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1.
A fast, simple, and reliable method for the isolation and determination of the vitamins thiamin, riboflavin, niacin, pantothenic acid, pyridoxine, folic acid, cyanocobalamin, and ascorbic acid in food samples is proposed. The most relevant advantages of the proposed method are the simultaneous determination of the eight more common vitamins in enriched food products and a reduction of the time required for quantitative extraction, because the method consists merely of the addition of a precipitation solution and centrifugation of the sample. Furthermore, this method saves a substantial amount of reagents as compared with official methods, and minimal sample manipulation is achieved due to the few steps required. The chromatographic separation is carried out on a reverse phase C18 column, and the vitamins are detected at different wavelengths by either fluorescence or UV-visible detection. The proposed method was applied to the determination of water-soluble vitamins in supplemented milk, infant nutrition products, and milk powder certified reference material (CRM 421, BCR) with recoveries ranging from 90 to 100%.  相似文献   

2.
A rapid, simple, and reliable liquid chromatographic method has been developed for the simultaneous determination of nicotinamide (niacinamide), thiamine, riboflavin, riboflavin sodium phosphate, pyridoxine, caffeine, and sodium benzoate in commercial oral liquid tonics. The 7 components are separated on a reverse phase C18 column using a mobile phase of acetonitrile-0.01M potassium dihydrogen phosphate-triethylamine (8 + 91.5 + 0.5 v/v/v) containing 5mM sodium octanesulfonate and adjusted to pH 2.8 with phosphoric acid. Components are detected at 254 nm with attenuation 0.02 AUFS. Acetanilide is used as an internal standard. In addition to the 7 components mentioned, nicotinic acid (niacin), cyanocobalamin, and folic acid are also separated under the same conditions. Sample preparation involves only addition to internal standard solution and dilution with mobile phase and then filtration. Recoveries of the 7 components and cyanocobalamin from spiked preparations ranged from 97 to 104% with coefficients of variation of 0.9-4.2%.  相似文献   

3.
A simple and rapid method is presented for the liquid chromatographic assay of ascorbic acid, niacinamide, pyridoxine, thiamine, and riboflavin from a single chromatogram. Ion-pair chromatography with a reverse phase C18 cartridge in a radial compression system is used. Quantitation is excellent with a total analysis time of less than 20 min. A mobile phase of methanol-water (15 + 85) (0.005M heptanesulfonic acid) with 0.5% triethylamine at pH 3.6 and a flow rate of 2.0 mL/min gives the most satisfactory separation of the 5 water-soluble vitamins. By using 2 detectors in series set at different wavelengths and sensitivities, all 5 vitamins, with peak heights on scale, can be measured from a single injection; peak elution order is ascorbic acid, niacinamide, pyridoxine, thiamine, and riboflavin. Ascorbic acid is measured at 254 nm and the other vitamins, at 280 nm. The amount of amine modifier in the mobile phase is critical to the separation of niacinamide and pyridoxine. Recoveries of 5 water-soluble vitamins from spiked placebos were in the range of 98.2-102.0%. Confidence limits, +/- 3 SD, were in the range of 1.0-5.4%. Overall, the results obtained using the liquid chromatographic method show excellent agreement with manual methods and automated analysis.  相似文献   

4.
Studies were conducted to determine the relationship of vitamin production and ability to dissolve bicalcium phosphate in bacteria isolated from rhizosphere, rhizoplane and control soil. Production of vitamin B12, riboflavin, niacin, pantothenate and biotin was determined using a bioassay procedure that may be useful for large-scale screening of bacteria for vitamin production.Among isolates producing one or more vitamins, 76.4, 37.5 and 57.5% of control, rhizosphere and rhizoplane isolates, respectively, solubilized phosphate. However, phosphate-solubilizing isolates from rhizosphere and rhizoplane were more active vitamin producers than solubilizing isolates from control soil, and non-solubilizing isolates from any of the three regions.Production of vitamin B12, riboflavin and niacin by rhizosphere isolates and of riboflavin by rhizoplane isolates was also correlated with ability to solubilize phosphate, but similar relationships were not observed for control isolates.  相似文献   

