豹皮菌中2-Amino-3-(1,2-dicarboxyethylthio)propanoic acid非对映异构体的绝对构型

Four stereoisomers of 2-amino-3-(1,2-dicarboxyethylthio) propanoic acid were prepared by reaction of L- and D-cysteine with fumaric acid. The absolute configuration of the diastereoisomer of 2-amino-3-(1,2-dicarboxyethylthio) propanoic acid from Amanita pantherina were assigned as (2R, 1'R) and (2R, 1'S) by analysis of the optical properties. Pharmacological tests showed that all of the four stereoisomers inhibited the depolarization of NMDA on spinal motorneurones in newborn rats, The inhibition intensity of L-A,D-A and D-B were higher than that of L-B.     

穆坪马兜铃化学成分的研究

自穆坪马兜铃(Aristolochia moupinensis Franch)根、茎中分得十三个化合物,其中化合物Ⅰ～Ⅻ经鉴定分別为马兜铃酸Ⅰ(aristolochic acid Ⅰ)(Ⅰ),尿囊素(allantoin)(Ⅱ),紫丁香酸(syringic acid)(Ⅲ),香豆酸(P-coumaric acid)(Ⅳ),马兜铃酸Ⅳ(aristolochic acid Ⅳ)(Ⅴ),β-谷甾醇(Ⅵ),木兰碱(magnoflorine)(Ⅶ),马兜铃酸Ⅳ甲醚aristolochic acid Ⅳmethyl ether(Ⅵ),棕榈酸(Ⅸ),马兜铃酸Ⅱ(aristolochic acid Ⅱ)(Ⅹ),N(Phydroxyphenethy1)P-coumaramide(Ⅺ),马兜铃酸Ⅳ甲醚甲酯(aristolochic acid Ⅳmethyl ether methyl ester)(Ⅻ),化合物ⅩⅢ为新化合物,经光谱分析和化学合成等方法证明其结构为N(P-hydroxyphenethyl)-ferulamide,命名为穆坪马兜铃酰胺(moupinamide)。初步药理试验表明穆坪马兜铃酰胺体外有抑制血小板聚集和影响血小板内前列腺素合成的作用。     

槲寄生化学成分的研究——Ⅷ.2,3-丁二醇单葡萄糖甙的分离和结构

From the ethanol extract of Viscum coloratum (Kom.) Nakai , a giucoside ofaliphatic diol and three other glucosides were isolated. Based on chemical and spectroscopic analysis,the structures have been elucidated as 2-β-D- glucosyl-3- methylpropanol (Ⅷ), syringin (Ⅸ),eleatheroside E(Ⅹ) and syringenin-4'-O-D-apiosylglucoside (Ⅺ). Ⅷ is a new glucoside of aliphaticdiol and named 3-β-D-glucopyranosyloxy-butanol-2. Three other compounds (Ⅸ～-Ⅺ) were foundfor the first time in this plant.     

锁阳中三萜及甾体成分的研究

From the whole parasitic plant of Cynomorium songaricum Rupr. three ursane type triterpenes, three steroidal compounds, palmitic acid and sucrose were isolated. The triterpenes were identified as acetyl ursolic acid (2), ursolic acid (3) and a new compound, ursa-12-ene-28-oic acid, 3β-propanedioic acid monoester (1). The steroidal compounds were identified as β-sitosterol palmitate (4), β-sitosterol (5) and β-sitosterol glucoside (daucosterol, 6). Compounds 2 and 5 were found in this genus for the first time.     

