宾川乌头中的生物碱及其结构的研究

从云南药用草乌之一的宾川乌头(Aconitum duclouxii Levl)根中分得两种结晶性生物碱,称为碱A及碱B。经鉴定,碱B为乌头碱(aconitine)。碱A分子式为C₃₄H₄₇O₁₀N,熔点168～169℃,[α]_D^28.1+28.3(C,1.43,氯仿),此系一新生物碱,命名为宾乌碱(duclouxine),经光谱分析,初步推定其化学结构式为12-β-羟基查斯乌头碱(12-β-hydroxy chasmaconitine)。宾乌碱经初步药理试验说明有镇痛作用。     

黑翠碱甲和黑翠碱乙的化学结构

从黑水翠雀(Delphinium potaninii W.T.Wang)根中分得2个新的牛扁碱型C₁₉-二萜生物碱(I和II),由光谱分析(¹HNMR,¹³CNMR和MS)和化学方法,确定碱I为黑翠碱甲(potanidineA)、碱II为黑翠碱乙(potanidineB)。     

UPLC-MS/MS测定大鼠血浆中胡蔓藤碱乙和胡蔓藤碱丁及其药动学与生物利用度研究

目的 建立一种检测大鼠血浆中蔓藤碱乙和胡蔓藤碱丁的UPLC-MS/MS法，并研究大鼠口服和舌下静脉给药方式下胡蔓藤碱乙和胡蔓藤碱丁的药动学差异。方法 大鼠分别灌胃和舌下静脉注射蔓藤碱乙和胡蔓藤碱丁，在一定时间内取血，离心获得血清；士的宁为内标，通过UPLC-MS/MS来测定血清中蔓藤碱乙和胡蔓藤碱丁的浓度，绘制药-时曲线，计算药动学参数。结果 经灌胃给药5 mg·kg^–1，胡蔓藤碱乙的t_1/2为(5.7±1.2) h，AUC_(0-t)为(59.6±20.1) ng·h·mL^–1，CL/F为(89.1±30.5) L·h^–1·kg^–1，C_max为(18.3±5.3) ng·mL^–1；经舌下静脉给药1 mg·kg^–1后，胡蔓藤碱乙的t_1/2为(1.5±0.3) h，AUC_(0-t)为(140.2±37.4) ng·h·mL^–1，CL为(7.6±2.3) L·h^–1·kg^–1，C_max为(114.9±36.0) ng·mL^–1。经灌胃给药5 mg·kg^–1，胡蔓藤碱丁的t_1/2为(4.7±4.1) h，AUC_(0-t)为(44.3±5.1) ng·h·mL^–1，CL/F为(100.3±11.7) L·h^–1·kg^–1，C_max为(13.0±4.0) ng·mL^–1；经舌下静脉给药0.1 mg·kg^–1后，胡蔓藤碱丁的t_1/2为(1.1±0.4) h，AUC_(0-t)为(72.9±19.1) ng·h·mL^–1，CL为(1.4±0.4) L·h^-1·kg^–1，C_max为(43.7±6.8) ng·mL^–1。胡蔓藤碱乙的生物利用度为8.5%；胡蔓藤碱丁的生物利用度为1.2%。结论 胡蔓藤碱乙、胡蔓藤碱丁吸收迅速，半衰期较短。     

口服制川乌提取物后大鼠体内乌头类生物碱的组织分布

目的建立HPLC法测定口服制川乌提取物后大鼠体内乌头类生物碱的方法。方法用Waters 2690@996 PAD系统，Halsil 100 C₁₈柱(250 mm×4.6 mm ID, 5 μm)，水-甲醇-二乙胺(75∶25∶0.1)为流动相，流速0.9 mL·min^-1，检测波长240 nm。结果乌头碱在心脏、脾脏、肺脏、肾脏的线性范围：0.4-100 μg·mL^-1，r分别为0.997 2,0.998 6,0.999 3,0.999 4；在肝脏的线性范围：2-200 μg·mL^-1，r为0.999 0。次乌头碱在心、肝、脾、肺、肾、脑和脊髓的线性范围：5-100 μg·mL^-1，r分别为0.999 4,0.999 7,0.999 8,0.998 4,0.999 8,0.999 8和0.999 7。乌头碱及次乌头碱的检测限(S/N=3)为0.4 μg·mL^-1。各组织中的回收率：乌头碱为88.7%-102.2%，次乌头碱为865%-101.3%。结论本法为确证乌头类生物碱的中毒提供了科学有效的依据。     

