RP-HPLC法测定牛蒡子中木脂素的含量

用RP-HPLC法分离并测定了牛蒡子中5种2,3-二苄基丁内酯型木脂素——牛蒡甙(Ⅰ)、牛蒡酚A(Ⅱ)、牛蒡酚F(Ⅲ)、牛蒡甙元(Ⅳ)、牛蒡素B(Ⅴ)。以安定为内标,分析柱C₁₈,甲醇-水-乙腈-四氢呋喃(57:49:11:1)为流动相,梯度流速,1.0～1.5m1/min。检测波长220nm,线性范围0.029～0.242μg,相关系数r=0.9993～0.9999,回收率96.14～104.99%。本法简便、快速、灵敏。     

甘肃产牛蒡子的质量评价研究

目的 对甘肃部分地区产牛蒡子进行质量评价研究,为完善甘肃产牛蒡子饮片的质量规范提供技术支持。方法 采用HPLC测定牛蒡苷、牛蒡苷元含量;采用UV测定总木脂素含量;采用醚浸出物法测定脂肪油含量。结果 收集到的甘肃地区产8个牛蒡子样品中牛蒡苷含量均达到中国药典标准要求,且甘肃定西、临洮、庆阳、和政和甘南产牛蒡子中所含牛蒡苷、牛蒡苷元、总木脂素及醚浸出物含量均不低于收集到的吉林、银川、康定、河南等地产的牛蒡子。结论 甘肃地区产牛蒡子药材质量较好,牛蒡子可作为甘肃开发引种药材新品种的选择。     

樟叶胡椒中新木脂素成分的研究

自胡椒科胡椒属植物樟叶胡椒(Piper polysyphorum C. DC)中分离到六个新木脂素(neolignans)类化合物,经光谱(UV,IR,MS,¹H-NMR,¹³C-NMR,2D-NMR,CD)分析及衍生物制备,确定Ⅱ为新化合物,即threo-△⁷-7-羟基-3,4,5,3′,5′-五甲氧基-8-O-4′-新木脂素,为一对对映体,命名为樟叶素(polysyphorin),Ⅰ,Ⅲ,Ⅳ为新的对映体,分別为(+)-virolongin,(+)-grandisin及(+)-lancifolin D.化合物Ⅴ为南藤素(wallichinine),Ⅵ为山蒟素D(hancinone D)。血小板活化因子(PAF)受体结合实验及PAF引起的血小板聚集实验证明化合物Ⅰ～Ⅴ具有明显的抑制活性。     

海风藤中新木脂素类PAF拮抗活性成分的研究

自中药海风藤[Piper kadsura (Choisy)Ohwi]的藤茎中又分离得到四个macrophyllin型双环[3,2,1]辛烷类新木脂素,经光谱分析及衍生物的制备,确定化合物Ⅰ和Ⅲ为新结构,命名为风藤素K(kadsurenin K)和风藤素L(kadsurenin L),其化学结构分别为7R,8R,3′R,5′R-△^8′-3,5′-二甲氧基-4-羟基-2′,3′,4′,5′-四氢-2′,4′-氧-7.3′,8.5′-新木脂素(Ⅰ)和7R,8R,3′S,4′R,5′R-△^8′-3,4,5′-三甲氧基-4′-乙酰氧基-2′,3′,4′,5′-四氢-2′-氧-7.3′,8.5′-新木脂素(Ⅲ)。化合物Ⅱ和Ⅳ分别为已报道过的风藤素C和风藤素B。化合物Ⅰ～Ⅳ均有明显的PAF受体拮抗活性。     

甘肃牛蒡不同部位总木脂素及牛蒡苷的含量测定

目的对甘肃临洮产牛蒡不同部位所含总木脂素及牛蒡苷含量进行测定。方法利用牛蒡子中总木脂素与牛蒡苷在同一峰位有吸收的特点,以牛蒡苷为对照品,以280 nm为测定波长,紫外分光光度法测定牛蒡不同部位总木脂素含量,同时采用HPLC测定其牛蒡苷含量。结果牛蒡苷浓度在0.005 7～0.079 5 mg.mL 1内,吸收度与浓度呈良好线性关系,线性方程为Y=9.244 9X+0.017 2,r=0.999 6,平均回收率98.2%,RSD=1.61%。以牛蒡苷计,牛蒡子中总木脂素含量为12.27%,牛蒡根、牛蒡叶、牛蒡茎中总木脂素的含量均在6%左右。牛蒡子中牛蒡苷的含量为6.19%(n=3),牛蒡根、牛蒡茎、牛蒡叶样品均未检测到牛蒡苷。结论采用紫外分光光度法和HPLC分别测定牛蒡不同部位总木脂素和牛蒡苷含量的方法快速、简捷,可全面控制牛蒡的质量。     

