、3、5~17、19、20为首次从该复方中分离得到,为阐明连花清瘟胶囊药效物质奠定了基础。     

HPLC波长切换法同时测定杜仲双降袋泡剂中7种成分的含量

目的建立高效液相(HPLC)波长切换法同时测定杜仲双降袋泡剂中桃叶珊瑚苷、京尼平苷酸、绿原酸、京尼平苷、松脂醇二葡萄糖苷、芦丁及槲皮素7种成分含量的方法。方法以80%甲醇为溶剂,加热回流提取;色谱柱:Hydrosphere C18(4.6 mm×200 mm,5μm);柱温:30℃;流动相:乙腈-0.1%磷酸溶液,梯度洗脱;检测波长:208 nm(桃叶珊瑚苷)、235 nm(京尼平苷酸、绿原酸、京尼平苷、松脂醇二葡萄糖苷)、270 nm(芦丁、槲皮素);流速:0.9 ml/min。结果桃叶珊瑚苷、京尼平苷酸、绿原酸、京尼平苷、松脂醇二葡萄糖苷、芦丁、槲皮素的质量浓度分别在10.97~274.25μg/ml(r=0.999 7)、9.78~244.50μg/ml(r=0.999 8)、6.86~171.50μg/ml(r=0.999 6)、2.47~61.75μg/ml(r=0.999 7)、8.11~202.75μg/ml(r=0.999 1)、4.59~114.75μg/ml(r=0.999 9)、1.85~46.25μg/ml(r=0.999 5)范围内线性关系良好;平均加样回收率分别为99.85%、98.92%、97.52%、97.08%、98.51%、97.10%、96.91%,RSD分别为0.93%、0.74%、1.26%、1.37%、0.88%、1.05%、1.33%。结论所建立的HPLC波长切换法可以同时测定杜仲双降袋泡剂中桃叶珊瑚苷、京尼平苷酸、绿原酸、京尼平苷、松脂醇二葡萄糖苷、芦丁和槲皮素的含量,方法简便准确、灵敏度高,可用于杜仲双降袋泡剂的质量控制。     

Flaxseed lignan lowers blood cholesterol and decreases liver disease risk factors in moderately hypercholesterolemic men

The effects of flaxseed lignan (secoisolariciresinol diglucoside [SDG]) intake on hypercholesterolemia and liver disease risk factors in moderately hypercholesterolemic men were investigated. In a previous study, we reported that SDG attenuates high-fat, diet-induced hypercholesterolemia in mice. Here, we report a double-blinded, randomized, and placebo-controlled study in moderately hypercholesterolemic men in which we investigated the hypothesis that oral administration of SDG (20 or 100 mg) would decrease the level of blood cholesterol and liver disease risk factors induced by hypercholesterolemia in humans. Thirty men with total cholesterol levels of 4.65 to 6.21 mmol/L (180-240 mg/dL) were randomly assigned to 3 groups; 2 groups received flaxseed lignan capsules (SDG, 20 or 100 mg/d) and the other received placebo capsules for 12 weeks. We found that, compared to the subjects who received placebo, those who received 100 mg of SDG exhibited a significant reduction in the ratio of low-density lipoprotein/high-density lipoprotein cholesterol at baseline (P < .05) and at week 12 (P < .05). In addition, in SDG-treated subjects, we also observed a significant percentage decrease in the levels of glutamic pyruvic transaminase and γ–glutamyl transpeptidase relative to the levels at baseline (P < .01) and a significant percentage decrease in the level of γ–glutamyl transpeptidase relative to the placebo-treated group (P < .05). These results suggest that daily administration of 100 mg SDG can be effective at reducing blood level of cholesterol and hepatic diseases risk in moderately hypercholesterolemic men.     

