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1.
Ionic liquid-modified silica, with functional groups based on imidazole as the cation, was obtained. A molecular imprinting technique was introduced to form the order of functional groups. The selectivity of the obtained ionic liquid-modified silica was successfully used as a special imprinted sorbent in the solid-phase extraction to isolate cryptotanshinone, tanshinone I and tanshinone IIA from Salvia miltiorrhiza Bunge. Several washing and elution solvents with different polarities were evaluated. The ionic liquid-modified silica as the sorbent exhibited a higher selectivity than blank ionic liquid-modified silica, traditional silica and C18 cartridges. A quantitative analysis was conducted by liquid chromatography with a C18 column and methanol/water (75:25, v/v, containing 0.5% acetic acid) as the mobile phase. A good linearity was obtained from 0.5 × 10?4 to 0.1 mg mL?1 (r 2  > 0.99) with relative standard deviations that were less than 4.6%.  相似文献   

2.
Titania (TiO2) and titania–silica (TiSi) aerogels are suitable for photocatalytic oxidation of volatile organic compounds for pollution mitigation; however, methods for fabricating these aerogels can be complex. In this work we describe the use of a rapid supercritical extraction (RSCE) technique to prepare TiO2 and TiSi aerogels in as little as 8 h. The RSCE technique uses a metal mold and a four-step hydraulic hot press procedure to bring the solvents in the sol–gel pores to a supercritical state and control the supercritical fluid release process. Resulting TiO2 aerogels were powdery with BET surface areas of 130–180 m2/g, pore volumes ~0.5 cm3/g and skeletal densities of 3.6 g/mL. Monolithic TiSi aerogels were made using two different methods. An impregnation process, in which titania precursor was added to a silica sol–gel, took 4–8 days to complete with a 7-h RSCE and resulted in translucent aerogels with high surface area (560–650 m2/g) and pore volume (2.0–2.6 cm3/g), bulk densities ranging from 0.1 to 0.4 g/mL and skeletal densities of 2.3 g/mL. A co-precursor method for preparing TiSi aerogels took 8 h to complete. The precursor chemical mixture was poured directly into the mold and processed in a 7-h RSCE process. The resulting aerogels were opaque, with high surface areas (510–580 m2/g), low bulk density (0.03 g/mL), skeletal densities of 2 g/mL and pore volumes of 2.6–3.5 cm3/g. Preliminary solar simulator studies show that TiO2 and TiSi aerogels are capable of photocatalytic degradation of methylene blue in aqueous solution.  相似文献   

3.
Accurate, sensitive, and precise high performance thin layer chromatographic (HPTLC) methods were developed and validated for the determination of sumatriptan and zolmitriptan in presence of their degradation products. Sumatriptan was separated from its degradation products and analyzed on TLC silica gel 60 F254 plates using chloroform–ethyl acetate–methanol–ammonia (4:3:3:0.1, v/v) as a developing system followed by densitometric measurement of the bands at 228 nm. Zolmitriptan was determined using chloroform–ethyl acetate–methanol–ammonia (3:3:3:1, v/v) as a developing system followed by densitometric measurement at 222 nm. The methods were validated over a range of 0.5–4 μg/spot for sumatriptan and 0.5–3 μg/spot for zolmitriptan. The proposed methods were successfully applied for the determination of the studied drugs in bulk powder and in their pharmaceutical formulations.  相似文献   

4.

A method of extraction based on matrix solid-phase dispersion has been developed, optimized, and validated by chromatographic analysis of cypermethrin pesticide residues in samples of cows’ milk. Milk (0.25 g) was fortified with cypermethrin and blended with 1 g each of C18 (octadecylsilane) silica and Na2SO4 (anhydrous sodium sulfate), used to trap fats and water, respectively. The homogenized material was transferred to a commercial SPE cartridge containing 1 g activated Florisil with 5 mL acetonitrile. Cypermethrin was eluted under vacuum with 5 × 2 mL acetonitrile and the extract was concentrated to 1 mL and analyzed by gas chromatography–mass spectrometry. The limits of detection and quantification of the method were 0.025 and 0.08 mg kg−1, respectively.

