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1.
The supramolecular interaction of curcumin and beta-cyclodextrin (beta-CD) has been studied by spectrophotometry. The mechanism of the inclusion was studied and discussed based on the variations of pK(a), absorption intensity, and infrared spectrograms. The results show that beta-CD reacts with curcumin to form a 2:1 host-guest complex with an apparent formation constant of 5.53 x 10(5) mol(-2) x L2. Based on the enhancement of the absorbance of curcumin produced through complex formation, a spectrophotometric method for the determination of curcumin in bulk aqueous solution in the presence of beta-CD was developed. The linear relationship between the absorbance and curcumin concentration was obtained in the range of 0-15 microg/mL, with a correlation coefficient (r) of 0.9991. The detection limit was 0.076 microg/mL. The proposed method was used to determine the curcumin in curry and mustard with satisfactory results.  相似文献   

2.
A highly sensitive extractive spectrophotometric method has been developed for the determination of copper(II) using pyridoxal-4-phenyl-3-thiosemicarbazone(PPT) as an analytical reagent. The PPT forms reddish brown species of copper(II) at a pH range of 3.0-5.5, and the complex was extracted into n-butanol. The Cu(II)-PPT complex shows maximum absorbance at 440 nm, with molar absorptivity and Sandell's sensitivity being 2.16 x 10(4) L mol(-1) cm(-1) and 2.94 x 10(-3) microg cm(-2), respectively. The system obeys Beer's law in the range of 0.2-5.0 mg/L. The regression coefficient of the Beer's law straight line is 0.338, and the correlation coefficient is 0.96. The detection limit of the method is 0.0065 microg mL(-1). Most of the common metal ions generally found associated with copper do not interfere. The repeatability of the method was checked by finding the relative standard deviation. The developed method has been successfully employed for the determination of copper(II) in leafy vegetable and pharmaceutical samples. The method is evaluated by analyzing samples from the Bureau of Analyzed Samples (BCS 233, 266, 216/1, 207, and 179) and by intercomparison of experimental values using AAS.  相似文献   

3.
Olive leaf extract, rich in oleuropein, formed an inclusion complex with beta-cyclodextrin (beta-CD) upon mixing of the components in aqueous media and subsequent freeze-drying. Inclusion complex formation was confirmed by differential scanning calorimetry (DSC). DSC thermograms indicated that the endothermic peaks of both the olive leaf extract and the physical mixture of olive leaf extract with beta-CD, attributed to the melting of crystals of the extract, were absent in DSC thermogram of inclusion complex. Moreover, DSC studies under oxidative conditions indicated that the complex of olive leaf extract with beta-CD was protected against oxidation, since it remained intact at temperatures where the free olive leaf extract was oxidized. Phase solubility studies afforded A L type diagrams, 1:1 complex stoichiometry, a moderate binding constant ( approximately 300 M (-1)), and an increase of the aqueous solubility by approximately 50%. The formation of the inclusion complex was also confirmed by nuclear magnetic resonance (NMR) studies of beta-CD solutions in the presence of both pure oleuropein and olive leaf extract. The NMR data have established the formation of a 1:1 complex with beta-CD that involves deep insertion of the dihydroxyphenethyl moiety inside the cavity from its secondary side.  相似文献   

4.
A flow injection spectrophotometric procedure with enzymatic hydrolysis was developed for determination of orthophosphate, phytate and total phosphorus in cereal samples. Phosphorus species were extracted from cereals with 0.05 mol L(-1) potassium hydrogen phthalate buffer solution at pH 5.7. Orthophosphate was directly determined in the extracts by molybdenum blue spectrophotometric method. The phytate was hydrolyzed by the enzyme phytase coupled to a solid phase packed into an enzymatic reactor, and the resulting hydrolyzed orthophosphate was also determined by spectrophotometry at 650 nm. After optimization for phosphorus species extraction and enzymatic hydrolysis, a linear calibration graph was obtained up to 196 x 10(-6) mol L(-1) orthophosphate (P conc = -2.67 + 0.52x, r = 0.9998). Measurements are characterized by relative standard deviation of 1.6% for a standard of 72 x 10(-6) mol L(-1) orthophosphate and no baseline drift was observed during 4 h operation periods. It provides 72 measurements per hour, with 2.4 x 10(-)6) mol L(-1) and 7.9 x 10(-6) mol L(-1) as detection and quantification limits, respectively.  相似文献   

