Determination of Camptothecin and 10-Hydroxycamptothecin in Camptotheca acuminata by LC-ESI-MS/MS

A rapid and sensitive liquid chromatography-tandem mass spectrometry method with multiple reaction monitoring was developed for the simultaneous determination of camptothecin and 10-hydroxycamptothecin in Camptotheca acuminata. The separation of camptothecin and 10-hydroxycamptothecin was performed on an Agilent Eclipse XDB-C18 column with a mixture of methanol and water (1:1, v/v) containing 0.2% formic acid as a mobile phase. The limits of detection of camptothecin and 10-hydroxycamptothecin were 4.0 ng/mL and 7.0 ng/mL (S/N = 3), respectively. Analysis took 10 minutes, making the method suitable for rapid determination of camptothecin and 10-hydroxycamptothecin in C. acuminata.     

反相高效液相色谱法测定喜树果中喜树碱的含量

采用反相高效液相色谱法,在Kromasil C18色谱柱(5 μm,250 mmx4.6 mm i.d.)上,以甲醇-水(体积比为60∶40)为流动相分离测定了喜树果中的喜树碱。流动相的流速为0.8 mL/min,紫外检测波长为254 nm。样品前处理中,采用了超临界CO2萃取(乙醇作提携剂)、甲醇-氯仿温浸的方法从喜树果中提取喜树碱。实验结果表明,该法的平均回收率为95.8%-100.8%,相对标准偏差为1.2%-2.0%。方法快速、准确,可用于实际样品的测定。     

Simultaneous determination of camptothecin and 10‐hydroxycamptothecine in the Camptotheca acuminate,its medicinal preparation and in rat plasma by liquid chromatography with fluorescence detection

Camptotheca acuminata Decne is an important medicinal plant that contains various cytotoxic alkaloids, such as camptothecine (CPT) and 10‐hydroxycamptothecine (HCPT). A rapid and sensitive liquid chromatography with fluorescence detection (LC‐FLD) method for the quantification of CPT and HCPT is described. The separation was carried out on a DL‐C_l8 column (4.6 × 150 mm, 5 µm), with the mobile phase of acetonitrile–sodium dihydrogen phosphate buffer (10 mm ) using an gradient elution at the flow rate of 0.6 mL/min. The LC‐FLD method was validated for linearity, sensitivity, accuracy and precision, and then used to determine the content of the above components. The lower detection limits of CPT and HCPT were 0.4 and 0.1 ng/mL, respectively. The precision was <1.58% and the mean recovery of the analytes was 96.0–98.6%. The LC‐FLD method was successfully applied to determine CPT and HCPT in real samples including C. acuminate, HCPT injection and rat plasma. Copyright © 2015 John Wiley & Sons, Ltd.     

Chemical Constituents of the Endophytic Fungal Strain Phomopsis sp. NXZ‐05 of Camptotheca acuminata

From the endophytic fungal strain Phomopsis sp. NXZ‐05 of Camptotheca acuminata Decne . (Nyssaceae), six new compounds were isolated, including the ten‐membered macrolides 1 – 4 and their (known) parent compound multiplolide A ( 7 ), as well as a new unsaturated fatty acid, (4E)‐6,7,9‐trihydroxydec‐4‐enoic acid ( 5 ) and its methyl ester 6 . Their structures were elucidated by spectroscopic and mass‐spectrometric analyses, including 1D‐ and 2D‐NMR experiments and HR‐ESI‐MS, and their biological activities were elucidated.     

A new dihydrochalcone glycoside from the stems of Homalium stenophyllum

A new dihydrochalcone glycoside, phloretin-4-O-β-D-glucopyranoside (1), together with seven known flavonoids (2–8), were isolated from the stems of Homalium stenophyllum. The structure of 1 was elucidated by extensive spectroscopic methods and the known compounds were identified by comparisons with data reported in the literature. The known compounds (2–8) were isolated from the genus Homalium for the first time. All compounds were evaluated for their antibacterial activities against six pathogenic bacteria in vitro.     