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5.
In a previous work, a continuous simultaneous saccharification and fermentation process to produce ethanol from cassava starch was studied, using a set of fixed-bed reactors. The biocatalyst consisted of glucoamylase immobilized in silica particles and co-immobilized with S. cerevisiae in pectin gel. Using 3.8 U mL?1 reactor and 0.05 gwet yeast mL?1 reactor at start-up, starch hydrolysis was the rate-limiting step. Maximum ethanol productivity was 5.8 gethanol L?1 h?1, with 94.0% conversion of total reducing sugars (TRS) and 83.0% of the ethanol theoretical yield. In this work, the molar mass of the substrate and the biocatalyst particle size were reduced in an attempt to improve the bioreactor performance. The diameters of silica and pectin gel particles were reduced from 100 μm and 3–4 mm, respectively, to 60 μm and 1–1.5 mm, and the degree of substrate prehydrolysis by α-amylase was increased. The bioreactor performance was assessed for different loads of immobilized glucoamylase (2.1, 2.8, and 3.8 U mL?1 reactor), for the same initial cell concentration (0.05 gwet yeast.mL?1 reactor). Feeding with 154.0 g L?1 of TRS and using 3.8 U mL?1 reactor, fermentation became the rate-limiting step. Productivity reached 11.7 g L?1 h?1, with 97.0% of TRS conversion and 92.0% of the ethanol theoretical yield. The reactor was operated during 275 h without any indication of destabilization.  相似文献   

6.
Two-stage microwave (microwave/NaOH pretreatment followed by microwave/H2SO4 pretreatment) was used to release monomeric sugars from Kans grass (Saccharum spontaneum) and Giant reed (Arundo donax). The optimum pretreatment conditions were investigated, and the maximum monomeric sugar yields were compared. The microwave-assisted NaOH and H2SO4 pretreatments with a 15:1 liquid-to-solid ratio were studied by varying the chemical concentration, reaction temperature, and reaction time to optimize the amount of monomeric sugars. The maximum amounts of monomeric sugars released from microwave-assisted NaOH pretreatment were 6.8 g/100 g of biomass [at 80 °C/5 min, 5 % (w/v) NaOH for S. spontaneum and at 120 °C/5 min, 5 % (w/v) NaOH for A. donax]. Furthermore, the maximum amounts of monomeric sugars released from microwave-assisted H2SO4 pretreatment of S. spontaneum and A. donax were 33.8 [at 200 °C/10 min, 0.5 % (w/v) H2SO4] and 31.9 [at 180 °C/30 min, 0.5 % (w/v) H2SO4] g/100 g of biomass, respectively. The structural changes of S. spontaneum and A. donax were characterized using Fourier transform infrared spectroscopy and scanning electron microscopy.  相似文献   

7.
Amino propyl silica (APS) gel reacts immediately with benzyl monopyridyl hydrazone (BMPH) to produce a new effective and selective derivative (BMPH-APS) for the separation and preconcentration of traces of Pd(II) in aqueous solution. Factors affecting the sorption and desorption of Pd ions have been investigated. Acidic aqueous solution of 0.5% thiourea in 0.5 mol L?1 HCl has been used as eluent for the desorption of Pd(II). The stripped metal ion was determined by flame AAS. The modified silica quantitatively sorbed Pd(II) at pH 2–4 with a sorption capacity of 0.65 mmol g?1 and preconcentration factor of 250 fold in less than one minute (t1/2). Common other ions did not interfere except Co(II) which was eliminated by EDTA . The limit of detection (LOD) is 0.1 ng mL?1 and the relative standard deviation (R. S. D.) for 10 replicate measurements at 20 ng mL?1 Pd level was 1.51%. The method was successfully applied for Pd preconcentration in highly concentrated salt solutions and in spiked clay, road dust, scrap and water samples.  相似文献   