5.
A direct determination of gallic acid was achieved at a carbon paste electrode modified with carbon nanotubes under differential pulse voltammetry conditions. The values obtained for gallic acid were used to estimate the antioxidant properties of the wine sample based on gallic acid oxidation. The proposed method is based on the gallic acid oxidation process at a modified carbon paste electrode (MCPE) containing 30% (m/m) of carbon nanotubes monitored at 0.35 V versus Ag/AgCl (KCl 3 mol L(-1)). Using the optimized experimental conditions, the calibration curve for gallic acid was linear in the concentration range from 5.0 × 10(-7) to 1.5 × 10(-5) mol L(-1) with a detection limit of 3.0 × 10(-7) mol L(-1). The MCPE was successfully applied for the determination of the antioxidant capacity for red and white wine samples without interference of glucose and ascorbic acid, and the obtained results were compared with the standard spectrophotometric method.  相似文献   

6.
A tungsten carbide coating on the integrated platform of a transversely heated graphite atomizer was used as a modifier for the direct determination of Se in soil extracts by graphite furnace atomic absorption spectrometry. Diethylenetriaminepentaacetic acid (0.0050 mol L(-1)) plus ammonium hydrogencarbonate (1.0 mol L(-1)) extracted predominantly available inorganic selenate from soil. The formation of a large amount of carbonaceous residue inside the atomizer was avoided with a first pyrolysis step at 600 degrees C assisted by air during 30 s. For 20 microL of soil extracts delivered to the atomizer and calibration by matrix matching, an analytical curve (10.0-100 microgram of L(-1)) with good linear correlation (r = 0.999) between integrated absorbance and analyte concentration was established. The characteristic mass was approximately 63 pg of Se, and the lifetime of the tube was approximately 750 firings. The limit of detection was 1.6 microgram L(-1), and the relative standard deviations (n = 12) were typically <4% for a soil extract containing 50 microgram of L(-1). The accuracy of the determination of Se was checked for soil samples by means of addition/recovery tests. Recovery data of Se added to four enriched soil samples varied from 80 to 90% and indicated an accurate method.  相似文献   

7.
The thermal stability of anthocyanin extract isolated from the dry calyces of Hibiscus sabdariffa L. was studied over the temperature range 60-90 degrees C in aqueous solutions in the presence or absence of beta-cyclodextrin (beta-CD). The results indicated that the thermal degradation of anthocyanins followed first-order reaction kinetics. The temperature-dependent degradation was adequately modeled by the Arrhenius equation, and the activation energy for the degradation of H. sabdariffa L. anthocyanins during heating was found to be approximately 54 kJ/mol. In the presence of beta-CD, anthocyanins degraded at a decreased rate, evidently due to their complexation with beta-CD, having the same activation energy. The formation of complexes in solution was confirmed by nuclear magnetic resonance studies of beta-CD solutions in the presence of the extract. Moreover, differential scanning calorimetry revealed that the inclusion complex of H. sabdariffa L. extract with beta-CD in the solid state was more stable against oxidation as compared to the free extract, as the complex remained intact at temperatures 100-250 degrees C where the free extract was oxidized. The results obtained clearly indicated that the presence of beta-CD improved the thermal stability of nutraceutical antioxidants present in H. sabdariffa L. extract, both in solution and in solid state.  相似文献   

