Silica Gel Method Research Articles

DNA extraction protocol from Myrciariacaerulescens J.M.A. Braga, M.T.C. Lacerda & Stadnik (MYRTACEAE)

Myrciaria caerulescens, a fruit-bearing species endemic to Bahia, Brazil, and recently described, has ecological and economic potential. The analysis of genetic diversity and the use of molecular techniques are essential for its conservation and genetic improvement of M. caerulescens.The objective of this work was to standardize the protocol for extracting total DNA from Myrciaria caerulescens in the municipalities of Caetité and Lagoa Real in Bahia. Young leaves were collected using three collection methods and added to aluminum foil stored on ice, aluminum foil with silica and silica in a 50 mL test tube, where they received alphanumeric identification.The material was taken to the Genetic Improvement and Biotechnology Center Laboratory at UFRB, the silica was removed from the samples and stored in an ultra freezer at -80°C. For genomic DNA extraction, the three collection and extraction methods of the 40 samples, three protocols were tested for each method. The protocols of Lodhi (1994), modified by Pereira (2005), Doyle and Doyle (1987) and Murray and Tompsom (1980).Liquid nitrogen was used for crushing, helping to break down the M.caerulescens material. The isolated DNA influenced the quality and quantity of the methods and protocols tested. Silica gel method in the test tube had a greater amount of DNA compared to the others.The best result in DNA bands was described in Lodhi (1994), modified by Pereira (2005), better quality and higher concentration of extracted DNA, the test tube with silica, greater presence of bands, following the aluminum foil with silica for both locations. CTAB protocols were efficient in extraction. The increase in the amount of NaCl (0.5 to 5M) made it possible to quantify DNA bands in the agarose gel with positive ions neutralizing the negative charge of the DNA phosphate group.

Chemical constituents from Alangium chinense subsp. pauciflorum

Chemical constituents of 70% ethanol extract of Alangium chinense subsp. pauciflorum were investigated. The 70% ethanol extract of A. chinense subsp. pauciflorum was isolated and purified by D-101 macroporous resins, silica gel, Sephadex LH-20 and other methods. As a result, nineteen compounds were isolated and identified as 4-cyclohexene-1α,2α,3α-triol-1-O-β-D-glucoside(1), 1β,4α,6α,13-tetrahydroxy-eudesm-11(12)-ene(2), sucrose(3), 1'-O-benzyl-α-L-rhamnopyranosyl-(1″→6')-β-D-glucopyranoside(4), bis(2-ethylhexyl)benzene-1,2-dicarboxylate(5),(Z)-10-heneicosenoic acid(6), di-O-methylcrenati(7), methyl-α-D-fructofuranoside(8), β-daucosterol(9), syringic acid(10), vanillicacid(11), octacosanol(12), isoarborinol(13), 2,7-dihydroxy-6-methyl-4-(1-methylethyl)-1-naphthalenecarboxylate(14),vanillin(15), coniferyl aldehyde(16), 9(11)-dehydroergosterolperoxide(17), 5α,8α-epidioxy-(22E,24R)-ergosta-6,22-dien-3β-ol(18), β-sitosterol(19), respectively. Compounds 1 and 2 were new compounds, compounds 5-11, 13, 15-18 were isolated from Alangium for the first time.The anti-inflammatory activity of compourd 1 was determinded by the LPS-induced RAW264.7 macrophage inflammation model. The results showed that the new compound 1 has a certain inhibitory effect on LPS-induced NO production of RAW264.7 cells, and the inhibitory rate was 54.57%.

