消炎止痢灵薄膜衣基片工艺研究

通过正交法对消炎止痢灵薄膜衣基片生产的主要影响因素,进行优选,确定淀粉浆浓度为14％;苦参生药粉与浸膏粉比例1：4;原辅料细度140目为最佳工艺条件。用该工艺条件生产的消炎止痢灵基片硬度与光洁度均符合消炎止痢灵薄膜衣技术要求,为消炎卡痢灵糖衣片改为薄膜衣片提供基础材料。     

止痢颗粒抗菌作用及急性毒性实验的研究

目的:研究止痢颗粒对大肠杆菌和痢疾杆菌感染小鼠的抗菌作用及对小鼠的急性毒性实验。方法:将小鼠随机分为阴性对照、阳性对照、止痢颗粒(2.5g.kg-1、5.0g.kg-1、10.0g.kg-1)5组,各组小鼠均腹腔注射(ip)一定量菌液,半小时后灌胃给药,每日1次,连续7天,记录各组小鼠死亡数。结果:止痢颗粒在5.8g.kg-1剂量时对大肠杆菌感染小鼠有明显的保护作用;在10.0g.kg-1剂量时对痢疾杆菌感染小鼠有明显的保护作用。急性毒性实验表明小鼠口服最大给药量相当于临床用量(15g/袋)104倍,口服安全。结论:止痢颗粒具有明显抗菌作用,口服安全无毒。     

速效止痢片中黄芩及马齿苋的薄层鉴别

速效止痢片收载于辽宁省药品标准(87年版),由磺胺脒、甲氧苄氨嘧啶、黄芩和马齿苋4味药组成,其质量控制仅有2味西药,本文采用薄层色谱法对速效止痢片中的黄芩和马齿苋进行了鉴别[1]。1　材料和试药速效止痢片,市售。黄芩、马齿苋经辽宁省药检所鉴定为正品。黄芩苷、酒石酸去甲肾上腺素、甲氧苄氨嘧啶由中国药品生物制品检定所提供。硅胶Ｇ:青岛海洋化工厂产品。其它试剂均为分析纯。磺胺脒由辽宁开原制药厂提供。2　薄层鉴别方法21　黄芩苷的薄层鉴别211　供试品溶液的制备　取速效止痢片5片,研碎,加乙醇20ｍＬ加热回流1ｈ,放冷过滤,滤液浓…     

HPLC法测定消炎止痢灵片中氧化苦参碱的含量

目的建立HPLC法测定消炎止痢灵片中氧化苦参碱的含量。方法采用KromasiL C18(200mm×4.6mm,5μm)柱,流动相为乙腈-甲醇-水(10∶5∶85),检测波长为220nm。结果测得线性范围为32~160μg(r=0.9998),平均回收率为99.26%,RSD为0.7%(n=5)。结论本方法方便,准确,可作为消炎止痢灵片的质量控制方法。     

凉血止痢汤合利福平治疗血痢临床观察

血痢是中医痢疾中的一种,临床以痢下鲜血或赤多白少为特征。笔者自1995～2001年,应用自拟凉血止痢汤配合利福平治疗血痢,疗效显著,现报告如下。1 临床资料 本文共27例,男17例,女10例。年龄6～72岁。其中住院病例15例,门诊病例12例。全部病例根据临床症状和大便常规检查确诊,均有腹痛、腹泻鲜血便,伴里急后重,左下腹压痛。发     

HPLC法测定消炎止痢灵片中甲氧苄啶的含量

本文建立测定消炎止痢灵片中甲氧苄啶含量的高效液相色谱法。样品经70%乙醇溶液超声处理30分钟提取,用微孔滤膜(0.45μm)滤过,即得。实验表明甲氧苄啶在0.1002～3.002μg范围内与峰面积值呈良好的线性关系(相关系数为0.9999);稳定性试验(n=5)RSD为0.51%;重复性试验(n=6)RSD为0.79%;平均回收率(n=6)为99.59%,RSD为0.22。该法样品处理起来简单,准确性高,精密度好,适合消炎止痢灵片中甲氧苄啶的含量测定。     

野牡丹止痢片的质量标准

目的：建立野牡丹止痢片的质量标准。方法：采用TLC法对野牡丹进行鉴别;用HPLC法对野牡丹中没食子酸进行含量测定,色谱柱：Thermo BDS HYPERSIL C18（250mm×4．6mm,5μm）,流动相：甲醇-0．1％甲酸（5：95）,检测波长：272nm,流速：1．0ml·min^-1。结果：本品鉴别薄层色谱特征明显;没食子酸线性范围0．12～1．6μg（r=0．9999）,平均回收率为100．6％（RSD=1．3％,11=9）。结论：鉴别和含量测定方法准确可行,重复性好,可作为药品标准控制野牡丹止痢片的质量。     