HPLC法同时测定杜仲皮中京尼平苷酸、绿原酸、京尼平苷和松脂醇二葡萄糖苷

目的 HPLC法同时测定杜仲皮中京尼平苷酸、绿原酸、京尼平苷、松脂醇二葡萄糖苷4种有效成分的量,为更好控制杜仲皮质量提供依据。方法 采用Kromasil C₁₈柱（200 mm×4.6 mm,5 μm）,乙腈（A）-0.1%磷酸水溶液（B）梯度洗脱,0～7 min,7% A;7～35 min,14% A;35～45 min,15% A。体积流量1.0 mL/min,检测波长235 nm,柱温30 ℃。结果 在该色谱条件下,京尼平苷酸、绿原酸、京尼平苷、松脂醇二葡萄糖苷分别在0.102 5～0.512 5（r＝0.999 9）、0.092 5～0.462 5（r＝0.999 9）、0.120 0～0.600 0（r＝0.999 6）、0.090 0～0.450 0 μg/mL（r＝0.999 8）内与色谱峰峰面积呈现良好的线性关系,加样回收率分别为98.97%、98.71%、98.20%、100.44%,RSD分别为1.54%、1.30%、0.76%、1.13%。结论 该分析方法快速准确、重现性好,可为杜仲药材的质量控制与标准的完善提供可靠的检测依据。     

无花果果实中化学成分研究

目的研究桑科榕属植物无花果Ficus carica果实的化学成分。方法综合运用硅胶柱色谱、ODS柱色谱、Sephadex LH-20凝胶柱色谱以及制备型高效液相色谱等技术进行系统分离,根据化合物的理化性质及波谱数据鉴定化合物的化学结构。结果从无花果果实的90%乙醇提取物中分离得到了16个化合物,分别鉴定为怀特酮(1)、甘草宁G(2)、4′-羟基-5,7-二甲氧基-6-(3-甲基-丁烯基)-异黄酮(3)、猫尾草异黄酮(4)、indicanine C(5)、木豆素(6)、美迪紫檀素(7)、高丽槐素(8)、4-羟基-3-甲氧基-8,9-亚甲二氧基紫檀烷(9)、3-羟基-9,10-二甲氧基紫檀烷(10)、松脂素(11)、杜仲树脂酚(12)、丁香树脂醇(13)、8-羟基松脂醇(14)、3-羟基-1-(4-羟基-3-甲氧基苯)-1-丙酮(15)和4-羟基-3-甲氧基苯乙醇(16)。结论所有化合物均为首次从无花果中分离得到。     

Cytostatic inhibition of cancer cell growth by lignan secoisolariciresinol diglucoside

Our previous study demonstrated that lignan metabolites enterolactone and enterodiol inhibited colonic cancer cell growth by inducing cell cycle arrest and apoptosis. However, the dietary lignans are naturally present as glycoside precursors, such as secoisolariciresinol diglucoside (SDG), which have not been evaluated yet. This study tested the hypothesis that dietary SDG might have a different effect than its metabolites in human colonic SW480 cancer cells. Treatment with SDG at 0 to 40 μmol/L for up to 48 hours resulted in a dose- and time-dependent decrease in cell numbers, which was comparable to enterolactone. The inhibition of cell growth by SDG did not appear to be mediated by cytotoxicity, but by a cytostatic mechanism associated with an increase of cyclin A expression. Furthermore, high-performance liquid chromatography analysis indicated that SDG in the media was much more stable than enterolactone (95% of SDG survival vs 57% of enterolactone after 48-hour treatment). When the cells were treated with either enterolactone or SDG at 40 μmol/L for 48 hours, the intracellular levels of enterolactone, as measured by high-performance liquid chromatography–mass spectrometry/electron spray ionization, were about 8.3 × 10⁻⁸ nmol per cell; but intracellular SDG or potential metabolites were undetectable. Taken together, SDG demonstrated similar effects on cell growth, cytotoxicity, and cell cycle arrest when compared with its metabolite enterolactone. However, the reliable stability and undetectable intracellular SDG in treated cells may suggest that metabolism of SDG, if exposed directly to the colonic cells, could be different from the known degradation by microorganisms in human gut.     

紫花野芝麻化学成分研究Ⅱ

目的:研究紫花野芝麻的化学成分。方法:色谱等方法分离纯化,理化性质和光谱分析法鉴定化学成分。结果:分离并鉴定了 6 个化合物,分别为水龙骨素(polypodine B)(Ⅰ),5 OH 8 epiloganin(Ⅱ),shanzhiside methylester(Ⅲ), liriodendrin(Ⅳ),槲皮苷(quercetin-3-O-α-L-rhamnopyranoside, quercitroside)(Ⅴ),尿苷(uridine)(Ⅵ)。结论:liriodendrin为首次从野芝麻属植物中分得,其余化合物为首次从该植物中得到。