蝙蝠葛化学成分的研究

从我国东北地区出产的蝙蝠葛Menispermum dauricnm DC.的根茎中分得五种生物碱,其中碱甲,碱乙和碱丙属于氧化异阿朴啡类生物碱。碱甲,碱乙和碱丙为新生物碱。根据红外,紫外光谱、质谱和核磁共振氢谱数据的分析,证明碱甲的结构为5,9-二甲氧基-7H-二苯基[de,h]喹啉-7-酮,命名为蝙蝠葛辛;碱乙证明为5,6-次甲二氧基9甲氧基-7H-二苯基[de,h]喹啉-7-酮,命名为蝙蝠葛定;碱丙证明为4,5,6,9-四甲氧基-7H-二苯基[de,h]喹啉-7-酮,命名为蝙蝠葛宁。其它二种为已知生物碱,为尖防己碱和N-去甲尖防己碱。     

蝙蝠葛中的新生物碱—N—去甲基蝙蝠葛碱

防己科植物蝙蝠葛(Menispermum dauricum DC.)的根茎,又名北豆根,是一常用中药,其总生物碱制成的北豆根片,临床用于咽喉炎的治疗;近年来又发现蝙蝠葛根茎中的主要生物碱-蝙蝠葛碱(dauricine)和酚性总碱均有较好的抗心律失常作用,并已用于临床治疗。由于蝙蝠葛新用途的发现,原料需求量日益增长。蝙蝠葛以往主产于我国东北地区,为了扩大药源,近年湖北咸宁地区对本地发现的少量野生蝙蝠葛进行了引种栽培,获得成功。为了考察咸宁栽培蝙蝠     

应用薄层荧光扫描法测定血清蝙蝠葛碱浓度

<正> 蝙蝠葛碱(Dauricime)系从防己科植物蝙蝠葛(Menispermum DauricumDC.)根茎中提出的一种双苄基异喹啉类生物碱。实验研究和临床试验均证明本品具有良好的抗心律失常作用。为进一步了解该药的体内过程,提供合理用药的药代动力学依据,测定蝙蝠葛碱血药浓度至为重要。目前,蝙蝠葛碱血浓测定方法学尚未见报道,本工作建立蝙蝠葛碱血清浓度测定法,实验证明采用薄层荧     

RP—HPLC法对不同产地蝙蝠葛几种主要生物碱的测定

目的：研究不同产地蝙蝠葛几种主要生物碱在质与量上的区别。方法：采用有机溶剂提取生药,应用ＲＰ－ＨＰＬＣ方法在东北产和咸宁产蝙蝠葛根茎中几种主要脂溶性生物碱定性定量测定。结果：东北生一最高的生物碱前３位依次是蝙蝠葛苏林碱、蝙蝠碱和ｇｕａｔｔｅｇａｕｎｅｒｉｎｅ;而咸宁药材则为蝙蝠葛碱、蝙蝠葛诺林碱及蝙蝠葛新诺林碱,不含蝙蝠葛苏林碱。结论：不同产地蝙蝠葛药材所含生物碱在质和量两方面均有显著差异。     

蝙蝠葛中的新生物碱——蝙蝠葛新林碱

防已科植物蝙蝠葛(Menispermum daurioum DC.)的根茎,即北豆根,是一种重要的中药,具有清热解毒、消肿止痛等功效。已知含有近二十种生物碱,其中五种属双苄基四氢异喹啉类,即蝙蝠葛碱(dauricine,Ⅰ)、蝙蝠葛诺林碱(daurinoline,Ⅱ)、蝙蝠葛新诺林碱     

蝙蝠葛中一新双苄基异喹啉生物碱

防己科植物蝙蝠葛（ＭｅｎｉｓｐｅｒｍｕｍｄａｕｒｉｃｕｍＤＣ．）根茎中的脂溶性酚性生物碱具有抗多种实验性心律失常活性〔１〕,近年研究表明,其主成分蝙蝠葛碱（ｄａｕｒｉｃｉｎｅ,１）和蝙蝠葛苏林碱（ｄａｕｒｉｓｏｌｉｎｅ,２）延长心肌动作电位时呈使用...     

RP-HPLC法测定北豆根药材中5个生物碱的含量

目的:采用RP-HPLC法同时测定中药材北豆根中青藤碱、蝙蝠葛苏林碱、蝙蝠葛诺林碱、蝙蝠葛新诺林碱和蝙蝠葛碱5种生物碱的含量。方法:采用色谱柱Welchrom-C18(250 mm×4.6 nm,5 mm),以甲醇(A)-乙腈(B)-0.4%二乙胺水溶液(C)为流动相,梯度洗脱[0～13 min,A-B-C(18:20:62);13～45 min,A-B-C(18:20:62)→A-B-C(37:20:43);45～60min,A-B-C(37:20:43)];流速1.0 mL·min-1;检测波长为285 nm。结果:青藤碱、蝙蝠葛苏林碱、蝙蝠葛诺林碱、蝙蝠葛新诺林碱和蝙蝠葛碱5种生物碱的线性范围分别为0.016～0.2μg(r=0.9995),0.029～0.363μg·mL-1(r=0.9996),0.09～1.125μg·mL-1(r=0.9996),0.336～4.2μg·mL-1(r=0.9997)与0.172～2.15μg·mL-1(r=0.9996);加样同收率(n=6)分别为99.2%,98.5%,102.2%,96.5%和98.4%。结论:该方法简便、快速、准确,重复性好,可以用于北豆根药材及其制剂的含量测定。     