止痢汤加甲氧苄氨嘧啶短疗程治疗细菌性痢疾的效果

我院采用止痢汤加氧苄氨嘧啶(TMP)短疗程治疗急性细菌性痢疾(菌痢)944例。     

双波长HPLC法同时测定止痢宁片中穿心莲内酯和脱水穿心莲内酯的含量

目的:建立高效液相色谱法同时测定止痢宁片中穿心莲内酯和脱水穿心莲内酯含量的方法.方法:色谱柱:CAPCELL PAK-C18柱(150 mm×4.6 mm,5 μm);流动相:甲醇-水(48:52);流速为1.0 ml·min-1;柱温:30℃;检测波长:225 nm(穿心莲内酯)、250 nm(脱水穿心莲内酯);进样量:5 μl.结果:穿心莲内酯在4.17～41.68 μg·ml-1 (r=0.999 9)、脱水穿心莲内酯在4.04～40.40 μg·ml-1(r=0.999 9)浓度范围内线性关系良好;穿心莲内酯回收率为99.21%(RSD=1.3%,n=6),脱水穿心莲内酯回收率98.73%(RSD=1.1%,n=6).结论:该方法简单、准确,可作为止痢宁片的质量控制.     

清热止痢合剂质量标准提升研究

目的提升清热止痢合剂的质量标准。方法采用薄层色谱(TLC)法对清热止痢合剂中的白头翁、儿茶、关黄柏、黄连、黄芩进行定性鉴别;采用高效液相色谱(HPLC)法测定没食子酸、葛根素、芍药苷、黄芩苷的含量。结果白头翁、儿茶、关黄柏、黄连、黄芩TLC特征斑点清晰,分离度好,专属性强;没食子酸、葛根素、芍药苷、黄芩苷的质量浓度分别在4.557 1~41.014 3μg/m L,3.450 0~31.050 0μg/m L,10.907 1~98.164 3μg/m L,18.500 0~166.500 0μg/m L范围内与峰面积线性关系良好(r≥0.999 4),平均加样回收率分别为100.43%,100.71%,98.28%,100.65%,RSD分别为0.86%,1.60%,0.84%,1.16%(n=6)。结论该方法准确可靠,重复性好,可用于清热止痢合剂的质量控制。     

Rearranged Abietane Diterpenoids from Clerodendrum Mandarinorum

Abstract

Five new abietane derivatives which have a commonly rearranged abietane skeleton contained a 17(15 → 16),18(4 → 3)-diabeo-abietane framework, mandarones D–H, were isolated from the stem of Clerodendrum mandarinorum Diels (Verbenaceae). The structures were characterized as (16S)-12,16-epoxy-11-hydroxy-17(15 → 16),18(4 → 3)-diabeo-abieta-3,5,8,11,13-pentaene-7-one (mandarone D, 1), 12,16-epoxy-11,14-dihydroxy-17(15 → 16),18(4 → 3)-diabeo-abieta-3,5,8,11,13,15-hexaene-7-one (mandarone E, 2), 12,16-epoxy-6,11,14-trihydroxy-17(15 → 16),18(4 → 3)-diabeo-abieta-3,5,8,11,13,15-hexaene-7-one (mandarone F, 3), 12,16-epoxy-11,14-dihydroxy-6-methoxy-17(15 → 16),18(4 → 3)-diabeo-abieta-3,5,8,11,13,15-hexaene-2,7-dione (mandarone G, 4) and 12,16-epoxy-11,14-dihydroxy-17(15 → 16),18(4 → 3)-diabeo-abieta-3,5,8,11,13,15-hexaene-1,7-dione (mandarone H, 5) respectively, mainly based on the spectral analysis and by comparison with those of closely related compounds.     