8.
The fluorescence intensity of the norfloxacin (NFX)-Tb3+ complex enhanced by DNA was studied. Therefore, a sensitive fluorescence method for the determination of DNA was developed. The optimal conditions of the method were as follows: the hexamethylenamine (HMA)-HCl buffer was adopted for adjusting the pH to 6.5 +/- 0.1, the concentrations of NFX and Tb3+ were both fixed in 1.0 x 10(-6) mol L(-1), and the excitation and emission wavelengths were selected at 290 and 545 nm, respectively. Under the optimal conditions, the enhanced fluorescence intensity was in proportion to the concentration of DNA in the same range of 5.0 x 10(-9) - 1.0 x 10(-6) g mL(-1) for hsDNA and thermally denatured ctDNA. The detection limits (S/N = 3) were 0.9 and 0.6 ng mL(-1), respectively. In addition, the interaction between NFX-Tb3+ and DNA was discussed in detail. The experimental results from UV absorption spectra, fluorescence spectra, and the salt effect study indicated that the interaction between norfloxacin-Tb3+ complex and DNA had at least two different binding modes: the electrostatic binding and the intercalation binding. The mechanism of the fluorescence enhancement effect was also discussed.  相似文献   

9.
Tocopherols (alpha, beta, gamma, and delta) and Trolox were found to deactivate triplet-excited riboflavin in homogeneous aqueous solution (7:3 v/v tert-butanol/water) with second-order reaction rates close to diffusion control [k2 between 4.8 x 10(8) (delta-tocopherol) and 6.2 x 10(8) L mol(-1) s(-1) (Trolox) at 24.0 +/- 0.2 degrees C] as determined by laser flash photolysis transient absorption spectroscopy. In aqueous buffer (pH 6.4) the rate constant for Trolox was 2.6 x 10(9) L mol(-1) s1 and comparable to the rate constant found for ascorbate (2.0 x 10(9) L mol(-1) s(-1)). The deactivation rate constant was found to be inferior in heterogeneous systems as shown for alpha-tocopherol and Trolox in aqueous Tween-20 emulsion (approximately by a factor of 4 compared to 7:3 v/v tert-butanol/water). Neither beta-carotene (7:3 v/v tert-butanol/water and Tween-20 emulsion), lycopene (7:3 v/v tert-butanol/water), nor crocin (aqueous buffer at pH 6.4, 7:3 v/v tert-butanol/water, and Tween-20 emulsion) showed any quenching on the triplet excited state of riboflavin. Therefore, all carotenoids seem to reduce the formation of triplet-excited riboflavin through an inner-filter effect. Activation parameters were based on the temperature dependence of the triplet-excited deactivation between 15 and 35 degrees C, and the isokinetic behavior, which was found to include purine derivatives previously studied, confirms a common deactivation mechanism with a bimolecular diffusion-controlled encounter with electron (or hydrogen atom) transfer as rate-determining step. DeltaH for deactivation by ascorbic acid, Trolox, and homologue tocopherols (ranging from 18 kJ mol(-1) for Trolox in Tween-20 emulsion to 184 kJ mol(-1) for ascorbic acid in aqueous buffer at pH 6.4) showed a linear dependence on DeltaS (ranging from -19 J mol(-1) K(-1) for Trolox in aqueous buffer at pH 6.4 to +550 J mol(-1) K(-1) for ascorbic acid in aqueous buffer pH 6.4). Among photooxidation products from the chemical quenching, lumicrome, alpha-tocopherol quinones and epoxyquinones, and alpha-tocopherol dimers were identified by ESI-QqTOF-MS.  相似文献   

10.
A simple flow injection potentiometric (FIP) system, which uses a tubular cobalt electrode, has been developed for phosphorus nutritional evaluation of seeds and grains. Inorganic phosphorus, P(i), is determined using a 1 x 10(-2) mol.L(-1) potassium phthalate buffer solution adjusted at pH 4. A sensitivity of 47 mV/decade and an operating range from 10 to 1000 mg.L(-1) (1 x 10(-4)-1 x 10(-2) M) of dihydrogen phosphate are obtained. The inositol phosphates amount, which is referred to the organic phosphorus, P(org), is directly determined from extracts using a 1 x 10(-2) mol.L(-1) Tris-HCl buffer solution adjusted at pH 8. A sensitivity of 127 mV/decade and an operating range of 10-1000 mg.L(-1) (2.5 x 10(-4)-5 x 10(-3) M) of P(org) (expressed as inositol hexakisphosphoric acid monocalcium) are achieved. Some samples of seed and grain are analyzed by an ICP-OES and a spectrophotometric method to compare results to the developed flow system; no significant differences at the 95% confidence level are observed using a paired t test. Other samples such as animal nursing feed, soybean meal, and corn are also analyzed with the proposed FIP system, showing a good correlation to the ICP-OES values.  相似文献   

