Interest in the metabolism and physiological action of vitamin D is increased exponentially. The most important metabolites of vitamin D are 25‐hydroxyvitamin and 1,25‐dihydroxyvitamin D3. The aim of the study was to develop a rapid and simple HPLC method for the measurement of 25‐hydroxyvitamin D3 in human plasma. A method for the measurement of 25‐hydroxyvitamin D3 using HPLC with UV detection and investigation into the extraction techniques with regard to stability and recovery are described. For the separation, RP column LiChroCart 125‐4, Purospher RP‐18e, 5 μm, was used. The mixture of methanol and deionized water (95:5 v/v) was used as mobile phase. The analytical performance of this method is satisfactory: the intra‐ and inter‐assay coefficients of variation were below 10%. Quantitative recoveries from spiked plasma samples were between 92.0–103.2%. The LOD was 10 nmol/L. The preliminary reference range of 25‐hydroxyvitamin D3 in a group of blood donors is 62 ± 26 nmol/L. 相似文献
We investigated the effects of the multilayer polymer‐clay nanohybrid passivation films on the stability of pentacene organic thin‐film transistors (OTFTs) exposed to air and UV irradiation. Well‐ordered multilayer films were deposited by the spin‐assisted layer‐by‐layer assembly method using photocrosslinkable poly(vinyl alcohol) with the N‐methyl‐4(4′‐formylstyryl)pyridinium methosulfate acetal group (SbQ‐PVA) and Na+‐montmorillonite in a water‐based solution process. When photocrosslinked, these SbQ‐PVA/clay multilayers were found to serve as excellent barriers to O2 and UV‐light. Moreover, when used as passivation layers, they enhanced the stability of pentacene OTFT devices exposed to air and UV radiation. 相似文献
Ascorbic acid (AA) is involved in important metabolic processes in the human body. However, its chemical instability requires the assessment of products containing AA. The aim of this study was to develop systems that improve AA stability and to evaluate its release profile, permeation, and skin retention in vitro. For this purpose, we prepared binary systems consisting of propylene glycol and water, microemulsions, liquid crystalline systems, and an emulsion. The AA content in these systems was evaluated over time by measuring the inhibition of 1,1-diphenyl-2-picrylhydrazyl (DPPH). Our results demonstrated that the binary systems and molecular aggregates were less stable and effective than the emulsion. Thus, in vitro AA release, skin permeation, and retention were evaluated using the emulsion. Our results indicate that AA exhibits low release and permeation levels and a high retention rate in the skin, characteristics desirable in cosmetic products. 相似文献
This study describes application of liquid chromatography coupled with triple quadrupole mass spectrometry (LC‐MS) for evaluation of vitamin C stability, the objective being prediction of the degradation products. Detection was performed with an UV detector (UV‐Vis) in sequence with a triple‐quad mass spectrometer in the multiple reaction mode. The negative ion mode of ESI and MS‐MRM transitions of m/z 175→115 (quantifier) and 175→89 (qualifier) for ascorbic acid was used. All the validation parameters were within the range of acceptance proposed by the Food and Drug Administration. The method was fully validated in terms of linearity, LOD, LOQ, accuracy, and interday precision. Validation experiments revealed good linearity with R2 = 0.999 within the established concentration range, and excellent repeatability (9.3%). The LOD of the method was 0.1524 ng/mL whereas the LOQ was 0.4679 ng/mL. LC‐MS methodology proves to be an improved, simple, and fast approach to determining the content of vitamin C and its degradation products with high sensitivity, selectivity, and resolving power within 6 minutes of analysis. 相似文献