Rearranged abietane diterpenoids from Clerodendrum mandarinorum

Five new abietane derivatives which have a commonly rearranged abietane skeleton contained a 17(15 → 16),18(4 → 3)-diabeo-abietane framework, mandarones D-H, were isolated from the stem of Clerodendrum mandarinorum Diels (Verbenaceae). The structures were characterized as (16S)-12,16-epoxy-11-hydroxy-17(15 → 16),18(4 → 3)-diabeo-abieta-3,5,8,11,13-pentaene-7-one (mandarone D, 1), 12,16-epoxy-11,14-dihydroxy-17(15 → 16),18(4 → 3)-diabeo-abieta-3,5,8,11,13,15-hexaene-7-one (mandarone E, 2), 12,16-epoxy-6,11,14-trihydroxy-17(15 → 16),18(4 → 3)-diabeo-abieta-3,5,8,11,13,15-hexaene-7-one (mandarone F, 3), 12,16-epoxy-11,14-dihydroxy-6-methoxy-17(15 → 16),18(4 → 3)-diabeo-abieta-3,5,8,11,13,15-hexaene-2,7-dione (mandarone G, 4) and 12,16-epoxy-11,14-dihydroxy-17(15 → 16),18(4 → 3)-diabeo-abieta-3,5,8,11,13,15-hexaene-1,7-dione (mandarone H, 5) respectively, mainly based on the spectral analysis and by comparison with those of closely related compounds.     

Triterpenes and xanthones from the stem bark of Garcinia tetralata

A new compound, 3β,18,19β-trihydroxylupane, was isolated from Garcinia tetralata, along with five known compounds, garcinexanthone B, morolic acid acetate, toxyloxanthone A, 6,11-dihydroxy-2,2-dimethylpyrano[3,2-c]xanthen-7(2H)-one, and 1,4-dihydroxy-5,6-dimethoxy-xanthone. The structure of the new compound was established by extensive spectroscopic techniques.     

Anti-lymphangiogenic diterpenes from the bark of Calocedrus macrolepis var. formosana

Eight new diterpenes, 6α,7β-dihydroxyferruginol (1), 6α,7α-dihydroxyferruginol (2), 6α-hydroxyhinokiol (3), 4α-hydroxy-7-oxo-18-norabieta-8,11,13-trien-4α-ol (4a), 15,16-dehydrosugiol (5), 7-methoxy-6,7-secoabieta-8,11,13-triene-6,12-diol (6), 7α-acetoxyabieta-8,12-diene-11,14-dione (7), 7α-butyloxyethyloxyabieta-8,12-diene-11,14-dione (8), along with four known compounds, 6,7-dehydroferruginol (9), 12-hydroxy-6,7-secoabieta-8,11,13-triene-6,7-dial (10), 7α-11-dihydroxy-12-methoxy-8,11,13-abietatriene (11), and 11,14-dihydroxy-8,11,13-abietatrien-7-one (12) were successfully isolated from the bark of Calocedrus macrolepis var. formosana. The structures of all isolates were elucidated by physical data (appearance, UV, IR, optical rotation) and spectroscopic data (1D, 2D NMR, and HREIMS). Compounds 9, 10, 11, and 12 showed promising growth-inhibitory effect on human lymphatic endothelial cells (LECs). Among these compounds, compound 10 exerted the most potent anti-lymphangiogenesis property by suppressing cell growth and tube formation of LECs. In conclusion, the results revealed the anti-lymphangiogenic potentials of Formosan C. macrolepis var. formosana.     

Parathesilactones and Parathesiquinones from Branches of Parathesis amplifolia.

Abstract

Three new lactone derivatives, (3E.)-5,6-dihydroxy-3-(3-hydroxy-4-nonyl-5-oxofuran-2(5H.)-ylidene)-7-nonyl-1-benzofuran-2(3H.)-one (1), (3E.)-5,6-dihydroxy-3-(3-hydroxy-4-decyl-5-oxofuran-2(5H.)-ylidene)-7-decyl-1-benzofuran-2(3H.)-one (2), and (3E.)-5,6-dihydroxy-3-(3-hydroxy-4-undecyl-5-oxofuran-2(5H.)-ylidene)-7-undecyl-1-benzofuran-2(3H.)-one (3), denominated as parathesilactones A, B, C, respectively, and two new quinone derivatives, (2,7,8-trihydroxy-3,6-didecyldibenzo[b,d.]furan-1,4-dione (4) and (2,7,8-trihydroxy-3,6-dinonyldibenzo[b,d.]furan-1,4-dione) (5), denominated as parathesiquinones A, B, respectively, were isolated from the branches of Parathesis amplifolia. Lund. (Myrsinaceae). In addition, three known triterpenes, α.-amyrin (6), β.-amyrin (7), and bauerenol (8), and four known alkenylresorcinols, 5-pentadec-8-enyl resorcinol (9), 5-pentadec-10-enyl resorcinol (10), 5-heptadec-8-enyl resorcinol (11), and 5-heptadec-10-enyl resorcinol (12), were also isolated. The structure elucidation was achieved by means of MS, GC-MS, IR, ¹H, ¹³C spectroscopy including Heteronuclear Multiple Quantum Coherence (HMQC), and Heteronuclear Multiple Bond Correlation (HMBC) techniques.     