Conformational Analysis of Germacrane Sesquiterpene Lactones. 1(10)Z,4E- and 1(10)E,4Z-Germacranolides

Molecular mechanics was used to study the structures of 1(10)Z,4E- and 1(10)E,4Z-germacranolides. Possible conformers, their probabilities, and barriers to conformational transitions were determined     

A new xanthone glycoside from Pyrrosia sheareri

A new xanthone glycoside, 3,5,7,8-tetramethoxyxanthone-1-O-β-D-glucopyranoside (1), along with five known compounds, mangiferin (2), kaempferol (3), quercetin (4), chlorogenic acid (5) and diploptene (6), was isolated from the whole plants of Pyrrosia sheareri (Bak.) Ching. The structure of compound 1 was established on the basis of extensive spectroscopic analyses and chemical methods.     

A Phenolic Glucoside from Alangium plantanifolium

Alangium, the sole genus in the family Alangiaceae, has a variety of about 20 species distributed in the tropical and subtropical area of the Eastern Hemisphere, and 13 species are known to occur in the south of China1. A. plantanifolium and A. chinense are used in chinese traditional medicine for the treatment of rheumatalgia, paralysis, cardianeuria, and wound2. Pharmacological studies of the extracts of these two species showed muscular relaxing activity, and anabasine was considered as t…     

Ailanthus altissima (Miller) Swingle fruit - new acyl β-sitosteryl glucoside and in vitro pharmacological evaluation

β-Sitosterol-3-O-(6?-O-13?-octadecenoyl)-β-D-glucoside (1), a new acyl β-sitosteryl glucoside, along with three known compounds β-sitosterol-3-O-β-D-glucoside (2), β-sitosterol (3) and methyl gallate (4) have been isolated from the ethyl acetate soluble fraction of methanolic extract of Ailanthus altissima fruits. Their structures were elucidated through spectroscopic data including 2D NMR, ESI-MS, methanolysis and oxidative cleavage of double bond. Antibacterial, antifungal, cytotoxic, phytotoxic and insecticidal activities were evaluated of compound 1, crude extract and its fractions so far for the first time. Pharmacological activities results showed that n-butanol fraction was good active against Pseudomonas aeruginosa and Salmonella typhi bacteria, and moderate active against Microsporum canis fungus. Crude extract, n-butanol and aqueous fractions showed good cytotoxicity. Moreover, compound 1, extract and all fractions showed notable phytotoxicity at higher concentrations, whereas all inactive against assayed insects.     

Two New Iridoid Glucosides from Lagotis yunnanensis

Two new iridoid glucosides 1 and 2, 10-O-(3, 4-dimethoxy-(E)-cinnamoyl)catalpol and 10-O-(3, 4-dimethoxy-(Z)-cinnamoyl)catalpol, were isolated from Lagotis yunnanensis. Their structures were elucidated by spectroscopic methods.     

A New Iridoid Glucoside from Lagotis yunnanensis

Phytochemical investigation of Lagotis yunnanensis led to the isolation andidentification of a new iridoid glucoside 1, named as 10-O-(3, 4-dimethoxy-(E)-cinnamoyl)aucubin.Its structure was elucidated by spectroscopic methods.     

A new proline-containing flavonol glycoside from Caragana leucophloea Pojark

One new proline-containing flavonol glycoside, namely kaempferol-3-O-methyl-7-O-β-d-glucopyranosyl-8-(1-methyleneproline)-4′-O-β-d-glucopyranoside (1), together with 15 known flavonoids, 3-O-methylkaempferol (2), 3-O-methylquercetin (3), quercetin (4), kaempferol (5), apigenin (6), rhamnazin (7), astragalin (8), alquds (9), quercitrin (10), rutin (11), isoquercitrin (12), apigetrin (13), myricitrin (14), hesperidin (15) and calycosin-7-O-β-d-glucopyranoside (16) were isolated from the aerial parts of Caragana leucophloea Pojark. (Leguminosae). Their structures were determined on the basis of spectroscopic analyses and by comparison with literature data. Compounds 2–4 revealed a strong antimicrobial activity with minimum inhibitory concentration values of 12.5–150 μg/mL and median inhibitory concentration (IC₅₀) values of 7.42–76.61 μg/mL. Compounds 3, 4, 6–8, 10–12 and 14 showed strong antioxidant activity. Compounds 2–7 exhibited moderate antinematodal activity on Caenorhabditis elegans with IC₅₀ values of 40.51–68.05 μg/mL.     