α,ω-双(对烃氧基苯氨基)-烷及 N,N′-双(对取代基苯基)-烃二醯胺类化合物的合成

1. α,ω-Bis- (p-alkoxyphenylamino) -alkanes, N,N'-bis-(p-substituted phenyl)- alkane dicarboxamides and N, N'-bis-(p-substituted phenyl)-alkane dicarboxylates were prepared for studying the relationship between chemical structure and thera- peutic activity, against Schistosomiasis japonica in experimental animals. 2. α,ω-Bis-(p-alkoxyphenylamino)-heptanes were prepared from p-alkoxyaniline and 1,7-dibromoheptane in the presence of sodium bicarbonate. α,ω-Bis-(p-alkoxy- phenylamino)-pentanes were prepared by hydrolysis of N,N'-bis-(p-alkoxyphenyl)- N, N'-bis-(p-toluene sulfonyl)-pentanediamines with 25% hydrochloric acid, while the latter were obtained by condensation of N-(p-alkoxyphenyl)-p-toluene sulfonamides with 1,5-dibromopentane in alcoholic alkaline solution. 3. N, N'-Bis-(p-substituted phenyl)-alkane dicarboxamides were prepared from p-substituted aniline and alkane dicarboxylic acid chlorides. According to Grimmel's method, we also prepared these compounds of this series by the reaction of p,p'-bis- (dimethylamino)-phosphazo benzene with corresponding alkane dicarboxylic acid. In the case of succinic acid, we obtained, however, mainly N-(p-dimethylaminophenyl)- succinimide instead of succinic diamide. 4. The intermediate, p-diethylamino-ethoxyaniline, was prepared by hydrolysis of the condensation product of p-acetaminophenol and diethylaminoethyl chloride. 5. Sodium salt of dimethylaminophenol was treated with alkane dicarboxylic acid chloride to give the corresponding N, N'-bis-(p-dimethylaminophenyl) -alkane dicar- boxylates.     

中药赤芍中化学成分的研究

Two new monoterpene glycosides were isolated from the ethanolic extract of the root of Paeonia laetiflora Pall. The structure of compound (Ⅰ) has been identified as (Z)-(1S, 5R)-β-pinen-10-yl β-vicianoside; Compound (Ⅱ) is named lactiflorin and tentatively assigned as (Ⅱ).Compound (Ⅰ) is the glycoside of the enol form of an aldehyde. In compound (Ⅱ), the sugar moiety is attached to the aglycone by two ether-like linkages. Both seem to be unprecedented.     

大腸菌变种用于維生素B12微生物测定法的研究

A mutant strain of E. coli (44110-1) was used in the cup-plate method for ultra-micro analysis of vitamin B₁₂. This method has been proved to be sensitive while the concentration of B₁₂ is within the range of 0.05—0.5γ/ml. B₁₂ contents in several samples of commercial liquid extract of liver were thus assayed and found to be approximately the same to that labelled. The cup-plate method of employing E. coli as an assay organism is superior to that using Lactobacilli, for culture media and instruments used are easily obtained and the whole assay is not difficult to control.     

中药秦艽中总生物碱的含量测定

A method for determining the total alkaloids of the Chinese drug Tsingjiu (秦艽) (Gentiana macrophylla) based on titration with silicotungstic acid was found. Weigh out accurately 2 g of pulverized (80 mesh) sample. Macerate it in a glass-stoppered flask with 50 ml of a mixture of chloroform-methanol-concentrated ammonia water (75: 25: 5) for 48 hours with occasional shaking. Take exactly 25 ml of the filtrate, evaporate and dissolve the residue in 0.6 N acetic acid, Impurities in the acetic acid solution are removed with lead acetate and the excess of Pb⁺² is removed by sodium sulphate. The clear filtrate is adjusted to about 50 ml with an acidity at about 0.5 N. The solution is titrated with 0.01 M silicotungstic acid, using malachite green as an outside indicator. Results are calculated on gentianine (C₁0H₉O₂N).     