11.
A procedure has been developed for the determination of iron(III) dimethyldithiocarbamate by converting it into the iron(II)-bathophenanthroline complex, which is then dissolved in acetone-water (1:1), and the absorbance is measured at 534 nm against a reagent blank. Beer's law is obeyed over the concentration range 0.5-20 microg x mL(-1) in the final solution. The method is sensitive and highly selective and is used for the direct determination of ferbam in a commercial sample and in mixtures with various dithiocarbamates (ziram, zineb, maneb, etc.) and from wheat grains.  相似文献   

12.
Two kinds of Schiff base metal complexes of 2-hydroxy-1-naphthaldehyde-2-amino-5-phenylthiazole (HANPTS), Mn(II)(HNAPTS)(2) and Fe(III)(HNAPTS)(2), were synthesized and used to mimic the active group of horseradish peroxidase (HRP). The catalytic characteristics of the mimic enzymes in the oxidation reaction of ascorbic acid (AsA) with the OOH group in polyethylene glycols (PEGs) have been studied by a spectrophotometric method. Fe(III) has remarkable coordinated catalysis to Mn(II)(HNAPTS)(2); as a result, the catalytic ability of Fe(III)-Mn(II)(HNAPTS)(2) is 75% of that of HRP. The possible mechanism of the reaction was discussed. The linear relationship between deltaA(265)(AsA) and OOH group concentrations was in the range of 1.5 x 10(-6) to 9.0 x 10(-4) mol/L. The proposed method was successfully applied to the determination of the OOH group level in different molecular weight PEGs.  相似文献   

13.
A study has been made of the analytical application of a nafcillin-imprinted sol-gel to the direct determination of the beta-lactamic antibiotic in spiked milk-based samples using a room temperature phosphorescent flow-through system. The influence of the sample matrix on the transduction and the recognition processes was statistically determined, and results demonstrated that the imprinted sol-gel optosensing system could be effectively applied to real sample analysis. The analytical performance characteristics were as follows: The detection limit results for aqueous and skimmed milk were 5.8 x 10(-6) and 3.3 x 10(-5) mol L(-1), respectively, and a relative standard deviation less than 5% was found for both matrices. Statistical analysis of variance studies have been shown to have no significant effect on different skimmed milk commercial products over the imprinted material recognition. This fact provides an indicator of the ruggedness/robustness of the proposed analytical system and the possibility to use external real matrix calibration. Application of the method to nafcillin analysis in other milk-based samples is outlined.  相似文献   