Synthesis and characterization of strontium tartrate tetrahydrate crystal using silica gel method

In the present study, strontium tartrate tetrahydrate crystals were grown using the silica gel method. Optimum growth parameters were obtained by varying molar concentration, volume of upper reactant solution, and pH of gel mixture at ambient temperature (31 °C). Large size crystal (9 × 8 × 4 mm3) of strontium tartrate tetrahydrate were obtained when the pH of the gel mixture was 4.2 and upper reactant had a molar concentration of 1.5 M and volume of 20 ml. As grown crystal was characterized using different techniques viz. Powder X-ray Diffraction (PXRD), Fourier Transform Infrared spectroscopy (FTIR), Energy Dispersive Analysis of X-ray (EDAX), and UV–vis spectral analysis. Analysis of Powder X-ray diffraction data carried out in the 2θ range 10°–60° revealed that as grown crystal had an orthorhombic structure with space group P2 2 2 and unit cell parameters a = 9.8865 Å, b = 10.0448 Å, c = 9.5186 Å, α = β = γ = 90°. Various vibrational peaks of hydroxyl group (OH) at wavenumber 3170.42, 3384.44, 3536.72 cm−1, carbonyl (CO) group at 1601.88 cm−1 were observed in FTIR spectroscopy. One peculiar peak at 478.2 cm−1 where one O− and was replaced by Sr2+ was also obtained in FTIR spectroscopy suggesting formation of strontium tartrate crystal. Energy dispersive analysis of X-ray confirms the presence of expected major elements like strontium, carbon, and oxygen in the crystal. UV–vis transmission spectrum of strontium tartrate tetrahydrate crystals was recorded in the wavelength range of 190 to 1100 nm. The energy bandgap estimated from transmission data is 5.64 eV. Non-linear Optical (NLO) competence of STT crystal is observed at 532 nm. The electrical property of pelletized samples was studied by dielectric measurement in the frequency range of 20 Hz–2 MHz at room temperature. It is observed that dielectric loss is very low at higher frequency.

Phytochemical Study of Euphorbia turcomanica Boiss.

The attraction to the Euphorbia genus, with its remarkable diversity in species, is due to its variety of chemical compositions. Euphorbia turcomanica is one of the species of the spurge family growing wildly in Iran. This research aims to investigate the presence of secondary metabolites, specially terpenoid compounds, in terms of structural determination. Samples of E. tucomanica were finely powdered and macerated with acetone/dichloromethane 2:1. Repeated column chromatography using silica gel, MPLC, and HPLC methods followed by the analysis of data obtained from spectroscopic means was carried out to purify and identify the terpenoid constituents. The chemical structures of nine known terpenoids were determined for the first time from E. turcomanica during this study. Loliolide (1), a monoterpene, and eight steroids and triterpenes, including simiarenol (2), isomultiflorenol (3), cycloart-25-ene-3β,24-diol (4), β-sitosterol (5), cycloart-23-ene-3β,25-diol (6), 3α, 11α-dihydroxyurs-12-ene (7), 3β, 24β, 25-trihydroxycycloartane (8), and 7α-hydroxystigmasterol (9) were isolated and identified. E. tucomanica, with a rich terpenoid profile, can be one of the valuable and economic sources providing compounds for drug development.

A new isoflavone from Dalbergia odorifera and inhibitory activity of its tyrosinase

Twelve flavonoids were isolated and purified from the ethyl acetate fraction of 95% ethanol extract of Dalbergia odorifera by heat reflux extraction, solvent extraction, recrystallization, normal phase silica gel, Sephadex LH-20, MCI gel and HPLC methods. The structures were identified with multiple spectroscopic methods, including 1 D-NMR, 2 D-NMR and MS. The compounds were identified as 6,7,8-trimethoxy-5,4'-dihydroxy isoflavone(1), medicarpin(2), 7,2'-dihydroxy-4'-methoxy-isoflavanol(3), biochanin A(4), prunetin(5), genistein(6), pratensein(7), 3-(4-hydroxyphenyl)-6-isopentenyl-7-methoxy-4H-chromen-4-one(8), tectorigenin(9), irisolidone(10), vestitol(11), and formononetin(12). Compound 1 was a new isoflavone, and compound 8 was isolated from D. odorifera for the first time. The results showed that compounds 1-3 had inhibitory effects on tyrosinase, with inhibition rates of 35.58%, 38.63% and 51.34% at the concentration of 1.0 mmol·L~(-1), respectively.