5α-△9(11)-16α-甲基-3β,17α,21-三羟基-孕甾烯-3β,21-双醋酸酯-20酮的微生物转化

简单节杆菌A₁及耻垢杆菌MS₁两种菌混合培养转化地塞米松中间体5α-△⁹⁽¹¹⁾-16α-甲基-3μ,17μ,21-三羟基-孕甾烯-3μ,21-双醋酸酯-20酮(Ⅲ)可得到16α-甲基-△^1.4.0(11)-孕甾烯-17α,21-双羟基-3,20双酮(Ⅳ)(65%收率)及少量的16α-甲基-△^1.4孕甾烯-9α,11α-环氧-17α,21双羟基-3,20双酮(Ⅴ)。     

A new ceramide from <Emphasis Type="Italic">Ramaria botrytis</Emphasis> (Pers.) Ricken

A new ceramide, (2S,2′R,3R,4E,8E)-N-2′-hydroxyoctadecanoyl-2-amino-9-methyl-4,8-heptadecadiene-1,3-diol (1), was isolated together with four known sterols, 5α,6α-epoxy-3β-hydroxy-(22E)-ergosta-8(14),22-dien-7-one (2), ergosterol peroxide (3), cerevisterol (4) and 9α-hydroxycerevisterol (5), from the fruiting bodies of Ramaria botrytis (Pers.) Ricken (Ramariaceae). The structure of the new compound was elucidated based on spectral data.     

金疮小草化学成分的分离与鉴定

目的对金疮小草的化学成分进行研究。方法采用硅胶吸附柱色谱、ODS柱色谱、制备薄层色谱和半制备型高效液相色谱分离纯化,根据1H-NMR、13C-NMR等谱学数据进行结构鉴定。结果从金疮小草干燥全草的甲醇提取物的乙酸乙酯萃取物中分离得到15个单体化合物,分别鉴定为ajugacumbin A(1)、ajugacumbin B(2)、ajuganipponin B(3)、ajugamarin F4(4)、ajugarin I(5)、ajugamarin A1(6)、ajugamarin A1 chlorhydrin(7)、芹菜素(apigenin,8)、木犀草素(luteolin,9)、金合欢素(acacetin,10)、咖啡酸甲酯(methyl caffeate,11)、4-hydroxy-4-(3-oxo-1-butenyl)-3,5,5-trimethylcyclohex-2-en-1-one(12)、香草酸(vanillic acid,13)、黑麦草内酯(loliolide,14)和(10E,15Z)-9,12,13-trihydroxyoctadeca-10,15-dienoic acid(15)。结论其中化合物11和12为首次从筋骨草属中分离得到,化合物7和15为首次从金疮小草中分离得到。     

瘿花香茶菜二萜成分的研究

从瘿花香茶菜Rabdosia rosthornii(Diels)Hara的叶和茎中分离出三种二萜类化合物。其中两种为已知化合物ponicidin和oridonin。另一种为新的二萜化合物。通过理化常数和光谱的分析以及衍生物的制备,测定了其结构,并命名为瘿花香茶菜甲素。     

5α-△9(11)-16β-甲基-3β,17α,21-三羟基-孕甾烯-3β,21-双醋酸酯-20酮和5α,17α-甲基-17β-羟基-雄甾-3酮的微生物转化

用诺卡氏菌与节杆菌混合菌种转化从蕃麻皂素制得的中间体5α-△⁹⁽¹¹⁾-16-16β-甲基-3β,17α,21三羟基孕甾烯-3β,21-双醋酸酯-20酮(Ⅰ)得50%的16β-甲基-△^1,4,9(11)-孕甾三烯-20酮(Ⅱ)和少量的16β-甲基-9,11α环氧-△¹,4孕甾二烯-20酮(Ⅲ)。另外,又用同样的混合菌种转化从剑麻皂素制得的中间体5α,17α甲基-17β羟基-雄甾-3酮(Ⅳ)得50%17α甲基-17β羟基-△^1,4-雄甾二烯-3酮(Ⅴ)。如改变培养基则得3,17β-羟基-17α-甲基-9酮基-9,10开环-1,3,5(10)雄甾三烯化合物。