8.
In this work, the films of poly(ether-block-amide) (Pebax 1657) and hydrophilic/hydrophobic silica nanoparticles (0–10 wt%) were coated on a poly(vinyl chloride) (PVC) ultrafiltration membrane to form new mixed matrix composite membranes (MMCMs) for CO2/N2 separation. The membranes were characterized by SEM, FTIR, DSC and XRD. Successful formation of a non-porous defect-free dense top layer with ~4 μm of thickness and also uniform dispersion of silica nanoparticles up to 8 wt% loading in Pebax matrix were confirmed by SEM images. The gas permeation results showed an increase in the permeance of all gases and an increase in ideal CO2/N2 selectivity with the increase in silica nanoparticle contents. Comparison between the incorporation of hydrophilic and hydrophobic silica nanoparticle into Pebax matrix revealed that the great enhancement of CO2 solubility is the key factor for the performance improvement of Pebax + silica nanoparticle membranes. The best separation performance of the hydrophilic silica nanoparticle-incorporated Pebax/PVC membrane for pure gases (at 1 bar and 25 °C) was obtained with a CO2 permeability of 124 barrer and an ideal CO2/N2 selectivity of 76, i.e., 63 and 35% higher than those of neat Pebax membrane, respectively. The corresponding values for hydrophobic silica nanoparticle-incorporated Pebax/PVC membrane were 107 barrer for CO2 permeability and 61 for ideal CO2/N2 selectivity. Also the performances of MMCMs improved upon pressure increase (1–10 bar) owing to the shift in plasticizing effect of CO2 towards the higher pressures. In addition, an increase in permeabilities with a decrease in ideal selectivity was observed upon temperature increase (25–50 °C) due to the intensification of chain mobility.  相似文献   

9.
《Analytical letters》2012,45(4):570-581
Two simple, sensitive, and specific high-performance liquid chromatography and thin-layer chromatography methods were developed for the simultaneous estimation of Amlodipine besilate (AM) and Valsartan (VL). Separation by HPLC was achieved using a xTerra C18 column and methanol /acetonitrile /water/ 0.05% triethylamine in a ratio 40:20:30:10 by volume as mobile phase, pH was adjusted to 3 ± 0.1 with o-phosphoric acid. The flow rate was 1.2 mL min?1. The linearity range was 0.2 to 2 µg mL?1 for amlodipine besilate and 0.4 to 4 µg mL?1 for Valsartan with a mean percentage recovery of 99.59 ± 0.523% and 100.61 ± 0.400% for amlodipine besilate and valsartan, respectively. The TLC method used silica gel 60 F254 plates; the optimized mobile phase was ethyl acetate/ methanol / ammonium hydroxide (55:45:5 by volume). Quantitatively, the spots were scanned densitometrically at 237 nm. The range was 0.5–4.0 µg spot?1 for amlodipine besilate and 2.0–12.0 µg spot?1 for valsartan. The mean percentages recovery was 99.80 ± 0.451% and 100.61 ± 0.363% for amlodipine besilate and valsartan, respectively. The HPLC method was found to be simple, selective, precise, and reproducible for the estimation of both drugs from spiked human plasma.  相似文献   