5.
Reported here is a simple liquid chromatographic (LC) method for the determination of riboflavin in milk (liquid, evaporated, and dry), yogurt, and cheese. The method involves passing liquid samples or filtrates of semisolid and solid samples through a C18 cartridge. Retained riboflavin is then eluted with an aliquot of 50% methanol in 0.02M acetate buffer of pH 4. A volume of the eluate is injected into the LC system consisting of a C18 column, a solvent of water-methanol-acetic acid (65 + 35 + 0.1, v/v) with a flow rate of 1 mL/min, and a UV detector set at 270 nm. The method is precise and accurate and compares favorably with the present AOAC method. Moreover, it involves fewer sample preparation steps and has a total analysis time of less than 1 h.  相似文献   

6.
Two independently developed liquid chromatography (LC) methods for the quantitative determination of biotin in multivitamin/multielement tablets (NIST Standard Reference Material 3280 (SRM 3280)) are described. The methods use distinctly different tablet extraction solvents (methanol vs 1.5% aqueous formic acid) and analyte detection principles (mass spectrometry (MS) versus evaporative light-scattering detection (ELSD)) to ensure quantitative reliability. The use of different extraction and detection procedures allows cross-validation of the methods and enhances confidence in the final quantitative results. Both methods yield highly comparable results for the mean level of biotin (LC/MS = 26.5 mg/kg +/- 0.3 mg/kg (n = 12); LC/ELSD = 24.7 mg/kg +/- 1.7 mg/kg (n = 12)) in SRM 3280, yet the methods differ considerably in their analytical characteristics. The isotope-dilution LC/MS method exhibits excellent linearity from 0.02 ng to 77 ng biotin on-column with a method limit of detection (LOD) and limit of quantification (LOQ) of 0.02 ng (S/N > 3) and 0.06 ng (S/N > 10) biotin on-column, respectively. The LC/ELSD method exhibits good linearity from 155 ng to 9900 ng biotin on-column with a method LOD and LOQ of 155 ng (S/N > 3) and 310 ng (S/N > 10) biotin on-column, respectively. Method performance data indicates that the LC/MS method is analytically superior to the LC/ELSD method; however, either method in combination with SRM 3280 should provide quality assurance, accuracy, and traceability for biotin levels in multivitamin/multielement dietary supplements.  相似文献   

7.
A simple, rapid liquid chromatographic (LC) method that uses UV/VIS detection has been developed for the determination in eggs of residues of the histomonostats dimetridazole (DMZ), ronidazole (RON), ipronidazole (IPR), and side-chain hydroxylated metabolites of DMZ and RON. Sample pretreatment includes an aqueous extraction, purification with an Extrelut cartridge, and acid partitioning with isooctane. An aliquot of the final aqueous extract is injected into a reverse-phase LC system; detection is performed at 313 nm. The limits of determination are in the 5-10 microgram/kg range. A UV/VIS spectrum can be obtained at the 10 microgram/kg level by using diode-array UV/VIS detection. Recoveries are between 80 and 98% with a coefficient of variation of about 5%. Some 20 samples can be analyzed per day. A side-chain hydroxylated metabolite of IPR can also be detected with this method, as demonstrated with samples from animal experiments. After a single oral dose of the drugs to laying hens, residues of the parent compound and/or the hydroxylated metabolites could be detected in eggs 5-8 days after dosing. Plasma distribution and excretion in feces were established both with and without deconjugation. DMZ and IPR were extensively metabolized to hydroxylated nitroimidazole metabolites; RON was excreted mainly as the parent compound.  相似文献   

8.
Bread flour was spiked with folic acid (1.40 mg/lb or 3.08 μg/g of flour) and processed into bread by the sponge and dough method. Changes that occurred to added folic acid and endogenous folate contents through different processing stages, including sponge formation, proofing, and baking, were assessed by reversed‐phase ion‐pair HPLC combined with UV and fluorometric detection. Sample extraction required α‐amylase and rat plasma deconjugase digestion, and sample preparation required purification by solid‐phase extraction. Added folic acid was measured by monitoring UV absorption at 280 nm. Four selected forms of endogenous folates including tetrahydrofolate (THF), 5‐formyl‐THF, 10‐formylfolate, and 5‐methyl‐THF were identified and quantified throughout the bread processing using a fluorescence excitation wavelength of 290 nm and emission wavelength of 350 or 450 nm. Data indicate a relatively good stability of added folic acid and native folates to the baking process, and increased endogenous folate contents in dough and bread as compared with the flour from which they were made.  相似文献   