The Effect of Mo Addition on Iron Oxide Magnetic Particles Synthesis by Silica Gel Method

The Effect of Mo Addition on Iron Oxide Magnetic Particles Synthesis by Silica Gel Method

Effects of ultra-dry storage on seed germination and seedling growth of <i>Handeliondendron bodinieri</i>

(H. Lév.) Rehder is a rare, endangered, and therefore, protected tree species native to China. However, there are serious limitations to the effective protection of the species, including a low seed germination-rate and difficult storage due to a high seed oil-content. Here, we evaluated the feasibility of ultra-dry seed storage and its effects on seedling growth. We used the silica gel method to prepare ultra-dry seeds with different moisture contents to find an optimal moisture content range (2.54%–4.77%). Ultra-dry treatment improved storability of . Furthermore, seeds with a moisture content of 4.77% stored at room temperature, and seeds with a moisture content of 3.97% stored at 4 °C yielded the best results. Priming with an appropriate concentration of polyethylene glycol had a certain repairing effect on ultra-dry stored seeds and improved seed vigor, with a two-day priming treatment with 20% polyethylene glycol having the best effect. Finally, compared with sand storage at 4 °C, ultra-dry storage promoted seedling growth and root development; furthermore, it alleviated storage damage to seeds, promoted soluble sugar and soluble protein accumulation, and increased seedling nitrogen, phosphorus, and potassium uptake. Therefore, ultra-dry storage can be effectively used to preserve seeds. Specifically, low-temperature storage of ultra-dry seeds with a moisture content of 3.97% enhanced seed vigor, and seedling growth and development.Handeliodendron bodinieriH. bodinieri seedsH. bodinieriH. bodinieriH. bodinieri

Operational Laboratory Methods for GDGTs Groups Separation

Glycerol dialkyl glycerol tetraethers (GDGTs), specific membrane lipids synthesized mainly by bacteria and archaea, can be divided into isoprenoids and methyl branched alkyl GDGTs (iGDGTs and brGDGTs, respectively). Three GDGTs groups (iGDGTs, brGDGTs, and other membrane lipids) in a peat sample were separated and collected in this study using semi-preparative high-performance liquid chromatography (HPLC) and silica gel column chromatography. The obtained recoveries for the whole analytical procedure were 85%−55% using semi-preparative HPLC and 70%−20% using gel column chromatography. In addition, in each method, the recoveries of brGDGTs and iGDGTs were similar, regardless of the huge difference in their contents. High purity was found in the fractionated groups, determined based on ether cleavage and reduction. Moreover, the semi-preparative HPLC method could realize a better separation efficiency than the silica gel method, but it was time-consuming and required expensive equipment, while the silica gel chromatography method featured merits of time saving and convenient operation at the cost of a slight reduction in separation efficiency. The advantages of the silica gel method make it an operational laboratory method for batch experiments and isotopic studies.

Identification of p53 gene alterations in canine mammary tumours using polymerase chain reaction and direct sequence analysis

Mammary tumours are mentioned as the most common tumours in female dogs and approximately half of them are detected malignant. p53 gene mutations are demonstrated to be the most common genetic alteration in canine mammary tumours. The present study was conducted to evaluate exon-1 of p53 gene mutations in tissue samples of canine mammary tumours by PCR and direct sequence analysis. After histopathological confirmation of the tissue sections by haematoxylin and eosin staining (10/26), deparaffinised samples were used for DNA extraction by silica gel method. Subsequently, p53 exon 1 was amplified through PCR assay using specific oligo nucleotide primers designed according to the canine DNA sequence available online. Microscopically, 10 out of 26 suspected tissue samples were recognised as malignant mammary gland tumours with various grades of malignancy. Surprisingly, one insertion of mutation was found in exon 1 of all examined samples corresponding to a sequence comprising 27 amino acids, between amino acids 30 to 57 in the p53 protein. Taken together, it seems that alteration of exon 1 p53 gene may lead to malignancy beha­viour, poor prognosis and short survival time in dogs with mammary carcinomas.