LC-MS/MS法测定人血浆中西酞普兰及其在制剂生物等效性中的应用

A sensitive and selective LC-MS/MS method for determination of citalopram in human plasma was established to study the bioequivalence of different formulations containing citalopram. The samples were simply pretreated by protein precipitation using acetonitrile, and then analyzed on a Zorbax Extend C₈column. The mobile phase consisted of acetonitrile-water-formic acid (60∶40∶0.2), at a flow-rate of 0.5 mL·min^-1. A Thermo Finnigan TSQ Quantum Ultra tandem mass spectrometer equipped with electrospray ionization source was used as detector and was operated in the positive ion mode. Selected reaction monitoring using the precursor to product ion combinations of m/z325 → m/z109 and m/z265 → m/z167 was performed to quantify citalopram and the internal standard, respectively. The pharmacokinetic parameters of citalopram in different formulations were calculated by non-compartment model. The linear calibration curves were obtained in the concentration range of 0.10-100 μg·L^-1. The lower limit of quantification was 0.10 μg·L^-1. The intra- and inter-day relative standard deviation (RSD) over the entire concentration range was less than 5.2%. Accuracy determined at three concentrations (0.25, 8.00 and 90.0 μg·L^-1 for citalopram) ranged from -4.7% to 1.3%. Each plasma sample was chromatographed within 3.0 min. The method was successfully used in bioequivalence study of citalopram in human plasma after oral administration of 20 mg citalopram. Calculated with AUC_{1-120 h}, the bioavailability of two formulations was (102.1±10.9)%. The method is rapid, selective, robust and is proved to be suitable for bioequivalence evaluation of different formulations containing citalopram.     

人尿中美沙芬及其代谢产物的气—质联用分析

A GC-MS method for the analysis of dextromethorphan and its metabolites is described. The urine sample was hydrolyzed with HCl, extracted with diethyl ether and derivatized with MSTFA (N-methyl-N-trimethylsilyltrifluoroacetamide)-MBTFA (N-methyl-bistrifluoroacetamide). Dextromethorphan and its 3 metabolites were detected in urine samples within 2～60 h after administration of the drug. Their structures and the variation of their concentration in urine were determined. The detection limit of dextromethorphan is 10 ng.     

高效液相色谱法测定细辛及其制剂中马兜铃酸A的含量

目的:测定细辛药材及感特灵胶囊中肾毒性成分马兜铃酸A的含量.方法:建立高效液相色谱方法,以十八烷基硅烷键合硅胶为填充剂,乙腈-1%HAC(39:61,v/v)为流动相;检测波长为390nm;流速为1.0mL·min-1;柱温为室温.分别测定3种细辛样品以及成品制剂感特灵胶囊中马兜铃酸A的含量.结果:高效液相色谱法的平均回收率为101.24%,RSD%为0.27%;结论:细辛药材的根部含马兜铃酸A极少,感特灵胶囊中细辛含量远低于检测限.     

高效液相色谱法测定人血清中马兜铃酸Ⅰ、Ⅱ的含量

目的建立以高效液相色谱法测定人血清中马兜铃酸Ⅰ、Ⅱ含量的方法。方法色谱柱为C18(250mm×4.6mm,5μm),流动相为甲醇-水-冰醋酸(72∶27∶1),检测波长为250nm,流速为1.0ml/min。结果马兜铃酸Ⅰ、Ⅱ检测浓度线性范围分别为0.84~13.50μg/ml(r=0.9997,n=5)、2.03~32.50μg/ml(r=0.9994,n=5),最低检测浓度分别为0.3、0.1μg/ml。结论本方法简便、易行,可为临床诊治马兜铃酸肾病提供依据。     

Short-term toxicity of aristolochic acid, aristolochic acid-I and aristolochic acid-II in rats.

