Seasonal variation of colchicine content in Colchicum brachyphyllum and Colchicum tunicatum (Colchicaceae)

As part of our continuing investigation of Jordanian Colchicum species, (-)-colchicine content in C. brachyphyllum Boiss. & Haussk. ex Boiss and Colchicum tunicatum Feinbr (Colchicaceae), growing wild in Jordan, was determined during different growth stages. Using external reference standard, a reverse-phase gradient photo-diode array high performance liquid chromatography (PDA-HPLC) method was adapted. Underground parts in both species and during different growth stages, always showed higher (-)-colchicine content than the above ground parts. In C. brachyphyllum total (-)-colchicine content of underground parts during flowering stage was found to be about 0.15% (wt/wt), while that of aerial parts was only about 0.04% (wt/wt). In C. tunicatum total (-)-colchicine content of underground parts was found to be 0.12% (wt/wt), and 0.13% (wt/wt) during flowering and vegetating stages, respectively, while that of aerial parts was only about 0.04% (wt/wt) and 0.02% (wt/wt), respectively. In C. tunicatum, stems, roots and unripe seeds are the main storages of (-)-colchicine at flowering, vegetating and seeding stages, respectively, while in C. brachyphyllum, corms are the main storage of (-)-colchicine at flowering and seeding stages.     

Phytochemical studies and cytotoxicity evaluations of Colchicum tunicatum Feinbr and Colchicum hierosolymitanum Feinbr (Colchicaceae): two native Jordanian meadow saffrons

As a part of our continuing investigation of Jordanian Colchicum species, the biologically active components of Colchicum hierosolymitanum Feinbr and Colchicum tunicatum Feinbr (Colchicaceae) were pursued. The brine shrimp lethality test (BSLT) was used to direct the fractionation and isolation of active components. Five and four known colchicinoids were isolated and characterized from C. tunicatum and C. hierosolymitanum, respectively. The known colchicinoids, reported for the first time from these two species are: (-)-colchicine (I), 3-demethyl-(-)-colchicine (II), (-)-cornigerine (III), beta-lumicolchicine (IV), and (-)-androbiphenyline (V) from C. tunicatum, and (-)-colchicine (I), 2-demethyl-(-)-colchicine (VI), (-)-cornigerine (III), and beta-lumicolchicine (IV) from C. hierosolymitanum. The chemical structures of the isolated compounds have been elucidated using a series of spectroscopic and spectrometric techniques principally; 1D-NMR (1H and 13C) and low resolution EI-MS and APCIMS. All pure compounds were evaluated for cytotoxicity against three human cancer cell lines; MCF-7 human breast carcinoma, NCI-H460 human large cell lung carcinoma, and SF-268 human astrocytoma. (-)-Colchicine (I) and (-)-cornigerine (III) were found to be the most bioactive of the identified compounds with EC50 values in the range of 0.016-0.097 microM.     

Development and optimization of a stability indicating method on a monolithic reversed-phase column for Colchicum dry extract

This article presents a method developed on a monolithic reversed-phase column for separation of related alkaloids and degradation products from colchicine in dry extract preparations from Colchicum seeds. Optimization was performed using an optimization software with variation of the pH of the mobile phase and the percentage of organic modifier. This method permits for the first time a fast separation of all alkaloids including colchiceine without prior derivatization or complexation with excellent linearity, precision and low limits of quantitation which makes it a suitable method for stability testing of extracts or drug formulations containing extracts of Colchicum seeds.     

POSSIBLE IN VIVO FORMATION OF LUMICHOLCHICINES FROM COLCHICINE BY ENDOGENOUSLY GENERATED TRIPLET SPECIES

Abstract In Colchicum autumnale L., colchicine is accompanied by its photoproducts, mainly β-lumicholchicine, even in parts not exposed to light such as the corm of plants grown in the dark. The transformation of colchicine into lumicolchicines can be efficiently accomplished in vitro by energy transfer from enzyme-generated triplet species to colchicine, thus providing additional evidence for'photobiochemistry without light'.     