14.
The efficacy of thiabendazole (TBZ) to control postharvest decay caused by Penicillium digitatum of citrus fruit can be enhanced by co-application with sodium bicarbonate (SBC) and/or heat treatment. The impact of these treatments was investigated in citrus fruit, as a function of TBZ and SBC concentration and temperature, and were related to the amount of TBZ residues in fruit (total residues), in fruit surface, in the cuticular wax, and in the inner fruit. The residue levels of TBZ were determined in 'Valencia' oranges following a 1 min dip in an aqueous mixture of SBC at 0.5, 1, or 2 wt %/vol and TBZ at 600 or 400 mg/L (active ingredient, a.i.) at 20 or 40 degrees C and after 0 and 20 days at 17 degrees C and 90% relative humidity. The influence of SBC and heat on the TBZ residue concentration on the fruit surface, in cuticular wax, and on the inner cuticle tissue was determined in 'Salustiana' oranges after a 1 or 3 min dip in TBZ alone at 600 mg/L and 20 or 50 degrees C or for 1 min in TBZ at 600 mg/L and SBC at 2% and 20 degrees C. The efficacy of heat treatments with water, SBC, and TBZ, applied separately or in combination, was investigated on artificially inoculated 'Nova' mandarins and 'Valencia' oranges for the control of postharvest green mold caused by a TBZ-sensitive (TBZ-s) or TBZ-resistant (TBZ-r) isolate of P. digitatum. The residue levels of TBZ in fruit, evaluated as total residues, were not affected by the co-application of SBC in most samples. While TBZ residues in the fruit surface were not significantly affected by the dip temperature or by co-application of SBC, the rates of diffusion and penetration of TBZ into cuticular wax markedly increased in the presence of SBC or when TBZ was applied in combination with heat. TBZ residues in the inner tissue of fruits treated at 20 degrees C were not dependent upon the dip time or by the presence of SBC and were similar to those found in fruit treated with TBZ at 50 degrees C for 1 min, whereas significantly higher values were recorded in samples treated with TBZ at 50 degrees C for 3 min. When TBZ at 600 mg/L and 20 degrees C was applied in the presence of SBC at concentrations of 1-2 or 0.5-2%, it effectively reduced decay caused by the TBZ-resistant isolate of green mold in 'Nova' mandarins and 'Valencia' oranges. This treatment was also significantly more effective than TBZ alone to control green mold caused by a TBZ-s isolate in 'Valencia' oranges. The combination with SBC and mild heat (40 degrees C) and TBZ at 400 mg/L generally improved the control of a TBZ-r isolate of green mold with respect to the combined treatment at 20 degrees C. TBZ efficacy was also improved when applied at reduced rates (200 mg/L) and 50 degrees C, significantly suppressing green mold caused by a TBZ-s isolate of P. digitatum and effectively controlling a TBZ-r isolate. The rate of weight loss of 'Valencia' oranges was significantly increased by SBC treatment and was positively dependent upon the concentration of SBC used in the treatment, while the temperature of the treatment solution had little influence on later weight loss.  相似文献   

15.
Photoirradiation of soy oil with UV/visible light has been shown to produce significant amounts of trans,trans conjugated linoleic acid (CLA) isomers through conversion of various synthesized intermediate cis,trans isomers. The objective of this study was to determine the kinetics of CLA isomers synthesis to better understand the production of various isomers. Soy oil was irradiated with UV/visible light for 144 h in the presence of an iodine catalyst and CLA isomers analyzed by gas chromatography (GC). Arrhenius plots were developed for the conversion of soy oil linoleic acid (A) to form cis-, trans/trans-, cis-CLA (B), conversion of cis-, trans/trans-, cis-CLA to form trans,trans-CLA (C) with respect to B, and formation of trans,trans-CLA isomers with respect to C. The kinetics of consumption of linoleic acid (LA) to form cis-, trans/trans-, cis-CLA was found to be of second-order with a rate constant of 9.01 x 10-7 L/mol s. The rate of formation of cis-, trans/trans-, cis-CLA isomers depends on the rate of formation from LA and its rate of consumption to form trans,trans-CLA isomers. The conversion of cis-, trans/trans-, cis-CLA isomers to trans,trans-CLA isomers was found to be of first-order with a rate constant of 2.75 x 10-6 s-1. However, the formation of thermodynamically stable trans,trans-CLA isomers (C) with respect to C was found to be a zero-order reaction with a rate constant of 10.66 x 10-7 mol/L s. The consumption of LA was found to be the rate-determining step in the CLA isomers formation reaction mechanism. The findings provide a better understanding of the mechanism of CLA isomers synthesis by photoirradiation and the factors controlling the ratio of various isomers.  相似文献   

16.
The effect of beta-cyclodextrin (beta-CD) on the improvement of the fungicidal activity of iprodione has been investigated. The inclusion complexation of beta-CD with iprodione has been prepared and characterized by integrating some analytical techniques (such as electrospray ionization-mass spectrometry, differential scanning calorimetry, thermogravimetry, x-ray diffraction, and scanning electron microscopy) and molecular simulation methods. The beta-CD/iprodione inclusion complex has exhibited different spectroscopic features and properties from iprodione. The stoichiometric ratio and stability constant describing the extent of formation of inclusion complexes have been determined by phase solubility studies. The calculated apparent stability constant of the iprodione/beta-CD complex was 407.5 M-1. The obtained inclusion complexes were found to significantly improve the water solubility of iprodione, and there is a 4.7-fold increase in the presence of 13 mM beta-CD as compared with the solubility of iprodione in deionized water in the absence of beta-CD. The bioassay demonstrated that the complex displayed over two-fold increase of the fungicidal activity. In addition, the possible structure of the beta-CD/iprodione complex was proposed according to the results of the molecular dynamic simulation. The present study provided useful information for a more rational application of iprodione, diminishing the use of organic solvents and increasing its efficacy.  相似文献   

