小酸浆中Withaphysalins的分离和结构鉴定

研究小酸浆Physalis minima L.的活性成分。小酸浆的地上部分经乙醇提取,氯仿萃取,D-101大孔树脂柱色谱粗分,Sephadex LH-20、MCI gel CHP 20P、RP-18等色谱柱分离,并通过理化常数和波谱学方法鉴定化合物结构。从小酸浆中分离鉴定了5个化合物,分别为Withaphysalin P(Ⅰ)、14,18-di-O-acetylwithaphysalin C(Ⅱ)、Withaphysalin Q(Ⅲ)、Withaphysalin型化合物1(Ⅳ)、Withaphysalin型化合物2(Ⅴ)。化合物Ⅳ、Ⅴ为新化合物,分别命名为Withaphysalin T、Withaphysalin U。     

Two sulfonate metabolites of physalin A in rats

1.?Physalin A is a bioactive withanolide isolated from the natural plant Physalis alkekengi var. franchetii (Solanaceae), a common traditional Chinese herbal medicine. This study aims to investigate the metabolites of physalin A in vivo.

2.?Two metabolites (M1 and M2) were characterized as sulfonate metabolites in the feces obtained from rats treated with physalin A orally at a dose of 15?mg/kg/day for 3 days, by application of a UPLC-Q/TOF-MS method. Furthermore, formation of the two sulfonate metabolites was verified by chemical synthesis and NMR, including ¹H NMR, ¹³C NMR and two-dimensional NMR. The structures of M1 and M2 were identified to be 3α-sulfo-2,25β,27-trihydrophysalin A and 3α,27-disulfo-2,25α-dihydrophysalin A, respectively.

3.?In summary, this study indicated that physalin A could be biotransformed to sulfonate metabolites with strong polarity, which contributed to the elimination of physalin A. A rare metabolic pathway has been revealed in this study.     

酸浆茎叶中的四甲基环己烯型单萜苷类化合物

目的研究茄科植物酸浆[Physalis alkekengiL.var.franchetii(Mast.)Makino]茎叶的化学成分。方法用体积分数为60%的乙醇水溶液加热回流提取,提取液浓缩后用水混悬,依次用环己烷、乙酸乙酯、正丁醇萃取;将正丁醇层通过聚酰胺柱色谱,Sephadex LH-20柱色谱、反相ODS开放柱色谱及反相制备HPLC等手段,共分离得到4个四甲基环己烯型单萜苷类(megastigmane glyco-sides)化合物;利用其理化性质和波谱学数据,鉴定化合物结构。结果分离得到4个四甲基环己烯型单萜苷类化合物,分别鉴定为(6S,9R)-长寿花糖苷[(6S,9R)-roseoside,1)]、(6S,9R)-长寿花糖苷[(6S,9S)-roseoside,2]、(6S,9R)-3-氧-α-紫罗兰醇-β-D-吡喃葡萄糖苷[(6R,9S)-3-oxo-α-ionol-β-D-glucopyranoside,3]、citroside A(4)。结论4个化合物均为首次从该属植物中分离得到。     

RP—HPLC测定酸浆药材中3种有效成分的含量

目的:采用 RP-HPLC 建立同时测定酸浆药材中酸浆苦味素 A、酸浆苦味素 D 及木犀草素含量的方法。方法:分析柱采用 Diamonsil C_(18)(200 mm×4.6 mm,5 μm)色谱柱,流动相为甲醇-0.2%醋酸(45:55,v/v);流速:1.0 mL·min~(-1);检测波长:220 nm。结果:酸浆苦味素 A、酸浆苦味素 D 及木犀草素浓度分别在0.15～1.20 mg·mL~(-1)(r=0.9995),0.10～0.81 mg·mL~(-1)(r=0.9996),0.12～0.96 mg·mL~(-1)(r=0.9997)范围内与峰面积呈良好的线性关系,酸浆苦味素 A 平均回收率分别为95.9%,97.1%,103%;RSD 分别为2.0%,0.7%,1.4%。酸浆苦味素 D 的平均回收率分别为97.3%,101%,97.1%;RSD 分别为1.0%,1.9%,1.3%。木犀草素的平均回收率分别为97.8%,97.8%,97.7%;RSD 分别为0.4%,2.9%,0.5%。结论:采用 RP-HPLC 同时测定酸浆药材中酸浆苦味素 A、酸浆苦味素 D 及木犀草素3种成分的含量,该法简单、可靠,可作为控制酸浆药材质量的参考标准。     