Three new acenaphthene derivatives from rhizomes of Musa basjoo and their cytotoxic activity

Three new acenaphthene derivatives cis-3-(4'-methoxyphenyl)-acenaphthene-1, 2-diol (1), trans-(1S, 2S)-3-phenyl-acenaphthene-1, 2-diol (2) and 8-(4-hydroxyphenyl)-2H-acenaphthylen-1-one (3) in company with six known compounds were isolated from the 70% ethanol extract of the rhizomes of Musa basjoo. Those chemical constituents were separated and purified by macroreticular resin, silica gel, Toyopearl HW-40F, SephadexLH-20 and other chromatographic methods, respectively. The chemical structures of new compounds were elucidated by HR-ESI-MS, 1H NMR, 13C NMR, HMQC, HMBC spectrum and specific optical rotations. Compound 4 was isolated for the first time from the genus Musa and compound 7 was firstly assigned the carbon spectrum. Furthermore, the cytotoxic activity of compounds 1–9 against WM9, MDA-MB231, HeLa, K562, DU145 and PC3 was screened with cisplatin as a positive control. Compound 9 showed promising cytotoxic activities with IC50 values of 2.65 ± 0.38 µM against the HeLa cell lines, while compound 8 possessed significant cytotoxicity with IC50 values of 6.51 ± 0.44, 18.54 ± 0.68 and 7.98 ± 1.44 µM against the HeLa, MDA-MB231 and WM9 cell lines, respectively.

Photoluminescence properties of fully concentrated Terbium oxalate: A novel efficient green emitting phosphor

A novel green emitting phosphor, Terbium oxalate decahydrate, was synthesized in crystalline form employing the hydro silica gel method. The structure of the sample was confirmed by x-ray diffraction analysis. Photoluminescence excitation spectrum of the sample shows several peaks in the deep UV to Visible region, matching well with the commercially available LED sources. Emission spectrum, recorded with representative excitation wavelengths revealed efficient luminescence, particularly the green emission at 543nm. The decay time of the sample was measured to be 0.81ms. It exhibits a colour purity of 68% with chromaticity coordinates (0.31, 0.57) which is very close to that of the European Broadcasting Union illuminant green.

A Novel Three‐Dimensional Copper(II) 1,2‐Ethylenediphosphonate Framework with Channel‐like Voids

AbstractTurquoise monoclinic single crystals of the novel three‐dimensional Cu2[μ8‐O3P(CH2)2PO3]·3.2H2O coordination polymer were prepared using the silica gel method. Space group C2/m (no. 12) with a = 1483.6(2), b = 668.44(8), c = 436.30(6) pm, β = 93.28(2)°. The Cu2+ cation is coordinated by four oxygen atoms stemming from the 1,2‐ethylenediphosphonate dianions in a square planar manner and two water molecules in the axial positions. The connection between the Cu2+ cations and the [CPO3] units from the 1,2‐ethylenediphosphonate dianions leads to layers parallel to (100), which are linked by the ethylene groups to a three‐dimensional framework with channel‐like voids. The channel‐like voids accommodate water molecules not bound to Cu2+ and extend parallel to [001] with an opening of about 550 pm × 260 pm. Magnetic measurements reveal an antiferromagnetic behavior due to a superexchange coupling between Cu2+ ions through an oxygen bridge. The UV/Vis spectrum reveals three d–d transition bands at 694, 774, and 918 nm. The compound can be fully dehydrated by thermal treatment and rehydrated by storage in ambient air.

A Novel Three-Dimensional Copper(II) 1,2-Ethylenediphosphonate Framework with Channel-like Voids

Turquoise monoclinic single crystals of the novel three-dimensional Cu2[µ8-O3P(CH2)2PO3)]•3.2H2O coordination polymer have been prepared using the silica gel method. Space group C2/m (no. 12) with a = 1483.6(2), b = 668.44(8), c = 436.30(6) pm, β = 93.28(2)°. The Cu2+ cation is coordinated by four oxygen atoms stemming from the 1,2- ethylenediphosphonate dianions in a square planar manner and two water molecules in the axial positions. The connection between the Cu2+ cations and the [PO3C] units from the 1,2- ethylenediphosphonate dianions leads to layers parallel to (100), which are linked by the ethylene groups to a three-dimensional framework with channel-like voids. The voids accommodate water molecules not bound to Cu2+ and extend parallel along [001] with an opening of about 550 x 260 pm. Magnetic measurements reveal an antiferromagnetic behaviour due to a superexchange coupling between Cu2+ ions through an oxygen bridge. The UV-Vis spectrum reveals three d−d transition bands at 694, 774, and 918 nm. The compound can be fully dehydrated by thermal treatment and rehydrated by storage in ambient air.