9.
A method is described for the determination of vitamins D2 + D3 in milk- and soy-based infant formula. Vitamins D2 and D3 are extracted from the saponified sample and converted to isotachysterols with acidified butanol. Reverse-phase liquid chromatography (LC) is used to remove interferences, and total vitamin D is quantitated using normal-phase LC. Recoveries of spiked samples averaged 97.6% for milk-based infant formula, and 98.8% for soy-based infant formula. This method quantitates vitamin D2 + D3 in infant formulas containing as low as 40 IU/qt when prepared according to label direction.  相似文献   

10.
 We have estimated the production of water-soluble B vitamins by plant growth-promoting rhizobacterium Pseudomonas fluorescens strain 267 in a minimal medium with different C sources and at different pH values. In the minimal medium, strain 267 produced large amounts of niacin (0.92 μg ml–1) and pantothenic acid (0.75 μg ml–1), but also other vitamins such as biotin, thiamine, cobalamine and pyridoxine. The production of B vitamins was dependent on the C source and pH of the growth medium. By random Tn5 mutagenesis, thiamine and niacin auxotrophs were isolated from P. fluorescens strain 267 and mutants were used to evaluate the vitamin production on colonization of clover roots under controlled conditions. Red clover root colonization decreased by about 1 order of magnitude in the case of the niacin auxotroph. The vitamin auxotrophs of P. fluorescens in a mixed inoculation of clover with R. leguminosarum bv. trifolii strain 24.1 showed no plant growth-promotion activity. Received: 23 May 2000  相似文献   

11.
A liquid chromatographic method is described for the analysis of natural vitamin E homologues, all-rac-alpha-tocopheryl acetate, retinyl palmitate (encapsulated and nonencapsulated), and beta-carotene in various fortified foods. The vitamins are extracted in 2-propanol and hexane without saponification and quantitated by normal phase chromatography with fluorescence and visible detection. The sample components were identified using an on-line three-dimensional photodiode array detector, which permitted profiling of the 190-800 nm absorption spectrum of any chromatographic peak. The method showed linearity for the analytes in their respective calibration ranges. The percent recoveries for retinyl palmitate using starch- and gelatin-encapsulated standards were 101.0 +/- 1.0 and 100.1 +/- 0.9, respectively. The method measures six or more analytes in a single injection and differentiates between natural and synthetic forms of vitamin E.  相似文献   

12.
In acidic medium, stanozolol reacts with phenoldisulfonic acid to form a stable yellow chromophore, which is quantitated by spectrophotometry at 385 nm. The reaction gives a linear response at concentrations from 5 to 50 micrograms/mL. The method is suitable for routine analytical control of stanozolol and its formulations.  相似文献   

13.
A method for the determination of vitamins D2 + D3 in fortified milk is described. Vitamins D2 and D3 are extracted from the saponified sample and converted to isotachysterols with antimony trichloride. The isotachysterols are quantitated using liquid chromatography with ultraviolet detection at 301 nm, which is the absorption maximum. At this wavelength other materials present in the sample do not interfere with the analysis of isotachysterols and therefore a cleanup step is avoided. Recoveries of vitamin D added to skim milk were 98.1% (SD 5.3), 96.7% (SD 3.3), and 96.0% (SD 5.1) for samples fortified with 200, 400, and 600 IU/quart, respectively. For whole milk, recoveries were 102.0% (SD 6.5) and 97.1% (SD 3.5) in samples fortified with vitamin D equivalent to 200 and 400 IU/quart, respectively. The detection limit for vitamin D is 40 IU/quart.  相似文献   

14.
Recent methods for determination of thiamine (thiochrome) and riboflavin by liquid chromatography (LC) are outlined and discussed, and a new method allowing the simultaneous determination of these 2 vitamins by using a single fluorescence detector is described. This system involves an ODS 5 micron ultrasphere column and a pH 7.5 mobile phase composed of 0.005M tetrabutyl ammonium phosphate in methanol-water (20 + 80).  相似文献   

15.
Unpublished data on the chemical composition and nutritional value of Pleurotus mushrooms, growing on Umbelliferous plants (Apiaceae), are here reported. Cultivated basidiomata of four different Pleurotus taxa were analyzed in order to evaluate the composition in lipids, sugars, nitrogen, water, vitamins, ashes, and energetic values. The results showed that Pleurotus mushrooms are suitable in every type of diet thanks to their low caloric content, gastronomic value, vitamins, and mineral salt contents. The presence of a high content of vitamin B(12) and riboflavin in Pleurotus nebrodensis is noteworthy.  相似文献   