Terpenoids from the barks of Magnolia maudiae (Dunn) Figlar

A new germacrenolide (1) and fourteen known terpenoids (2–15) were isolated from the barks of Magnolia maudiae (Dunn) Figlar (Magnoliaceae). The structure of (7αH,11βH)-2α,8α-dihydroxy-4α,5β-epoxy-germacr-1(10)-en-6α,12-olide (1) was elucidated by physical and spectroscopic data analysis, including 1D, 2D NMR and HR-ESI-MS. Lyratol F (9) was isolated from Magnolia for the first time. The structures of known compounds were established by comparing their spectroscopic data with those in literatures.     

Effect of Epoxidation of Carbocyclic Double Bonds on Conformational Flexibility of 1(10)E,4E-Germacranolides

The effect of substitution of double bonds by epoxy groups in 1(10)E,4E-germacranolides is studied by molecular mechanics. The probabilities of forming conformers in the epoxy derivatives are determined. Barriers to possible conformational transitions are estimated     

Syntheses and crystal structures of two maleonitriledithiolate complexes containing the 1-(R-benzyl)pyrazinium cation (R = 4′-nitro or 4′-bromo)

The complexes [NO₂BzPz]₂[Ni(mnt)₂] (1) and [BrBzPz]₂[Pd(mnt)₂] (2) have been prepared by reaction of Na₂mnt, NiCl₂·6H₂O or PdCl₂, and the corresponding 1-(R-benzyl)pyrazinium bromide salt (R = 4′-nitro, R = 4′-bromo). Crystallographic data for 1: monoclinic, P2₁/n, a = 7.3494(15), b = 15.223(3), c = 15.054(3)?Å, β = 102.42(3)°, V = 1644.8(6)?ų, Z = 2. Data for 2: monoclinic, P2₁/n, a = 7.399(2), b = 19.024(4), c = 12.224(2)?Å, β = 94.62(3)°, V = 1715.0(7)?ų, Z = 4. In both complexes, the [M(mnt)₂]^2? anion has a centre of symmetry at the metal atom and two cations are related to each other by the symmetry centre. The [M(mnt)₂]^2? anion exhibits a quasi-planar structure in both complexes, which show similar crystal packing.     

7,8-二甲基-10-(D-1-核糖醇基)-异咯嗪半合成中间体气相色谱分析

提出以三氟乙酸酐作为衍生化试剂,将核黄素半合成中问体N-(D)-脱氧核糖醇基-3,4-二甲苯胺(Ⅰ)及4,5-二甲基-N-(D)-脱氧核糖醇基-2-偶氮苯基苯胺(Ⅱ)转化为低沸点易汽化物质,采用以苯乙酮作内标,测定中间体(Ⅰ)和(Ⅱ)纯度的气相色谱法.方法具有分析速度快、准确度高、重现性好等优点,方法回收率(Ⅰ)为96.9%～101.2%、(Ⅱ)为99.4%～100.4%,相对标准偏差(Ⅰ)在4.4%、(Ⅱ)在2.6%以内.     

A new 3-(3,4-methylenedioxyphenyl)-propane-1,2-diol glycoside from the roots of Cinnamomum camphora

A new 3-(3,4-methylenedioxyphenyl)-propane-1,2-diol glycoside,named cinnamomdiol A(1),together with two known compounds,3-(3,4-methylenedioxyphenyl)-propane-1,2-diol(2) and taxifolin(3),was isolated from the roots of Cinnamomum camphora.Their structures were determined on the basis of spectroscopic evidences.Compounds 2 and 3 were isolated from the title plant for the first time.     

Synthesis of New Porphyrin-Containing Peptidyl Phosphonates

Synthesis of new, porphyrin-containing peptidyl aminophosphonates is described. The products, derived from 5-(4′-carboxyphenyl)-10,15,20-tri-p-tolylporphyrin and some heterocyclic aminophosphonates were obtained in high yield in the reaction of the 5-(4′-carboxyphenyl)-10,15,20-tritolylporphyrin with selected thiophene and pyridine aminophosphonate diphenyl esters by applying a DCC coupling method used in the peptide synthesis. The obtained porphyrin aminophosphonate products were characterized by spectroscopic methods.