M2(H2O)[μ10‐C6H2(COO)4] (M = Ba2+, Pb2+) – Two Isotypic Three‐Dimensional Coordination Polymers with a Layer‐like Separation between Anions and Cations

AbstractMonoclinic single crystals of Ba2(H2O)[μ10‐C6H2(COO)4] (1) and Pb2(H2O)[μ10‐C6H2(COO)4] (2) were obtained using the silica gel method [space group C2/c (no. 15), Z = 4; 1: a = 780.89(4), b = 1756.19(8), c = 914.80(5) pm, β = 114.512(5)°; 2: a = 756.70(10), b = 1772.8(2), c = 890.2(2) pm, β = 113.590(10)°]. There are two crystallographically independent M2+ ions (M = Ba, Pb). M(1) is surrounded by eight carboxylate oxygen atoms and one water molecule forming a tricapped trigonal prism. M(2) is coordinated by ten carboxylate oxygen atoms in the shape of a tetracapped octahedron. The connection between the M(1) and M(2) polyhedra leads to infinite layers parallel to (010), which are linked by [C6H2(COO)4]4– anions to form a three‐dimensional framework. The [C6H2(COO)4]4– anion adopts a μ10 coordination mode. Compound 1 reveals short Ba–Ba contacts of 426.46(2) pm, whereas the Pb–Pb distance of 411.01(6) pm in 2 is larger than twice the van der Waals radius.

A new aurone glycoside with antifungal activity from marine- derived fungus Penicillium sp. FJ-1

Endophytic fungi which reside in the tissue of mangrove plants seem to play an important role in the discovery of new biologically active substances. During the course of screening for the antimicrobial metabolites from the endophytic fugus Penicillium sp. FJ-1 of mangrove plant Avicennia marina, a new aurone glycoside (1) was isolated by repeated column chromatography on silica gel and recrystallization methods. The structure of 1 was elucidated as (Z)-7,4'-dimethoxy-6-hydroxy-aurone-4-O-β-glucopyranoside, on the basis of spectroscopic analysis. Compound 1 exhibited antifungal activity against Candida sp., with the potency comparable to amphotericin B and much better than fluconazole. Compound 1 can also inhibit extracellular phospholipase secretion in a concentration-dependent manner.

First Report of Artichoke yellow ringspot virus in Globe Artichoke in Turkey.

Turkey is one of the main globe artichoke (Cynara cardunculus L. subsp. scolymus (L.) Hayek) producers in the world. Cultivation of this crop is done mainly in the Aegean and Eastern Marmara regions with asexually propagated cultivars such as Bayrampasa and Sakiz. More than half of total globe artichoke production in Turkey is obtained from the provinces of Izmir, Aydin, and Mugla in the Aegean region. Surveys in 2011 and 2012 were carried out to look for the presence of Artichoke yellow ringspot virus (AYRSV), Tobacco mosaic virus (TMV), and Tomato spotted wilt virus (TSWV) in the globe artichoke production areas in these three provinces. Double antibody sandwich (DAS)-ELISA and reverse transcriptase (RT)-PCR assays conducted for TMV and TSWV showed that the samples were not infected with these two viruses. Due to the lack of commercial ELISA kits against AYRSV, RT-PCR and biological indexing were used for its identification. Leaf tissues from 35 symptomatic and 25 symptomless plants were sampled and analyzed by RT-PCR using as template total RNAs extracted by a silica gel method (1). RT-PCR was conducted as previously reported (1). A PCR product of the expected size (about 530 bp) was obtained from five plant samples that were collected from Izmir province and had symptoms of bright yellow spots and line patterns on the leaves. The incidence of diseased plants in the fields ranged from 1 to 5%. In previously conducted studies, these symptoms were defined as typical symptoms of AYRSV on artichokes (2,3,4). One of the PCR products was cloned and sequenced. BLASTn analysis of the obtained sequence (GenBank Accession No. KC622054) showed 92% nucleotide identity with the partial RNA1 sequence of an AYRSV isolate from Allium cepa (AM087671.2). Furthermore, selected test plants were mechanically inoculated with sap from plant samples that were positive in RT-PCR. Chlorotic local lesions and systemic mottling symptoms were observed on Chenopodium quinoa; chlorotic lesions, mosaic, and deformation on Cucumis sativus; and systemic mosaic, reddish necrotic local lesions, and malformation on Phaseolus vulgaris (French bean). Results of the biological tests were confirmed by RT-PCR. AYRSV has a wide host range including artichoke and six other cultivated plant species and can be easily transmitted by seed, plant sap, and vegetative propagation (3). To our knowledge, this is the first report of natural infection of globe artichoke by AYRSV in Turkey. AYRSV infections can have a detrimental effect on the growth and yield of artichoke plantings. This assay will be useful for further epidemiological studies.