17.
The liquid chromatographic determination previously developed for benzimidazoles in cattle liver has been slightly modified and applied to the determination of 4 benzimidazoles in milk. Recoveries of fenbendazole (FBZ), oxfendazole (OFZ), and thiabendazole (TBZ) from milk fortified at the 10 ppb level were 80% or greater with an intralaboratory coefficient of variation of 11% or less. Recovery of 5-hydroxythiabendazole (5-OH-TBZ) at the 30 ppb level averaged 56% with an intralaboratory coefficient of variation of 5%. Limited data on the depletion of FBZ, OFZ, TBZ, and 5-OH-TBZ in milk were also generated.  相似文献   

18.
Natamycin is a broad spectrum antimycotic with very low water solubility, which is used to extend the shelf life of shredded cheese products. beta-Cyclodextrin (beta-CD), hydroxypropyl beta-cyclodextrin (HP beta-CD), and gamma-cyclodextrin (gamma-CD) were found to form inclusion complexes with natamycin in aqueous solution. The increase in solubility of natamycin with added beta-CD was observed to be linear (type A(L) phase solubility diagram). The 1:1 stability constant of natamycin:beta-CD complex was estimated from its phase solubility diagram to be 1010 M(-1). The phase solubility diagrams of both gamma-CD and HP beta-CD exhibited negative deviation from linearity (type A(N) diagram) and, therefore, did not allow the estimation of binding constants. The water solubility of natamycin was increased 16-fold, 73-fold, and 152-fold with beta-CD, gamma-CD, and HP beta-CD, respectively. The natamycin:CD inclusion complexes resulted in in vitro antifungal activity nearly equivalent to that of natamycin in its free state.  相似文献   

19.
The supramolecular interaction of disulfide linked β-cyclodextrin (β-CD) dimer and dimethomorph has been studied by spectrofluorimetry. Based on the significant enhancement of the fluorescence intensity of dimethomorph, a new spectrofluorimetric method with high sensitivity and selectivity was developed for the determination of dimethomorph in bulk aqueous in the presence of the disulfide linked β-CD dimer. The inclusion complexation behavior of β-CD dimer with dimethomorph was studied in a KH(2)PO(4)-H(3)PO(4) buffer solution of pH 3.86 at room temperature. The apparent association constant of the complex was 2.25 × 10(4) L/mol. The linear range was 12-7500 ng/mL with the detection limit 3.70 ng/mL, and the limit of quantification was 12.4 ng/mL. The proposed method had been successfully applied to the determination of dimethomorph residues in vegetables with recoveries of 89.0-115%.  相似文献   

20.
A technique of high-performance liquid chromatography (HPLC) was described for the measurement of total uronic acids in tea polysaccharide conjugates. This method was applied to polysaccharide conjugate extracts obtained from green tea after most of the components that produce interference were removed. The preliminary extraction process was according to the procedure of isolation of polysaccharide conjugates. The uronic acid content of different polysaccharide conjugate fractions was quantified by HPLC on a Sugar-Pak I column with a 1.0 x 10(-)(4) mol x L(-)(1) calcium disodium ethylenediaminetetraacetic acid solution as the mobile phase and refractive index detection. The validation study showed high recoveries (>97.0%) and low coefficients of variance (<3.0%). The minimum detectable limit concentration of uronic acid was 10 microg x mL(-)(1). The analysis of a standard range of galacturonic acid concentrations (100-4000 microg x mL(-)(1)) yielded linear results. The use of the method on different polysaccharide conjugate fraction samples confirmed its effectiveness. With the high content of uronic acids in polysaccharide conjugates, the stronger reactive oxygen species scavenging activities were found.  相似文献   

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