HPLC法对不同产地北豆根中蝙蝠葛碱的测定

目的　研究不同产地北豆根中蝙蝠葛碱含量的差异。方法　以北豆根饮片为分析对象,用phenomenexC18(4 . 6mm×15 0mm,5 μm)色谱柱,采用乙腈和0 . 2 %磷酸洗脱,流速1. 0ml·min-1,检测波长为2 84nm,对北豆根中的蝙蝠葛碱进行定性定量测定。结果　东北北豆根药材中生物碱含量最高,其次是山东产北豆根,河北产北豆根药材中蝙蝠葛碱含量较低。结论不同产地北豆根药材所含生物碱在质和量两方面均有较大差异。     

HPLC法同时测定北豆根胶囊中蝙蝠葛新苛林碱等5种生物碱的含量

目的建立HPLC法同时测定北豆根胶囊中5种生物碱的含量。方法采用phenomenex C18色谱柱(150 mm×4.6 mm,5μm),以体积分数0.1%三乙胺水溶液(A)-乙腈(B)为流动相,梯度洗脱,检测波长为284 nm。结果蝙蝠葛新苛林碱、蝙蝠葛新诺林碱、N-去甲基蝙蝠葛碱、蝙蝠葛苏林碱和蝙蝠葛碱的线性范围为4.76~38.08、9.16~73.28、5.88~47.04、42.52~340.2和52.48~419.8 mg·L-1,线性关系良好(r≥0.999 4);平均加样回收率分别为102.6%、97.4%、96.8%、97.9%和98.9%,RSD(n=9)分别为2.4%、2.3%、3.1%、2.7%和2.5%。结论该方法可用于北豆根胶囊的质量控制,为其临床用药的安全性和有效性提供质量保证。     

山豆根碱的体内动力学研究

山豆根碱(dauricine)是从防己科植物蝙蝠葛(Menisppermnm dauricum D C.)中提取的酚性生物碱之一,是异喹啉类生物碱。动物实验证明有较好的降压效果。为此我们进行了山豆根碱的体内动力学研究。     

苦木生物碱的化学研究

苦木(Picrasma quassioides (D.Don)Benn.)总生物碱的各种制剂在临床上证明是有效的抗菌消炎药物。为了阐明其有效成分,对其生物碱进行了研究,自其茎心的乙醇提取物通过硅胶和氧化铝柱层析以及制备性薄层层析,分离得到七个生物碱,根据光谱分析,物理化学常数的测定和衍生物的制备,其中四种鉴别为已知的生物碱:1-甲氧甲酰-β-咔巴啉(Ⅱ),4.5-二甲氧基铁屎米酮(Ⅳ),铁屎米酮(Ⅴ),4-甲氧基-5-羟基铁屎米酮(Ⅵ)。另外三种为新的天然产物,证明其结构为1-乙氧甲酰-β-咔巴啉(Ⅰ),1-甲酰-β-咔巴啉(Ⅲ)和1-乙烯基-4.8-二甲氧基-β-咔巴啉(Ⅶ)。体外抗菌实验表明碱(Ⅱ),(Ⅳ),(Ⅵ)和(Ⅶ)为有效成分。其他生物碱因量少未进行抗菌实验。     

Stability of ciprofloxacin and norfloxacin in the presence and absence of metal ions in acidic solution

A thin-layer chromatographic-densitometric method was used to determine the stability of ciprofloxacin and norfloxacin in the presence and absence of metal ions in acidic solutions at 22°C, 50°C and 90°C. The degradation of ciprofloxacin and norfloxacin followed first order reaction kinetics in presence of metal ions. The extent of this degradation however depended on the type of metal ion and temperature. Product structures of ciprofloxacin (1-cyclopropyl-6-fluoro-7-(piperazin-1-yl)quinolin-4(1H)-one) and norfloxacin (1-ethyl-6-fluoro-7-(piperazin-1-yl)quinolin-4(1H)-one) were determined by analysis of UV spectra and using LC-MS method.     

A microbial model of mammalian metabolism: biotransformation of 4,5-dimethoxyl-canthin-6-one using Cunninghamella blakesleeana CGMCC 3.970

1.?A filamentous fungus, Cunninghamella blakesleeana CGMCC 3.970, was applied as a microbial system to mimic mammalian metabolism of 4,5-dimethoxyl-canthin-6-one (1). Compound 1 belongs to canthin-6-one type alkaloids, which is a major bioactive constituent of a traditional Chinese medicine (the stems of Picrasma quassioides).