Purification of biodiesel using activated carbons produced from spent tea waste

Waste cooking oil was converted into biodiesel through base catalyzed transesterification. After separating the glycerol, the crude methyl esters were purified using activated carbons produced from spent tea waste. Yield and fuel properties of the produced biodiesels were compared with those purified by using silica gel and conventional method namely water washing method. The study revealed that using activated carbons for the purification of biodiesel resulted in higher yield and better fuel properties compared to those purified using silica gel and water washing method. Furthermore, the spent activated carbon was regenerated and reused for the same purpose. However, the results showed that the yield and fuel properties of those purified using the regenerated activated carbon were also better than those purified using silica gel and water washing method.

Spectroscopic properties of Pr3 + -doped erbium oxalate crystals

Spectroscopic properties of praseodymium ions-doped erbium oxalate (Er2(C2O4)3 · nH2O) crystals have been investigated. The crystals were grown by hydro silica gel method under suitable pH conditions and by single diffusion method. The well-grown crystals are bright and transparent. The dark green colour of these crystals changes with the variation of the concentrations of the dopant ions. The absorption spectra have been measured in the region 200–800 nm at room temperature. Judd–Ofelt intensity parameters for f–f transitions of the Pr3+ ions have been determined as Ω2 = 166.7, Ω4 = 1.103 and Ω6 = 2.898. Analyses of the absorption spectra also show a possible energy transfer from the host material to the dopant.

Raman Study of Synthetic Witherite–Strontianite Solid Solutions

ABSTRACT Characterization of zoned crystals of a synthetic witherite–strontianite solid solution (BaxSr1-xCO3) was carried out using electron microprobe analysis and Raman spectroscopy. The sample was obtained by coprecipitation using the silica gel method. As each carbonate crystal from this preparation showed the whole range of intermediate compositions BaxSr1-xCO3, 0.1 ≤ x ≤ 0.9, the solid solution could be studied for single crystals. Peak-shape analysis of the Raman bands showed that the peak shifts depend on the replacement of the Ba and Sr cations introducing different radii and masses. We observed a shift to higher wave numbers for an increase of the SrCO3 content.

Energy transfer and thermal studies of Pr3+ doped cerium oxalate crystals

Energy transfer process at room temperature for cerium (sensitizer) oxalate single crystals doped with different concentrations (10, 13, 15, 17 and 20%) of praseodymium ions (activator) grown by hydro silica gel method has been evaluated. The analysis of energy level diagrams of cerium and praseodymium ions indicates that the energy gap between the sensitizer and the activator ions varies in a small range suggesting a possible energy transfer from the Ce3+ to Pr3+. The emission and absorption spectra of these crystals were recorded. The overlapping of the absorption spectra of Pr3+ and emission spectra of Ce3+ at wavelengths 484 and 478 nm, respectively, strongly supports the possible energy transfer process in this system. From the absorption spectra, oscillator strength, electric dipole moment, branching ratio and Judd-Ofelt parameters of this system were evaluated by least square programming. The quantum efficiency, energy transfer probabilities and thermal properties have been studied.