柄果花椒树皮的化学成分研究

本文主要报道自芸香科(Rutaceae)花椒属植物柄果花椒Zanthoxylum Podocarpum Hemsl.树皮中分得九种结晶性化合物,经物理常数测定,光谱分析以及化学反应分别鉴定了β-香树脂醇Ⅰ、1-细辛素Ⅲ、1-芝麻素Ⅴ、柄果脂素Ⅵ和新棒状花椒酰胺(neoherculin)Ⅷ。此外,尚有β-谷甾醇Ⅳ和山蓊酸(behenic acid)为主的混合长链脂肪酸Ⅶ。柄果脂素Ⅵ属于细辛素类木脂体,为Pluviatilol的r,r-二甲基烯丙基醚,是一新木脂体,经药理筛选发现具有中枢神经抑制作用。结晶Ⅱ和Ⅸ的结构尚待证实。     

山荷叶中木脂素成分的研究

从陕西产山荷叶(Diphylleia sinensis Li.)根茎中分得9个木脂素和1个黄酮化合物,通过光谱分析证明化合物Ⅸ为新木脂素,即苦鬼臼素-1-乙基醚(picropodophyllin-1-ethyl ether),其它化合物分别为鬼臼毒素(podophyllotoxin,Ⅰ)、异苦鬼臼酮(isopicropodophyllone,Ⅱ)、去氢鬼臼毒素(dehydropodophyllotoxin,Ⅲ)、山荷叶素(diphyllin,Ⅳ)、苦鬼臼素(picropodophyllin,Ⅴ)、鬼臼酯酮(podophyllotoxone,Ⅵ)、4′-去甲基鬼臼毒素(4′-demethylpodophyllotoxin,Ⅶ)、苦鬼臼素葡萄糖甙(picropodophyllin slucoside,Ⅷ)和山奈酚(kaempferol,Ⅹ)。其中化合物Ⅱ,Ⅵ,Ⅶ和Ⅷ为首次从山荷叶属植物中分得。     

仙茅的酚性甙成分研究

从仙茅科仙茅(Curculigo orchioides Gaerth.)根茎的水溶性部位中,分离得到一个新的酚性甙和两个新的含氯酚性甙。经光谱(UV,IR.¹HNMR,^{13CNMR和MRMS,FAB-MS)解析及化学方法,确定了它们的结构,并且分别命名为仙茅甙乙(Curculigoside B),仙茅素B和C(curculigine B和C)。}     

何首乌乙酸乙酯不溶部分化学成分的研究

从四川何首乌(polygonu mnultiflorum Thunb)块根乙醇提取物的乙酸乙酯不溶部分分离得到五个单体,经理化常数测定,光谱(IR,UV,FAB-MS,¹HNMR,¹³CNMR,¹H-¹³CCOSY和NOE差谱)分析及衍生物制备,确定了两个化合物的结构为新化合物。化合物Ⅰ1,3-二羟基-6,7-二甲基酮-1-O-β-D-葡萄糖甙,命名为何首乌乙素,化合物Ⅱ为2,3,5,4′-四羟基-二苯乙烯-2,3-二-O-β-D葡萄糖甙,命名为何首乌丙素。其余三个结晶因量少有待进一步分离、鉴定。     

宝藿甙-Ⅰ,Ⅵ,Ⅶ和宝藿素的分离和结构研究

自宝兴淫羊藿(Epimedium davidii Franch)中分离出8个黄酮类化合物,根据理化数据、光谱分析(UV,IR,¹HNMR,¹³CNMR,MS)和水解实验证明,其中E₃,E₁₃和E₈分别为已知成分淫羊藿甙、淫羊藿素和苜蓿素。E₁,E₁₁、E₁₆和E₁₅是新黄酮类化合物,并证明结构,分别命名为宝藿甙-Ⅰ(baohuoside Ⅰ),宝藿甙-Ⅵ(baohuoside Ⅵ),宝藿甙-Ⅶ(baohuo side Ⅶ)和宝藿素(baohuosu)。E¹⁷的结构待定。     