The natural abundance of 13C, 15N, 34S and 14C in archived (1923-2000) plant and soil samples from the Askov long-term experiments on animal manure and mineral fertilizer

The Askov field experiment (Denmark), established in 1894, provides a unique opportunity to examine long-term effects of animal manure and mineral fertilizer on soil organic matter quality and turnover. This sandy loam soil is classified as Alfisol (Typic Hapludalf). Soil C, N, S, 13C, 15N, 34S and 14C contents were measured in a selection of archived soil samples (1923, 1938, 1945, 1953, 1964, 1976, 1985, 1996 and 2000) from unfertilized (O), animal manure (1 AM) and mineral fertilizer (1 NPK) treatments. These treatments are imbedded in a four-course crop rotation of winter cereals, root crops, spring cereals and a clover/grass mixture. The contents of C, N, S, 13C, 15N and 34S in selected crop samples (1953-1996) and in contemporary samples of animal feed and manure were also determined. Temporal soil nutrient and isotope trends between fertilizer treatments were significantly different, except for S content in 1 AM and 1 NPK. The total soil C and S was higher in 1 AM and 1 NPK than in the O treatment. The total soil N content (1 AM>1 NPK>O) and the delta15N content (1 AM>1 NPK and O) were also different. Analyses of plant, animal feed and manures confirmed that differences in soil 15N values were related to delta15N values of added source inputs. Soil and crop delta13C values were similar, but manures had slightly lower values. The variation of soil delta34S (and total S) from 1923 to 1996 was larger in the O than 1 AM and 1 NPK plots reflecting changes in atmospheric S inputs. The total contents of soil C, N and S were significantly correlated, but their isotopic signatures were not, suggesting that the C, N, S turnovers in soil are subject to different controls. The 14C content was generally higher in the 1 AM than 1 NPK and O, with bomb-14C incorporation modelling indicating that mean residence time (MRT) was ca. 170 years in the 1 AM, but closer to 250-290 years in the 1 NPK and O treatments. The measured trends in soil C and 14C during 1923-1996 were successfully modelled using the RothC model. The OM accumulation in the Askov soils was generally dominated by microbial decomposition products rather than by recalcitrant components of the various inputs.     

Alkaloid specioseine from Colchicum speciosum

The fraction of weak bases fromColchicum speciosum Stev. (family Liliaceae) has yielded a new compound — specioseine. The structure of 10-demethylspeciosine has been established for this base by chemical and spectral methods.V. I. Lenin Tashkent State University. Translated from Khimiya Prirodnykh Soedinenii, No. 2, pp. 253–258, March–April, 1991.     

Variation in antioxidant attributes at three ripening stages of guava (Psidium guajava L.) fruit from different geographical regions of Pakistan

The present investigation was carried out to appraise the levels of total phenols and vitamin C as well as antioxidant potential at three different ripening stages (un-ripe, semi-ripe and fully-ripe) of guava (Psidium guajava L.) fruit collected from three different geographical regions of Pakistan (Islamabad, Faisalabad and Bhakkar). The antioxidant potential of guava fruit extracts was assessed by means of different in-vitro antioxidant assays, namely inhibition of peroxidation in linoleic acid system, reducing power and radical scavenging capability. Overall, fruit at the un-ripe stage (G1) exhibited the highest levels of TPC, TFC, reducing power and DPPH radical scavenging activity, followed by the semi-ripe (G2) and fully-ripe (G3) stages. On the other hand, vitamin C content increased as the fruit maturity progressed, with highest value seen at the fully-ripe stage (G3) followed by the semi-ripe (G2) and un-ripe stage (G1). The concentration of vitamin C in fruits varied as: Faisalabad (136.4-247.9 mg 100 g?1), Islamabad (89.7-149.7 mg 100 g?1) and Bhakkar (73.1-129.5 mg 100 g?1). The results showed that different stages of maturation and geographical locations had profound effects on the antioxidant activity and vitamin C contents of guava fruit.     

Structure of alkaloid L-5 fromColchicum luteum

Conclusions FromColchicum luteum Baker collected in the gorge of the Sazan-Ata River in the Chimkent region have been isolated the known alkaloids colchamine, 3-desmethylcolchamine, 3-desmethyl--lumicolchicine, colchicine, 2-desmethylcolchicine, -lumicolchicine, N-desacetyl-N-formylcolchicine, and luteidine, and the new alkaloids L-5 and L-6. The first three bases have been obtained from this plant for the first time.Paper chromatography showed the presence of another three new alkaloids with R _f 0.38, 0.40, and 0.86. On the basis of UV, IR, and NMR spectroscopy and chemical reactions, the structure of 2-desmethylcolchiceine has been proposed for the alkaloid L-5.Khimiya Prirodnykh Soedinenii, Vol. 6, No. 1, pp. 82–88, 1970     

Phytochemical study and cytotoxicity evaluation of Colchicum stevenii Kunth (Colchicaceae): a Jordanian meadow saffron