16.
A liquid chromatographic (LC) method is described for determination of ethopabate residues in chicken tissues. The drug is extracted from tissues with acetonitrile, and the extract is concentrated to 2-3 mL. This aqueous solution is rinsed with ethyl acetate and cleaned up by Florisil column chromatography. LC analysis is carried out on a Zorbax ODS column, and ethopabate is quantitated by using a fluorometric detector set at 306 nm (excitation) and 350 nm (emission). Recoveries of ethopabate added to chicken tissues at levels of 0.01 and 0.05 ppm were 87.8 and 92.7%, respectively. The detection limit was 100 pg for ethopabate standard, and 0.5 ppb in chicken tissues.  相似文献   

17.
This study compared the compositional changes in mushrooms exposed to sunlight with those occurring after commercial ultraviolet (UV) light processing. Button mushrooms (75 kg) were processed in the presence or absence of UVB light; a third group was exposed to direct sunlight. Mushroom composition was evaluated using chemical analyses. Vitamin D concentrations were 5, 410, and 374 μg/100 g (dw) in control, UVB, and sunlight groups, respectively. On a dry weight basis, no significant changes in vitamin C, folate, vitamins B(6), vitamin B(5), riboflavin, niacin, amino acids, fatty acids, ergosterol, or agaritine were observed following UVB processing. Sunlight exposure resulted in a 26% loss of riboflavin, evidence of folate oxidation, and unexplained increases in ergosterol (9.5%). It was concluded that compositional effects of UVB light are limited to changes in vitamin D and show no detrimental changes relative to natural sunlight exposure and, therefore, provide important information relevant to the suitability and safety of UVB light technology for vitamin D enhanced mushrooms.  相似文献   

18.
Formaldehyde is readily quantitated at micrograms/L levels in drinking water. The analyte present in 1 L water samples is derivatized with 2,4-dinitrophenylhydrazine in a 2M acid medium and then extracted with chloroform. After the solvent is exchanged for methanol, the product is separated and quantitated using reverse-phase liquid chromatography with UV detection (365 nm). Reporting limits as low as 20 micrograms/L (corrected for laboratory blank) are routinely achieved. Formaldehyde recovery typically exceeds 90% at 20-200 micrograms/L. The method was applied to hot and cold water samples from thirty-four 1- and 2-story houses equipped with poly(acetal) plumbing elbows and tees. The drinking water samples were accompanied by sets of blanks and spikes specified by a quality assurance/quality control plan. Formaldehyde was observed above the reporting limit in 80% of hot and cold water samples from the 1-story dwellings, but in less than 50% of those from the 2-story dwellings. The results may depend on both the construction of the houses (1- vs 2-story) and the time of year the water is sampled (mid-summer).  相似文献   

19.
Methods and their applications are described for the determination of fluorene in fish, sediment, and plants. Sample extracts are enriched by using 2 or more of the following: gel permeation, silica gel, potassium silicate, sulfuric acid-impregnated silica gel, and activated carbon. Efficiency was improved by applying the adsorbents in combination or as tandem enrichment modules. Analyses by liquid chromatography (LC) with ultraviolet or fluorescence detection (LC/UV or LC/F) yielded limits of detection of 30, 3, and 30 ng/g and average recoveries of 80, 81, and 74% for fish, sediment, and plants, respectively.  相似文献   

20.
A liquid chromatographic (LC) method for the determination of colchicine in pharmaceutical dosage forms and the bulk drug was evaluated in an interlaboratory study which included 13 participating laboratories. The method involves extraction (or dissolution) of the active ingredient with methanol-water (1 + 1), followed by filtration of the extract and reverse phase LC using an octylsilane bonded phase column and UV detection at 254 nm. The mobile phase consists of a methanol-phosphate buffer mixture (pH = 5.5). Three commercial tablet formulations (0.5-0.6 mg colchicine/tablet), 1 synthetic injectable preparation (0.510 mg colchicine/mL), and 1 bulk drug sample were assayed in duplicate by the proposed method. The reproducibility and repeatability standard deviations based on nonpooled results for each sample ranged from 0.0062 mg/mL to 0.0147 mg/tablet and from 0.0037 mg/mL to 0.0127 mg/tablet, respectively; the corresponding coefficients of variation ranged from 1.21 to 2.54% and from 0.73 to 2.19%, respectively. The mean recovery from the synthetic injectable formulation was 100.0%. The method has been adopted official first action.  相似文献   

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