苦蘵多糖的提取及体外抗氧化活性的研究

目的研究苦蘵多糖的醇沉条件及其体外抗氧化活性。方法经超声提取,除脂,除蛋白等工艺得到苦蘵粗多糖,并考察了醇沉条件(醇沉比、温度、pH、时间、浓缩比)对多糖沉淀的影响。采用体外实验研究了苦蘵多糖对·OH和DP-PH的清除作用及对大鼠肝匀浆脂质过氧化的抑制作用。结果在最佳的醇沉条件(浓缩比4∶1,温度-20℃,醇沉时间16h,醇沉比为1∶4,pH为7)下,多糖提取率为3.15%。多糖对大鼠肝匀浆脂质过氧化的抑制率可达80%,对·OH和DPPH也都有很好的清除作用。结论苦蘵果实中多糖有良好的体外抗氧化活性。     

酸浆水提物最佳提取工艺的研究

目的 探讨酸浆水提物的最佳提取条件.方法 精称酸浆粉20 g,按正交试验列号提取,滤过,合并滤液,浓缩至膏状.结果 影响酸浆出膏率的因素主次顺序为:提取次数＞提取水量＞提取温度＞提取时间.结论 酸浆水提物的最佳提取条件:提取水量6倍,提取温度110℃,提取时间2h,提取次数3次.     

酸浆化学成分的研究

目的 研究酸浆Physalis alkekengi var. franchetii的活性成分。方法 酸浆的宿萼经乙醇渗漉提取,提取物经硅胶、Sephadex LH-20色谱分离,并通过理化常数和波谱学方法鉴定化合物结构。结果 分离鉴定了11个化合物,分别为β-谷甾醇(Ⅰ)、酸浆苦素A(Ⅱ)、酸浆苦素B(Ⅲ)、酸浆苦素O(Ⅳ)、酸浆苦素L(Ⅴ)、酸浆苦素M(Ⅵ)、胡萝卜苷(Ⅶ)、商陆素(Ⅷ)、5,4′,5′-三羟基-7,3′-二甲氧基黄酮醇(Ⅸ)、木犀草素(Ⅹ)、木犀草素-7-O-β-D-葡萄糖苷(Ⅺ)。结论 化合物Ⅸ为新化合物,命名为酸浆黄酮醇(physaflavonol)。     

Metabolomics Analysis of Health Functions of PhysalisPubescens L. using by Ultra-performance LiquidChromatography/Electrospray Ionization QuadrupleTime-of-Flight Mass Spectrometry

Herbal medicines may benefit from metabolomics studies, and applying metabolomics may provide answers about which herbal interventions may be effective for individuals, which metabolic processes are triggered, and the subsequent chemical pathways of activity. Physalis pubescens L (PPL) is an herbal fruit for one year living plant and has been developed into healthy function’s food. However, the mechanisms of health functions are still unclear. To comprehensively and holistically assess its anti-fatigue and antioxidant effects, a novel integrative metabolomics approach was applied. In this study, we present metabolomics analysis applying ultra performance liquid chromatography coupled to quadrupole with time-of-flight mass spectrometry (UPLC-Q/TOF-MS) to determine metabolite alterations after oral administration PPL to rats. Fifteen metabolites in urine were identified as potential biomarkers. Pattern analysis of the UPLC-Q/TOF-MS data disclosed that PPL could relieve fatigue rats by ameliorating the disturbance in amino acids metabolism and energy metabolism, alleviating the oxidative stress from reactive oxygen species and the inflammatory damage, and recovering the destructed regulation. Based on these results, we demonstrated that PPL is a promising source of natural anti-fatigue and antioxidants material for use in functional foods and medicines.     

毛酸浆的化学成分研究

对毛酸浆的干燥宿萼95%乙醇提取物的二氯甲烷部分进行化学成分的研究。利用正相硅胶柱色谱及反相制备高效液相色谱等方法分离纯化,得到10个化合物,通过质谱、一维及二维核磁共振波谱等手段对这些化合物的化学结构进行了鉴定,分别为5-O-(E-feruloyl)blumenol(1),异香草醛(2),反式对羟基肉桂酸乙酯(3),对羟基苯甲醛(4),对甲苯酚(5),反式肉桂酸甲酯(6),7,3',4'-三甲氧基槲皮素(7),5,3', 5'-三羟基-3,7,4'-三甲氧基黄酮(8),danielone(9),5,5'-二异丁氧基-2,2'-联呋喃(10),其中化合物1为新化合物,化合物7~10为首次从该属植物中分离得到。