腺嘌呤衍生物的合成及体外抗疱疹病毒活性

以腺嘌呤为母体,在其9位引入活性基团N-取代缩氨基硫脲(TSC),设计合成了12个6-氨基-9(N^4'-取代乙醛缩氨基硫脲)嘌呤衍生物(4a～1),并进行了体外抗单纯疱疹病毒I型(HSV-1),II型(HSV-2),水痘-带状疱疹病毒(VZV)活性试验及细胞毒性试验。结果表明,除化合物4e及4f对HSV-1及VZV有较高活性外,其余化合物对上述两种病毒的活性均不明显。另外,将4e与4f分别与无环鸟苷(ACV)联合用药,其最小抑制浓度(MIC)及细胞毒性(MCC)均显著下降。     

Synthesis and Antimicrobial Activities of a Novel Series of Heterocyclic α‐Aminophosphonates

Two series of novel α‐aminophosphonates having heterocyclic moieties were synthesized in high yields. The structures of the newly synthesized compounds were confirmed by their elemental analyses, IR, ¹H NMR and MS spectral data. These compounds were screened for their antibacterial activities against Escherichia coli (NCIM2065) as a Gram‐negative bacterium, Bacillus subtilis (PC1219) and Staphylococcus aureus (ATCC25292) as Gram‐positive bacteria, and Candida albicans and Saccharomyces cerevisiae as fungi. The minimum inhibitory concentrations (MICs) of the synthesized compounds show high antibacterial and antifungal activities at low concentrations (10–1000 µg/mL). Furthermore, their lethal doses indicated that such compounds are safe for use as antimicrobial agents.     

疟疾防治药物的研究——Ⅹ.2,4-二氨基-6-N1,N2-二取代肼基-喹唑啉类衍生物的合成及其抗疟作用

本文报道了2,4-二氨基-6-N¹,N²-二取代肼基-喹唑啉类衍生物的合成及其抗疟活性的研究。这类化合物的合成是以2,4-二氨基6-取代苄基氨基-喹唑啉为原料经亚硝化、还原成为2,4-二氨基6-(N¹-取代苄基)—肼基喹唑啉,再与相应的醛缩合而成。此类化合物经伯氏鼠疟原虫抑制性治疗初筛表明有少数具有一定的效果。有11个化合物经约氏鼠疟原虫—斯氏按蚊系统病因性初筛有效。其中化合物Ⅱ_1,7,8,11,15和Ⅲ₁口服2.5mg/kg,连续3天,可使受试小鼠全部得到保护。     

人工蛹虫草子实体化学成分

目的　研究人工培养蛹虫草（Cordyceps militaris）干燥子实体的化学成分。方法　利用各种色谱技术进行分离纯化,通过理化方法及光谱（UV,IR,HRMS,EIMS,¹HNMR,¹³CNMR,FGCOSY,DEPT,FGHMQC和FGHMBC）分析鉴定其化学结构。结果　从人工培养蛹虫草干燥子实体的乙醇提取物中分离得到7个化合物,分别鉴定为: 3′-脱氧腺苷（3-deoxyadenosine, 1）, 腺苷（adenosine, 2）, N⁶-甲基腺苷（N⁶-methyladenosine, 3）, O^5′-乙酰基虫草素(O^5′-Acetylcordycepin, 4), N⁶-［β-(乙酰胺甲酰)氧乙基］腺苷（N⁶-［β-(acetylcarbamoyloxy) ethyl］ adenosine, 5）,虫草环肽A(cordycepeptide A, 6)和麦角甾醇过氧化物（ergosterol peroxide, 7）。结论　化合物(5）和(6)为两个新化合物,并首次归属这些化合物波谱信号。     

土茯苓化学成分的研究(Ⅲ):光叶菝葜甙的分离和鉴定

土茯苓化学成分的研究（Ⅲ）：光叶菝葜甙的分离和鉴定易以军，曹正中，杨文红，洪武奇，曹园，冷宗康（南京药物研究所２１０００９）土茯苓为百合科植物光叶菝葜（ＳｍｉｌａｘｇｌａｂｒａＲｏｘｂ）的干燥根茎，为常用中药之一，有解毒、除湿、利关节的功效。在对其化...     