Isolation, characterization, and biological evaluation of active components of Colchicum stevenii Kunth (Colchicaceae) are described. Colchicum stevenii is an unexplored Jordanian specie with toxic reputation. Directed by brine shrimp lethality test (BST), methanolic extraction, liquid-liquid partition, preparative TLC, and semi-preparative HPLC, it resulted in the isolation of six cytotoxic compounds. The compounds, reported for the first time from this specie, are: (-)-colchicine (1), 2-demethyl-(-)-colchicine (2), (-)-cornigerine (3), beta-lumicolchicine (4), (-)-isoandrocymbine (5) and (-)-O-methylandrocymbine (6). A new, in-house developed, acidic-based reverse-phase gradient semi-preparative HPLC method for the separation of colchisides is presented here. Structural elucidation was based on spectroscopic techniques principally; 1H-NMR and low resolution EIMS. Based on BST results, reported as LC50 values in microg mL(-1) (ppm) with 95% confidence intervals, (-)-colchicine (2.5 ppm) and (-)-cornigerine (2.7 ppm) were the most potent.     

Bioremediation of Marine Sediments Impacted by Petroleum

The aim of this work was to optimize the bioremediation of crude oil-contaminated sand sediment through the biostimulation technique. The soil was obtained in the mid-tide zone of Guanabara Bay, Rio de Janeiro, Brazil and was artificially contaminated with crude oil at 14 g kg^?1. Bioremediation optimization was performed using an experimental design and statistical analysis of the following factors: supplementation with commercial biosurfactant Jeneil® IBR 425 and commercial mineral NPK fertilizer. The response variable used was the biodegradation of the heavy oil fraction, HOF. The analysis of the studied factors and their interactions was executed using contour plots, Pareto diagram and ANOVA table. Experimental design results indicated that the supplementation with fertilizer at 100:25:25 C/N/P ratio and biosurfactant at 2 g kg^?1 yielded biodegradation of HOF at about 30% during 30 days of process. Some experiments were carried out using the experimental design results, yielding 65% of biodegradation of HOF and 100% of n- alkanes between C15 and C30 during 60 process days. Intrinsic biodegradation test was carried out, yielding 85% of biodegradation of n-alkanes between C15 and C30 during 30 days of process.     

超临界二氧化碳萃取秋水仙碱（英文）

 利用超临界二氧化碳对秋水仙块根（经粉碎）中的秋水仙碱进行了萃取,采用高效液相色谱法对萃取出的秋水仙碱的质量分数进行了测定。实验选择40℃20～40MPa作为超临界苹取的操作条件,采用体积分数为95％的乙醇在索氏提取器中对样品进行了对比苹取实验。结果表明:不加浸泡剂进行浸泡处理的样品中的秋水仙碱很难被超临界二氧化碳萃取,在40℃,35MPa条件下,消耗1．28mol的二氧化碳只得到3％的萃取率。加入极少量的有机溶剂浸泡处理样品15min后再进行超临界萃取,可以极大程度地提高秋水仙碱的萃取率。     

Antioxidant capacity and phenolic content of Caesalpinia pyramidalis Tul. and Sapium glandulosum (L.) Morong from Northeastern Brazil

The aims of this study were to quantify the phenolic content and evaluate the antioxidant potential of extracts from the bark and leaves of C. pyramidalis and S. glandulosum. The total phenolic content (TPC) and total tannin content (TTC) were determined using the Folin-Ciocalteu method, and the total flavonoids content (TFC) was measured via complexation with aluminum chloride. The antioxidant activity was evaluated with DPPH (2.2-diphenyl-1-picrylhydrazyl) and FIC (ferrous ion chelating) assays. The TPC ranged between 135.55 ± 9.85 and 459.79 ± 11.65 tannic acid equivalents (TAE) in mg/g material (mg TAE/g). The leaves of both species contained high levels of tannins and flavonoids. The crude ethanol extracts (CEE) from the bark of C. pyramidalis showed high antioxidant activity when compared to ascorbic acid and rutin, whereas the CEE from the leaves was more efficient in chelating ferrous ions. C. pyramidalis had very high phenolic content and anti-radical activity, which indicates a need for further studies aimed at the purification and identification of compounds responsible for the antioxidant activity.     