东北延胡索中白元胡碱的化学结构

自东北延胡索Corydalis ambigna cham et Schltd(罂粟科)块茎的乙醚提取物中,分离出一种苯菲啶类新生物碱。根据其紫外光谱、红外光谱、核磁共振氢谱、碳谱和质谱的分析以及共衍生物的制备,并与苯菲啶类已知物紫堇灵(corynoline)及其衍生物的光谱数据进行比较,确定了该生物碱的化学结构为(Ⅰ),并命名为白元胡碱ambinine,C₂₃H₂₇O₆N,mp 218～219°,[α]_D²⁹—98°(c 0.11 CHCl₃)。     

平贝碱乙的分离和鉴定

本文报道了自东北平贝母(Fritillaria ussuriensis Maxim)中分得一种新的甾体生物碱,经光谱(IR,MS,¹HNMR及¹³CNMR)解析和衍生物制备,推定其结构为5α,17β,22α-cevanine-3 β,6α,12α,14α,16β,20β-hexol,定名为平贝碱乙。     

中国乌头的研究——ⅩⅩ.赣皖乌头的研究

本文报道了从赣皖乌头Aconitum finetianum Hand-Mazz的根中分到三个二萜类生物碱A.B.c。经鉴定B和C分别为lappaconitine和ranaconitine。碱A,C₃₂H₄₄N₂O₁₀,熔点220～221℃,[α]_D²²+44.7°(甲醇),为一个新生物碱,暂称赣乌碱finaconitine,经光谱推定化学结构为10-β-羟基-冉乌头碱。     

伊贝母中伊贝碱甙C的分离和结构鉴定

自吉林栽培的伊贝母(Fritillaria pallidiflora Schrenk)中分得一种新的甾体生物碱甙,命名为伊贝碱甙C(yibeinosideC)。根据红外、质谱、氢谱、碳谱、¹H-¹HCOSY和¹H-¹³CCOSY谱确定其结构为22,26-环亚胺胆甾-6-酮-3-O-β-D-吡喃葡萄糖-(1→4)-β-D-吡喃半乳糖甙(1)。     

十大功劳属部分植物茎中生物碱的高效毛细管电泳法测定

目的：对十大功劳属植物中3种生物碱的含量进行测定,为其内在质量的评价提供科学依据。方法：运用毛细管区带电泳(CZE)模式,以马钱子碱为内标化合物,测定了小檗碱、巴马亭和药根碱的含量。背景缓冲溶液为0.1 mol.L^-1磷酸缓冲液(pH 7.0)与甲醇(2∶1)的混合体系。线性范围：盐酸小檗碱为4.9～498.6 μg.mL^-1(γ=0.9990);盐酸巴马亭为5.0～504.9 μg.mL^-1(γ=0.9996);盐酸药根碱为5.1～505.8 μg.mL^-1(γ=0.9984)。回收率：盐酸小檗碱为96.00%～101.66%;盐酸巴马亭为100.15%～102.97%;盐酸药根碱为96.68%～102.44%。结果：不同品种、不同产地、不同采集时间的植物中的生物碱含量均有较大差别。结论：高效毛细管电泳法是中草药质量控制的一种简便、快速、有效的方法。十大功劳属多种植物生物碱含量较高,可作为新的药用资源。     

雷公藤倍半萜生物碱的分离与结构

从雷公藤(Tripterygiu mwilfordii Hook.f.)根皮中分离到二个倍半萜生物碱,即碱Ⅰ和碱Ⅱ,根据理化性质和光谱(UV,IR,MS,HRMS,^lHNMR,¹³CNMR(COM和OFR),¹H-¹HCOSY,¹H-¹³CCOSY,NOESY和COLOC]解析,鉴定生物碱Ⅰ为euonymine,生物碱Ⅱ为一种新的生物碱,命名为雷公藤明碱(wilfordsine)。初步药理实验证明雷公藤明碱有免疫抑制活性。     

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.     

New lignan glycosides from Cupressus duclouxian (Cupessaceae)

From the branches and leaves of Cupressus duclouxiana two new lignan glycosides named cupressoside A (1) and cupressoside B (2), together with matairesinoside (3), dihydrodehydrodiconiferyl alcohol (4), dihydrodehydrodiconiferyl alcohol-9-O-α-l-rhamnopyranoside (5), dihydrodehydrodiconiferyl alcohol-4-O-α-l-rhamnopyranoside (6), ( ? )-isolariciresinol (7) and ( ? )-isolariciresinol-9-O-β-d-xylopyranoside (8), were isolated. The structures of these compounds were determined on the basis of their HR-FAB-MS, IR, UV, ¹H and ¹³C NMR (DEPT), and 2D NMR (HMQC, HMBC, COSY, NOESY) spectral data.     

Two new compounds from Bombyx batryticatus

Two new compounds beauvericins M1 (1) and S1 (2) were isolated from Bombyx batryticatus. Their structures were established as (3α,6α)-3-benzyl-6-secbutyl-4-methylmorpholine-2,5-dione (1) and (5α,8α)-epidioxyergosterol-24-one-6,22-dien-3β-ol (2) by various spectroscopic techniques including 1D NMR (¹H NMR and ¹³C NMR), 2D NMR (HSQC, HMBC, ¹H–¹H COSY, NOESY), and HR-ESI-TOF-MS.     