Substituted adamantylphthalimides: Synthesis,antiviral and antiproliferative activity

In this study, three groups of adamantylphthalimides, bearing different substituents at the phthalimide moiety, N-(4′-R²)phthalimidoadamantanes ( 1 – 7 ), 3-[N-(4′-R²)phthalimido]-1-adamantanols ( 8 – 10 ), and 3-[N-(4′-R²)phthalimido]adamantane-1-carboxylic acids ( 11 – 15 ), were synthesized and screened against tumor cells and viruses. The most potent compounds are not substituted at the adamantane and bear an OH or NH₂ substituent at the phthalimide (compounds 3 and 5 ). The antiproliferative activities of compounds 3 and 5 are in the micromolar range, much higher than the one of thalidomide. A minor antiviral activity against cytomegalovirus and varicella-zoster virus was found for compounds 3 and 5 , but these compounds lacked selectivity. The results presented are important for the rational design of the next-generation compounds with anticancer and antiviral activities.     

Reliable identification and quantification of anabolic androgenic steroids in dietary supplements by using gas chromatography coupled to triple quadrupole mass spectrometry

The aim of the present research was the identification and quantification of specific anabolic androgenic steroids (AASs) and other sterane structured compounds in dietary supplements (DSs). The adulteration of DSs by these compounds is of a particular concern in athletes, because it might lead to a positive doping result. The research was focused on the optimization of a highly sensitive and selective GC-based analytical strategy using triple quadrupole MS as detector. Chromatographic method and multiple reaction monitoring (MRM) transitions of 28 target compounds were optimized. Sample clean-up was carried out by using a solid phase extraction (SPE) procedure, while the derivatization of AASs was performed by using N-methyl-N-(trimethylsilyl)-trifluoroacetamide (MSTFA). The method was validated, and the following parameters were investigated: linearity range, limit of detection, accuracy, and precision expressed in terms of intra-day precision. The calibration curves were evaluated by using regression model and resulting in a good determination coefficients (R² ≥ 0.9912). The residuals were scattered randomly around zero. The limits of detection (LODs) were lower than 7.0 ng g⁻¹ or ng ml⁻¹. The accuracy assessment was evaluated in different forms of DSs characterized by high sample-to-sample variability (liquid, powder, tablet, capsule, protein, and herbal-based). Intra-day assay precision was in all cases lower than 20%. The developed analytical method was successfully applied to the analysis of 67 commercially available dietary supplements. In five cases, one or more steroid-type compounds were found in the concentration of 5 ng g⁻¹–100 μg g⁻¹, which might result adverse analytical findings in athletes.     

3′(5α-3β,17β-双羟基-雄甾烷-17α)-丙酸内酯(Ⅴ)的微生物转化——螺旋内酯甾(Ⅱ)的合成

3′-(5α-3β,17β-双羟基-雄甾烷-17α)-丙酸内酯(Ⅴ)经诺卡氏菌(Nocardia sp.)转化获得6个化合物(Ⅱ和Ⅵ～Ⅹ),其中螺旋内酯甾(Ⅱ)为其主要产物(～50%)。Ⅷ～Ⅹ是尚未被鉴定的羟基化合物。化合物(Ⅴ)用诺卡氏菌在氮源贫乏的培养基中转化主要生成△⁴-3-酮化合物,而在氮源丰富的培养基中转化则主要为△^1,4-3-酮的产物。     

西南獐牙菜化学成分的研究

从西南獐牙菜的全植物中分离出五个化合物,其中四个分别被鉴定为β-谷甾醇(Ⅶ),齐墩果酸(Ⅵ),1,3,7,8-四羟基咄酮(Ⅴ)和山楂酸(Ⅱ)。另一化合物系新的三萜酸糖酯甙,命名为獐牙菜皂甙(swericinctoside,Ⅰ),其结构为2α,3β-二羟基齐墩果-12-烯-28-羧酸-28-O-β-D-葡萄吡喃糖基-(1-6)-β-D-葡萄吡喃糖基-(1-2)-β-D-葡萄吡喃糖甙。     

Synthesis of some novel orsellinates and lecanoric acid related depsides as α-glucosidase inhibitors

Abstract

Sixteen novel orsellinic esters (6a-l, 7a-d) along with four lecanoric acid related depsides (3a-c, 4) were synthesized and confirmed their structures by spectroscopic data (¹H, ¹³C & HRMS). The synthesized compounds were evaluated for their in vitro α-glucosidase (Saccharomyces cerevisiae) inhibitory potential. Among the tested compounds, 3c (IC₅₀: 140.9 μM) and 6c (IC₅₀: 203.9 μM) displayed potent α-glucosidase inhibitory activity and found more active than the standard drug acarbose (IC₅₀: 686.6 μM). Both the test compounds were subjected to in vivo antihyperglycemic activity using sucrose loaded model in Wistar rats and found compound 3c exhibited significant reduction in glucose levels.