10.
An analytical method for the determination of both sulfadiazine (SDZ) and trimethoprim (TMP), and also N4-acetyl-sulfadiazine (AcSDZ), the main metabolite of SDZ, in fish muscle plus skin has been developed and validated. Dapsone was used as internal standard. The method involves extraction of the analytes from fish tissue by pressurized liquid extraction using water as extractant. Sample cleanup was carried out by solid phase extraction using Abselut Nexus cartridges. Target analytes were quantitatively determined by liquid–chromatography mass spectrometry using single ion monitoring. The developed method was validated according to the European Union requirements (decision 2002/657/EC). The limit of detection for SDZ and AcSDZ was 3.0 and 2.5 µg kg?1 for TMP. The limit of quantification (LOQ) was 10 µg kg?1 for SDZ and AcSDZ and 7.5 µg kg?1 for TMP. The recovery experiments carried out included the concentration levels of 0.5, 1 and 1.5 times the MRLs for SDZ and TMP. Concentration levels for AcSDZ were the same as SDZ. The values obtained were higher than 92.0% with coefficient of variation (CV, %) below 8.6%. The precision of the method, calculated as CV (%), ranged from 0.2 to 6.8% and from 0.8 to 8.9% for intra–day and inter–day analysis, respectively. Decision limit (CCα) was calculated as 104.3, 53.7 and 105.3 µg kg?1 for SDZ, TMP and AcSDZ, respectively. Detection capability (CCβ) was calculated as 110.0, 58.8 and 109.7 µg kg?1 for SDZ, TMP and AcSDZ, respectively. “Matrix effect” and “relative matrix effect” were also evaluated. The method was used for the analysis of fish samples purchased from local markets.  相似文献   

11.
《Analytical letters》2012,45(11):1921-1930
This paper describes a simple and sensitive method for the determination of manganese in human urine by graphite furnace atomic absorption spectroscopy (GFAAS), which includes sample preparation by microwave digestion. Matrix modifier combinations, the digestion power, pyrolysis, and atomization temperatures were optimized. A mixture of 5.0 µg Pd(NO3)2 and 3.2 µg Mg(NO3)2 modifier presented the best performance. The optimal temperatures for pyrolysis and atomization were 1500°C and 1950°C, respectively. The GFAAS method was compared to inductively coupled plasma–mass spectrometry (ICP–MS) for the determination of manganese in urine. Analytical figures of merit for GFAAS and ICP–MS were: accuracy (3.46%, 2.19%), precision (3.61%, 5.84%), LOD (0.109 µg · L?1, 0.015 µg · L?1), LOQ (0.327 µg · L?1, 0.045 µg · L?1), and recovery (80–100%, 74–89%). Both methods were employed for the determination of Mn in urine and the results were compared statistically.  相似文献   

12.
《Analytical letters》2012,45(16):2359-2366
Phenolic compounds are one of the major compounds in Laminaria japonica Aresch. Solid-phase extraction was used to separate the two phenolic compounds (4-hydroxybenzoic acid and 4-hydroxybenzaldehyde). A new monolithic sorbent was developed and used successfully as a special sorbent in a solid-phase extraction process. The effects on different SPE cartridges using silica, C18, and monolithic were compared. Quantitative analysis was carried out using a C18 analysis column (5 µm, 150 × 4.6 mm). Good linearity was obtained for the two targets, ranging from 0.5 to 100 µg mL?1 (r 2  > 0.999), with relative standard deviations <4.7%.  相似文献   

13.
NaBH4 in the presence of charcoal (0.4–0.8 g) reduces varieties of nitroarenes to their corresponding amines. Reduction reactions were carried out in a mixture of H2O‐THF (1:0.5 mL) at 50–60°C with high to excellent yields of products.  相似文献   

14.
The composite/nanocomposite powders of Mn0.5Ni0.5Fe2O4/Fe type were synthesized starting from nanocrystalline Mn0.5Ni0.5Fe2O4 (D = 7 nm) (obtained by ceramic method and mechanical milling) and commercial Fe powders. The composites, Mn0.5Ni0.5Fe2O4/Fe, were milled for up to 120 min and subjected to heat treatment at 600 °C and 800 °C for 2 h. The manganese-nickel ferrite/iron composite samples were subjected to differential scanning calorimetry (DSC) up to 900 °C for thermal stability investigations. The composite component phases evolution during mechanical milling and heat treatments were investigated by X-ray diffraction technique. The present phases in Mn0.5Ni0.5Fe2O4/Fe composite are stable up to 400–450 °C. In the temperature range of 450-600 °C, the interdiffusion phenomena occurs leading to the formation of Fe1?xMnxFe2O4/Ni–Fe composite type. The new formed ferrite of Fe1?xMnxFe2O4 type presents an increased lattice parameter as a result of the substitution of nickel cations into the spinel structure by iron ones. Further increases of the temperature lead to the ferrite phase partial reduction and the formation of wustite-FeO type phase. The spinel structure presents incipient recrystallization phenomena after both heat treatments (600 °C and 800 °C). The mean crystallites size of the ferrite after heat treatment at 800 °C is about 75 nm. After DSC treatment at 900 °C, the composite material consists in Fe1?xMnxFe2O4, Ni structure, FeO, and (NiO)0.25(MnO)0.75 phases.  相似文献   