CPT accumulation in the fruit and during early phases of plant development in Camptotheca acuminata Decaisne (Nyssaceae)

We describe the dynamics of camptothecin (CPT) accumulation during the early phases of plant development in Camptotheca acuminata. TLC and HPLC analyses were performed on the entire mature fruit and all of its parts and on the organs of seedlings in different developmental stages. In the mature fruit, the CPT content was relatively high (2.83 mg g(-1) DW); it was accumulated especially in the endosperm (1.82 mg g(-1) DW) and embryo (1.10 mg g(-1) DW). Regarding seedlings, CPT was present in all of the organs, at all developmental stages. In the cotyledons, content was greatest in the early developmental stages (4.23 mg g(-1) DW) and drastically decreased once the organ reached maturity (0.34 mg g(-1) DW). A similar trend was observed for the true leaves. The results suggest that CPT is translocated from the organs at an advanced developmental stage to those at an early stage.     

Simultaneous quantification of adrenergic amines and flavonoids in C. aurantium, various Citrus species, and dietary supplements by liquid chromatography

An analytical method was developed for the simultaneous quantitative analysis of 6 amines and 20 flavonoids in fruits and extracts of 30 Citrus species, including C. aurantium, near-Citrus relatives, and dietary supplements by liquid chromatography with photodiode array detection. The separation was achieved with a Phenomenex Synergi Hydro reversed-phase column using gradient mobile phase of sodium acetate buffer (pH 5.5) and acetonitrile. Elution was run at a flow rate of 1.0 mL/min and UV at 254, 280, and 330 nm. Among the amines analyzed, synephrine, the main component, was present in the levels from 0.11 to 2.0 mg/g dry weight in 21 Citrus species and 0.07 to 18.62% in dietary supplements claiming to contain C. aurantium. The flavanones and flavones were analyzed in the same Citrus samples and were species-specific. The levels of flavones were very low compared with those of flavanones. The method facilitated the simultaneous quantification of 6 amines and 20 flavonoids in various Citrus species, the distinction between the different Citrus species, and the analysis of dietary supplements containing C. aurantium.     

Determination of arsenic, cadmium, cobalt, chromium, lead, molybdenum, nickel, and selenium in fertilizers by microwave digestion and inductively coupled plasma-optical emission spectrometry detection: collaborative study

There is increasing regulatory interest in the non-nutritive metals content of fertilizer materials, but at present there is no consensus analytical method for acid digestion and instrument detection of those elements in fertilizer matrixes. This lack of method standardization has resulted in unacceptable variability of results between fertilizer laboratories performing metals analysis. A method has been developed using microwave digestion with nitric acid at 200 degrees C, followed by inductively coupled plasma-optical emission spectrometry instrument detection, for the elements arsenic, cadmium, cobalt, chromium, molybdenum, nickel, lead, and selenium. The method has been collaboratively studied, and statistical results are here reported. Fourteen collaborators were sent 62 sample materials in a blind duplicate design. Materials represented a broad cross section of fertilizer types, including phosphate ore, manufactured phosphate products, N-P-K blends, organic fertilizers, and micro-nutrient materials. As much as possible within the limit of the number of samples, materials were selected from different regions of the United States and the world. Limit of detection (LOD) was determined using synthetic fertilizers consisting of reagent grade chemicals with near zero levels of the non-nutritive elements, analyzed blindly. Samples with high iron content caused the most variability between laboratories. Most samples reasonably above LOD gave HorRat values within the range 0.5 to 2.0, indicating acceptable method performance according to AOAC guidelines for analyses in the mg/kg range. The method is recommended for AOAC Official First Action status.     

Chemical Transformation of Humic Acid Molecules under the Influence of Mineral,Fungal and Bacterial Fertilization in the Context of the Agricultural Use of Degraded Soils

The main goal of this work was to study the structural transformation of humic acids (HAs) under the influence of selected strains of fungi (Aspergillus niger and Paecilomyces lilacinus) and bacteria (Bacillus sp., Paenibacillus polymyxa and Bacillus amyloliquefaciens) with/without the presence of NPK fertilizers. Two-year experiments were conducted on two different soils and HAs isolated from these soils were examined for structure, humification degree, and quantity using fluorescence and UV-Vis spectroscopy, elemental analysis, and extraction methods. Results showed that the applied additives contributed to the beneficial transformation of HAs, but effects differed for various soils. HAs from silty soil with higher organic carbon content showed simplification of their structure, and decreases in humification, molecular weight, and aromaticity under the influence of fungi and bacteria without NPK, and with NPK alone. With both fungi and NPK, increases in O/H and O/C atomic ratios indicated an increase in the number of O-containing functional groups. HAs from sandy soil did not show as many significant changes as did those from silty soil. Sandy soil exhibited a strong decline in HA content in the second year that was reduced/neutralized by the presence of fungi, bacteria, and NPK. Periodically observed fluorescence at ~300 nm/450 nm reflected formation of low-molecular HAs originating from the activity of microorganisms.     