We compared the short-term toxicity of toxic components of aristolochic acid in rats. Twenty-four female Wistar rats were divided into 4 groups and treated orally every 3-days with 10 mg/kg each of aristolochic acid, aristolochic acid-I and aristolochic acid-II for 19 days. After treatment, the relative ratio of liver and kidney weight to body weight, the concentrations of RBC, hemoglobin and hematocrit in the blood, the levels of aspartate amino transferase, alanine amino transferase, alkaline phosphatase, blood urea nitrogen and creatinine in the plasma, and the levels of urinary urea nitrogen and creatinine in the urine were significantly increased. Body weight of rats and the levels of Na(+), K(+), Ca(2+) in the urine were significantly decreased, especially for groups treated with aristolochic acid and aristolochic acid-II. Pathological examination of liver and kidney also showed cell enlargement and lesions, especially for groups treated with aristolochic acid and aristolochic acid-II. The aristolochic acid exhibited significant toxicity, and the short-term toxicity of aristolochic acid-II and aristolochic acid was similar to each other. Renal but not hepatic failure induced by aristolochic acid could be prevented by pentoxifylline.     

含马兜铃酸中药的安全性探讨

目的 探讨含马兜铃酸中药的安全性,为临床合理用药提供参考.方法 通过检索国内外公开发表的文献和各国官方网站,收集与马兜铃酸有关的不良反应病例,分析其安全性.结果 与马兜铃酸有关的不良反应主要为肾损害,部分病例出现尿道上皮癌.结论 临床应重视含马兜铃酸药物的潜在肾毒性,保障人民用药安全.     

木通马兜铃化学成分研究

从木通马兜铃(Aristolochia manshuriensis Kom)茎皮中分得一个新化合物(5),经光谱(IR,UV,HRMS,^{1HNMR,NOEDS)鉴定为3,4-二甲氧基-10-硝基菲-1-羧酸甲酯,命名为马兜铃酸BII甲酯。另11个已知化合物是马兜铃酸Ⅰ,Ⅱ,Ⅲa,Ⅳ,Ⅳa,对羟基桂皮酸,β-谷甾醇,豆甾烷-3,6-二酮,6-羟基-豆甾-4-烯-3-酮,胡萝卜甙,二十八酸甘油单酯;其中二十八酸甘油单酯为首次从该属植物中分得。}     

HPLC测定关木通配伍前后马兜铃酸A煎出量的变化

目的 比较关木通配伍前后马兜铃酸A含量的差异,探讨龙胆泻肝汤配伍的合理性.方法 采用HPLC法,测定关木通单煎液与龙胆泻肝汤中马兜铃酸A的含量.结果 马兜铃酸A在0.76～51.00 μg·ml-1范围内线性良好,关木通单煎液和复方煎液的方法回收率分别为98.6%和96.5%;单煎液中马兜铃酸A的含量明显高于复方煎液(P＜0.05).结论 关木通在龙胆泻肝汤中配伍以后可以降低马兜铃酸A的煎出量.     

马兜铃酸类化合物使用现状及肾脏毒性研究进展

马兜铃酸类化合物是一类广泛存在于多种天然药物中的物质,具有抗病毒、抗炎等多种疗效.但是,较强的肾毒性阻碍了马兜铃酸类化合物更加广泛的利用.虽然已有部分药材被禁用,但至今仍有大量含有马兜铃酸类化合物的药材,故对马兜铃酸类化合物进行研究仍十分有必要.本文将对含有马兜铃酸类化合物的天然药物的使用现状和肾毒性研究进展进行综述.     

不同产地细辛中有效成分与马兜铃酸Ⅰ含量差异比较

目的：测定不同产地细辛及其不同入药部位中的肾毒性成分和有效成分的含量,优选出肾毒性成分含量低、有效成分含量高的细辛药材品种及产地。方法：HPLC法测定马兜铃酸Ⅰ及细辛脂素的含量;GC法测定甲基丁香酚含量。结果：不同产地细辛中,马兜铃酸Ⅰ含量以陕西宁强（华细辛）地下部分最高,为0.4528mg/g,以吉林通化（北细辛）地上部分最低,为0.0083mg/g;甲基丁香酚含量以吉林合龙（汉城细辛）地下部分含量最高,为1.35%,细辛脂素含量以吉林合龙（汉城细辛）地下部分含量最高,为3.92mg/g。结论：不同产地细辛马兜铃酸Ⅰ、细辛脂素、甲基丁香酚含量差异较大。