15.
This study evaluated the production of hydrogen and propionic acid in an expanded granular sludge bed (EGSB) reactor by co-fermentation of cheese whey (CW) and crude glycerol (CG). The reactor was operated at hydraulic retention time (HRT) of 8 h by changing the CW/CG ratio from 5:1 to 5:2, 5:3, 5:4, and 5:5. At the ratio of 5:5, HRT was reduced from 8 to 0.5 h. The maximum hydrogen yield of 0.120 mmol H2 g COD?1 was observed at the CW/CG ratio of 5:1. Increasing the CG concentration repressed hydrogen production in favor of propionic acid, with a maximum yield of 6.19 mmol HPr g COD?1 at the CW/CG ratio of 5:3. Moreover, by reducing HRT of 8 to 0.5 h, the hydrogen production rate was increased to a maximum value of 42.5 mL H2 h?1 L?1at HRT of 0.5 h. The major metabolites were propionate, 1,3-propanediol, acetate, butyrate, and lactate.  相似文献   

16.
Silica–titania mixed oxide were prepared by sol–gel method from tetraethylorthosilicate and titanium (IV) isopropoxide as precursors in the presence of room temperature ionic liquid (RTIL), 1-butyl-3-methylimidazolium bis(trifluoromethylsulfonyl) imide [C4MIm][NTf2]. The effects of [C4MIm][NTf2] on the structural and textural characteristics of silica–titania matrix are investigated in this paper. The materials obtained were well characterized by Fourier transform infrared spectroscopy (FTIR), thermogravimetric analysis X-ray powder diffraction (XRPD), field emission scanning electron microscope (FESEM) and N2 adsorption–desorption analysis. It is believed that the [C4MIm][NTf2] plays an important role as a template and the high surface area of the samples is thought to mainly attribute to the formation of microporous in the reaction. The synthesized materials showed the presence of C–N groups in the FTIR spectrum which indicates the presence of RTIL in the silica–titania matrix. XRPD, FESEM and N2 adsorption–desorption analysis results indicated that the composite materials possessed good microporous character. The subsequent material displayed average pore diameter of 1.70–2.12 nm, pore volume of 0.08–0.19 cm3/g and BET surface area of 191–386 m2/g. Increasing the content of RTIL resulted in an increase of the average pore diameter of the silica–titania gel.  相似文献   

17.
Cobalt ferrite magnetic nanoparticles (CoFe2O4-MNPs) were synthesized by hydrothermal and co-precipitation methods using different precursors such as nitrates, chlorides, and acetates, at different concentrations with/without surfactant under different growth conditions. The structural and morphological analyses reveal the formation of a single-phase CoFe2O4 in nanoplatelet-shaped NPs with average particle size between 11 and 26 nm depending on synthesis condition. The specific surface area of these NPs obtained by hydrothermal method was ~ 34 m2 g?1. Electrochemical performances of the obtained nanoparticles in a three-electrode configuration with a 6 M KOH electrolyte revealed a specific capacitance (C s) of 429 F/g at 0.5 A/g, with excellent capacitance retention of 98.8% after 6000 cycles at 10 A/g for the electro-active NPs synthesized by hydrothermal method at 200 °C for 18 h.  相似文献   