Norditerpenoid alkaloids from Delphinium anthriscifolium

Two new norditerpenoid alkaloids with lycoctonine skeleton, anthriscifolcones A (1) and B (2), were isolated from the whole plant of Delphinium anthriscifolium var. Majus by extensive column chromatography. Their structures were established by IR, MS, ¹H NMR, ¹³C NMR, and 2D NMR methods (including HSQC, ¹H–¹H COSY, HMBC, and NOESY experiments).     

Two new secolignans from the roots of Urtica fissa

Two new secolignans, 3,4-trans-3-hydroxymethyl-4-[bis(4-hydroxy-3- methoxyphenyl)methyl]butyrolactone (1) and 3,4-trans-3-hydroxymethyl-4- [bis(3,4-dimethoxyphenyl)methyl]butyrolactone (2) have been isolated from the roots of Urtica fissa E.Pritz. Their structures were determined on the basis of spectroscopic methods, especially ¹H NMR, ¹³C NMR, 2D NMR, and HR-ESI-MS. The inhibitory effects on N1 and N2, two subtypes of neuraminidases (NAs), of these two compounds were assayed.     

Chemical constituents of Stellera chamaejasme L.

A new biflavanone, 7-methoxyneochamaejasmin A, and a new chromone derivative, isomohsenone, were isolated from the roots of Stellera chamaejasme L. The structures of two compounds were determined by means of ESI-MS, ¹H NMR and ¹³C NMR, especially 2D NMR spectral analyses.     

Seimisochromenes A and B: two new dihydroisochromenes from the endophytic fungus,Seimatosporium sp.

Two new dihydroisochromenes, named seimisochromenes A and B (1 and 2), were isolated from an endophytic fungus, Seimatosporium sp. The structures of seimisochromenes A and B have been determined from 1D (¹H and ¹³C NMR spectra) and 2D (COSY, HMQC, HMBC, and NOESY) NMR experiments.     

Novel Cationic Quinazolin‐4(3H)‐one Conjugated Fullerene Nanoparticles as Antimycobacterial and Antimicrobial Agents

A series of novel cationic fullerene derivatives bearing a substituted‐quinazolin‐4(3H)‐one moiety as a side arm were synthesized using the 1,3‐dipolar cycloaddition reaction of C₆₀ with azomethine ylides generated from the corresponding Schiff bases of substituted quinazolinones. The synthesized compounds 5a – f were characterized by elemental analysis, FT‐IR, ¹H NMR, ¹³C NMR, and ESI‐MS and screened for their antibacterial activity against Mycobacterium tuberculosis (H₃₇RV) and antimicrobial activity against selected Gram‐positive (Staphylococcus aureus and S. pyogenes) and Gram‐negative (Pseudomonas aeruginosa, Klebsiella pneumonia and Escherichia coli) bacterial and fungal strains (Candida albicans, Aspergillus clavatus, and A. niger), respectively. All the compounds exhibited significant activity, with the most effective compounds having MIC values and zones of inhibition comparable to those of standard drugs.     

Note: A new chromone from Ficus lyrata

A new chromone, named 5,6-dihydroxy-2-methylchromone (FL-2), along with seven known flavonoids, 5-hydroxy-7,3,3′,4′-tetramethoxyflavone (FL-3), 5,4′-dihydroxy-6,7,8-trimethoxyflavone (FL-4), 5,4′-dihydroxy-7,8-dimethoxyflavone (FL-5), 4-methoxychalcone (FL-6), 7,4′-dimethoxyapigenin (FL-7), 5,7,4′-trihydroxy-2′,3′,6′-trimethoxyisoflavone (FL-8?a rare flavonoid), acacetin-7-O-glucoside (FL-9) and acacetin-7-O-neohesperidoside (FL-10), and β-sitosterol-d-glucoside (FL-1) have been isolated from the leaves of Ficus lyrata. Their structures have been established on the basis of chemical and spectral evidence (IR, UV, ¹H NMR, ¹³C NMR and mass spectra).     

Study on chemical constituents of Cyclocarya paliurus

A new dammarane triterpenoid glycoside named cyclocarioside J (1) and other three known triterpenoid glycosides were isolated from the leaves of Cyclocarya paliurus. Based on ESI-MS, HR-ESI-MS, ¹H NMR, ¹³C NMR, and 2D NMR techniques including ¹H–¹H COSY, HMBC, HMQC, and NOESY correlations, the structure of cyclocarioside J was elucidated as (20S,24R)-epoxydammarane 3β,12β,25-trihydroxy-12-O-β-d-quinovopyranosyl-3-O-α-l-arabinopyranoside.