2.?After 72?h of incubation in potato dextrose broth, 1 was metabolized to seven metabolites as follows: 4-methoxyl-5-hydroxyl-canthin-6-one (M1), 4-hydroxyl-5-methoxyl-canthin-6-one (M2), canthin-6-one (M3), canthin-6-one N-oxide (M4), 10-hydroxyl-4,5-dimethoxyl-canthin-6-one (M5), 1-methoxycarbonl-β-carboline (M6), and 4-methoxyl-5-O-β-D-glucopyranosyl-canthin-6-one (M7).

3.?The structures of metabolites were determined using spectroscopic analyses, chemical methods, and comparison of NMR data with those of known compounds. Among them, M7 was a new compound.

4.?The metabolic pathways of 1 were proposed, and the metabolic processes involved phase I (O-demethylation, dehydroxylation, demethoxylation, N-oxidation, hydroxylation, and oxidative ring cleavage) and phase II (glycosylation) reactions.

5.?This was the first research on microbial transformation of canthin-6-one alkaloid, which could be a useful microbial model for producing the mammalian phase I and phase II metabolites of canthin-6-one alkaloids.

6.?1, M1?M5, and M7 are canthin-6-one alkaloids, whereas M6 belongs to β-carboline type alkaloids. The strain of Cunninghamella blakesleeana can supply an approach to transform canthin-6-one type alkaloids into β-carboline type alkaloids.     

东风桔化学成分的研究

从东风桔根中分离到一种新的吖啶酮类生物硷。根据紫外,红外,核磁共振谱和质谱等证明其结构为N-甲基-1,4,5-三羟基-3,6-二甲氧基吖啶酮-9,命名为东风桔碱B。     

宁国贝母生物碱的分离和结构鉴定

从贝母新种——宁国贝母(Fritillaria ningguoensis S. C. Chen et S. F. Yin)鳞茎中分离出五个生物碱,其中碱V是一种新的生物碱,命名为宁贝新(ningpeisine),根据理化常数和光谱解析以及衍生物制备,测定其结构为N-methyl-3β-hydroxy-5α-veratranine-6-one。其余四种生物碱鉴定为浙贝甲素(peimine,verticine,Ⅰ),浙贝乙素(peiminine,verticinone,Ⅱ),异浙贝甲素(isoverticine,Ⅲ)和贝母辛(peimisine,Ⅳ)。     

Acetylenchemie, 3. Mitt. Ein einfacher Zugang zum Flindersin via Phasen-Transfer-Reaktion

Acetylene Chemistry, III: A Simple Approach to Flindersine by Phase-Transfer Reaction Reaction of 4-hydroxyquinolin-2-one (4) with 3-chloro-3-methylbut-1-yne by phase-transfer catalysis affords flindersine (3) and 2,3-dihydro-3,3-dimethyl-2-methylenefuro[3,2-c]quinolin-4-one (5) , whereas indolin-2-one (4g) yields N-(1′,1′-dimethylprop-2-yn-1-yl)indolin-2-one (19) . The reaction mechanism is discussed and studied by varying the reaction conditions.     

1,3-Dihydro-2H-imidazo[4,5-b]quinolin-2-ones--inhibitors of blood platelet cAMP phosphodiesterase and induced aggregation.

A series of 1,3-dihydro-2H-imidazo[4,5-b]quinolin-2-one derivatives was synthesized and evaluated as inhibitors of cAMP hydrolysis by a crude human platelet phosphodiesterase preparation and as inhibitors of ADP- and collagen-induced aggregation of rabbit blood platelets. The parent structure 7a, demonstrated potent inhibitory activity that was enhanced by the introduction of alkyl, alkoxy, or halogen substituents at the 5-, 6-, 7-, and 8-positions. Methylation at N-1 or N-3 produced weaker inhibitors of cAMP PDE and platelet aggregation. 1,3,9,9a-Tetrahydro-2H-imidazo[4,5-b]quinolin-2-ones (6) were found to be equipotent with their fully oxidized congeners (7). On the basis of platelet inhibitory properties in vitro, efficacy at preventing thrombus formation in animal models of thrombosis, and a favorable hemodynamic profile, 1,3-dihydro-7,8-dimethyl-2H- imidazo[4,5-b]quinolin-2-one (7o, BMY 20844) was selected for advancement into toxicological evaluation and clinical trial. An efficient synthesis of 7o is described.     

Two new alkaloids from the rhizome of Polygonatum sibiricum

Two new alkaloids named polygonatine A (1) and polygonatine B (2) have been isolated from the rhizome of Polygonatum sibiricum Redoute (Liliaceae). By spectral data (IR, UV, MS, 1D and 2D NMR) and chemical evidence, their structures were elucidated as 3-hydroxymethyl-5,6,7,8-tetrahydroindolizin-8-one (1) and 3-ethoxymethyl-5,6,7,8-tetrahydroindolizin-8-one (2).     

东风桔化学成分的研究

从东风桔根中分离到一种新的吖啶酮类生物硷。根据紫外,红外,核磁共振谱和质谱等证明其结构为N-甲基-1,4,5-三羟基-3,6-二甲氧基吖啶酮-9,命名为东风桔碱B。