18.
In this study, carbohydrates (cellulose plus hemicellulose) in corncob were effectively converted furfuralcohol (FOL) via chemical–enzymatic catalysis in a one-pot manner. After corncob (2.5 g, dry weight) was pretreated with 0.5 wt% oxalic acid, the obtained corncob-derived xylose (19.8 g/L xylose) could be converted to furfural at 60.1% yield with solid acid catalyst SO4 2?/SnO2-attapulgite (3.6 wt% catalyst loading) in the water–toluene (3:1, v/v) at 170 °C for 20 min. Moreover, the oxalic acid-pretreated corncob residue (1.152 g, dry weight) was enzymatically hydrolyzed to 0.902 g glucose and 0.202 g arabinose. Using the corncob-derived glucose (1.0 mM glucose/mM furfural) as cosubstrate, the furfural liquor (48.3 mM furfural) was successfully biotransformed to FOL by recombinant Escherichia coli CCZU-A13 cells harboring an NADH-dependent reductase (SsCR) in the water-toluene (4:1, v/v) under the optimum conditions (50 mM PEG-6000, 0.2 mM Zn2+, 0.1 g wet cells/mL, 30 °C, pH 6.5). After the bioreduction for 2 h, FAL was completely converted to FOL. The FOL yield was obtained at 0.11 g FOL/g corncob. Clearly, this one-pot synthesis strategy shows high potential application for the effective synthesis of FOL.  相似文献   

19.
Silver-doped silica was prepared by hydrolysis and condensation of tetraethyl orthosilicate (TEOS, Si(OC2H5)4) in the presence of a silver nitrate (AgNO3) solution by two different synthesis methods. In the first synthesis route, sol-gel mixtures were prepared using an acid catalyst. In the second synthesis route, silver-doped silica gels were formed by two-step acid/base catalysis. For the same concentration of silver dopant [AgNO3]/[TEOS] = 0.015 acid-catalyzed sol-gel formed a microporous silica with an average pore size of <25 Å whereas the two-step catalyzed silica had an average pore size of 250 Å and exhibited a mesoporous structure when fully dried. The differences in the pore size affected the silver particle formation mechanism and post-calcination silver particle size. After calcination at 800 °C for 2 h the acid-catalyzed silica contained metallic silver particles size with an average particle size of 24 ± 2 nm whereas two-step catalyzed silica with the same concentration of [AgNO3]/[TEOS] = 0.015 contained silver nanoparticles with an average size of approximately 32 ± 2 nm. Mechanisms for silver particle formation and for silica matrix crystallization with respect to the processing route and calcination temperature are discussed.  相似文献   

20.
Present study describes the adsorption of carbofuran (CF) from aqueous solutions using p-tetranitrocalix[4]arene based modified silica through batch and column methods. Various parameters were optimized including initial pesticide concentrations (5 mg L?1), pH (2–10), contact time (60 min) and adsorbent dosage (30 mg). Modified silica was characterized by FT-IR and scanning electron microscope. The adsorption was further explained by Langmuir, Freundlich and Dubinin–Radushkevich (D–R) models. Moreover, adsorption kinetics and adsorption thermodynamics were also investigated. Adsorption in dynamic mode was evaluated by breakthrough volumes and the Thomas model, applying batch conditions using 30 mg of modified silica at pH 5. It has been noticed that CF removal efficiency of modified silica was 98 % as compared to bare silica (48 %). Adsorption of CF on modified silica was found to be multilayer and physical in nature. Consequently, adsorption obeys pseudo-second-order kinetic equation following external mass transfer diffusion process as the rate-limiting step. Thermodynamic parameter (ΔG, ΔS, ΔH) values suggest that the adsorption of CF is spontaneous and exothermic in nature. Thomas model rate constant k TH (cm3 mg?1 min?1) and maximum solid phase concentration (q o mg g?1) was found to be 0.52 and 12.3, respectively, in dynamic mode.  相似文献   

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