Estimation of total as well as bioaccessible levels and average daily dietary intake of iodine from Japanese edible seaweeds by epithermal neutron activation analysis

An epi-thermal instrumental neutron activation analysis (EINAA) method in conjunction with Compton suppression spectrometry (EINAA-CSS) was used for the determination of total iodine in eight different species of edible seaweeds from Japan. This method gave an absolute detection limit of about 2 μg. The accuracy of the method was evaluated using various reference materials and found to be generally in agreement within ±6% of the certified values. The longitudinal distributions of iodine at different growing stages in Japanese sea mustard and tangle seaweeds were investigated. For a 150-cm-high tangle, the highest concentration (5,360 mg/kg) of iodine was found at the root, then decreased slowly to 780 mg/kg in the middle portion (60–75 cm), and increased to 2,300 mg/kg at the apex. On the other hand, for a 190-cm-high sea mustard the highest levels of iodine were found both at the roots (164 mg/kg) and apex (152 mg/kg) with lower values (98 mg/kg) in the middle section. In order to estimate the bioaccessible fraction of iodine, seaweeds were digested by an in vitro enzymolysis method, dietary fibre separated from residue, and both fractions analyzed by EINAA-CSS. The average daily dietary intakes of total (0.14 mg) as well as bioaccessible fraction (0.12 mg) of iodine from the consumption of sea mustards were estimated.     

ICP-AES法对不同施肥、生长年限秦艽宏量和微量元素的测定

采用硝酸、高氯酸进行消解,用ICP-AES对秦艽中的宏量和微量元素含量进行了测定,比较了不同施肥处理与不同生长年限处理对植株内宏量和微量元素的影响.结果表明,不同施肥及生长年限处理秦艽所含宏量和微量元素含量不同,不同施肥处理与CK相比,施NPK混合肥最好,能够增加Fe、Mn、zn、Na、Mg的含量,分别为18.5%、1...     

Correlations of Fat Content in Human Milk with Fat Droplet Size and Phospholipid Species

Fat globule size and phospholipid (PL) content in human milk (HM) were investigated. HM was classified into three groups depending on fat content (A < B < C). PL content (mg/100 g HM) was significantly higher in the C group (p < 0.05), indicating its positive relationship with HM fat content. When the PL content was normalized (mg/g fat), that of group A was significantly higher (p < 0.05) and fat droplet size in group C was slightly larger, suggesting that HM fat content is affected by fat droplet numbers to a larger extent than by fat droplet size. A correlation between PC and SM content in HM was observed regardless of fat content, while correlation between PE and either PC or SM increased in the order of C > B > A, hence the composition and content of PL species in HM varied according to its fat content.     

Single, binary and multi-component adsorption of copper and cadmium from aqueous solutions on Kraft lignin--a biosorbent

A new biosorbent for removing toxic metal ions from water/industrial wastewater has been investigated using by-product lignin from paper production. Lignin was extracted from black liquor waste, characterized and utilized for the removal of copper and cadmium from aqueous solutions in single, binary and multi-component systems. Adsorption studies were conducted at different temperatures, lignin particle sizes, pHs and solid to liquid ratios. All the studies were conducted by a batch method to determine equilibrium and kinetic parameters. The Langmuir and Freundlich isotherm models were applied. The Langmuir model fits best the equilibrium isotherm data. The maximum lignin adsorption capacities at 25 degrees C were 87.05 mg/g (1.37 mmol/g) and 137.14 mg/g (1.22 mmol/g) for Cu(II) and Cd(II), respectively. Adsorption of Cu2+ (68.63 mg/g at 10 degrees C and 94.68 mg/g at 40 degrees C) and Cd2+ (59.58 mg/g at 10 degrees C and 175.36 mg/g at 40 degrees C) increased with an increase in temperature. Copper and cadmium adsorption followed pseudo-second order rate kinetics. From kinetic studies, various rate and thermodynamic parameters such as effective diffusion coefficients, activation energy, and activation entropy were evaluated. Adsorption occurs through a particle diffusion mechanism at temperatures 10 and 25 degrees C while at 40 degrees C it occurs through a film diffusion mechanism. The sorption capacity of black liquor lignin is higher than many other adsorbents/carbons/biosorbents utilized for the removal of Cu(II) and Cd(II) from water/wastewater in single and multi-component systems.