A simple and sensitive reversed-phase high performance liquid chromatographic method (HPLC) has been developed and validated for the routine analysis of diltiazem in human plasma and the study of the pharmacokinetics of the drug in the human body. Diltiazem and diazepa (internal standard) were extracted with a mixed organic solution of hexane, chloroform and isopropanol (60:40:5, v/v/v), and then HPLC separation of the drugs was performed on an Spherisorb C(18) column and detected by ultraviolet absorbance at 239 nm. The use of methanol-water solution (containing 2.8 mm triethylamine, 80:20, v/v) as the mobile phase at a fl ow-rate of 1.2 mL/min enables the baseline separation of the drugs free from interferences with isocratic elution. The method was linear in the clinical range 0-300 ng/mL and the lower limit of detection of diltiazem in plasma was 3 ng/mL. The range of percentage of relative standard deviation (%RSD) was from 3.5 to 6.8% for within-day analyses and from 6.2 to 8.4% for between-day analyses, respectively. The extraction recoveries of diltiazem from spiked human plasma (n = 5) at three concentrations were 91.4-104.0%. The method has been used to determine diltiazem in human plasma samples from eight volunteers who had taken diltiazem hydrochloride slow release tables and the data obtained was fitted with a program on computer to study the pharmacokinetics. The results showed that the peak level in plasma approximately averaged 118.5 +/- 14.3 ng/mL at 3.1 +/- 0.4 h, and the areas under the drug concentration curves (AUC) was 793.1 +/- 83.1 ng.h/mL. 相似文献
Finely tuned : A stable dye‐sensitized solar cell that contains a molecularly engineered organic dye has been prepared. The efficiency of the cell remains at 90 % after 1000 h of light soaking at 60 °C. The remarkable stability of the cell is also reflected in the open‐circuit voltage value (Voc), short‐circuit photocurrent‐density value (Jsc), and the fill factor, which also show barely no decline (see picture).
Two novel copolymers based on benzothiadiazole (BT) or difluorobenzothiadizole (ffBT) with 2,2′‐(perfluoro‐1,4‐phenylene)dithiophene (2TPF4), namely PBT‐2TPF4 and PffBT‐2TPF4, are synthesized for applications in polymer solar cells (PSCs). A noticeably high open‐circuit voltage (V oc) of 1.017 and 0.87 V are achieved for PffBT‐2TPF4 and PBT‐2TPF4‐based devices, respectively. Although only a moderate efficiency (5.7%) of PBT‐2TPF4‐based devices is obtained, it is first demonstrated that 2TPF4 is a promising acceptor block for construction of the donor copolymers which possess high V oc, prominent crystallinity, and long‐term stability, simultaneously. Besides, two thienyl flanking the tetrafluorophenylene can decrease torsion angle between conjugated units, resulting in a high coplanar structure of copolymers to enhance their charge carrier mobility. The findings may open a promising and practical way to accelerate the commercialization of PSCs by developing a series of new donor copolymers for efficient and long‐term stable thickness bulk heterojunction PSCs.
This communication describes the determination of an essential amino acid, L ‐methionine (L ‐Met) in the presence of important interferents, ascorbic acid (AA) and uric acid (UA) at physiological pH using a glassy carbon electrode modified with an electropolymerized film of 3‐amino‐5‐mercapto‐1,2,4‐triazole (p‐AMTa). The bare glassy carbon electrode fails to show a voltammetric signal for L ‐Met in the presence of AA and UA at pH 7.2. However, the p‐AMTa electrode separates the voltammetric signals of AA, UA and L ‐Met with pronounced oxidation currents. The amperometric current of L ‐Met was increased linearly from 1.0×10?7 to 1×10?4 M and the detection limit was found to be 4.12×10?10 M (S/N=3). 相似文献
HPLC stability-indicating method was validated for Vitamin C (ascorbic acid) in semisolid pharmaceutical/cosmetic formulations containing glutathione and sodium metabisulfite, as antioxidants. The described procedure included a reliable, precise, accurate and specific method determination employing a 250 mm × 4.6 mm C18 column, 0.2% metaphosphoric acid/methanol/acetonitrile (90:8:2, v/v/v) as the mobile phase and detection at 254 nm. Nicotinic and ascorbic acids were employed as standards, both presenting purity of 99.0%. Linearity was established for the ascorbic acid concentrations ranging form 1.0 to 12 μg mL−1, accuracy/recovery percentage was 95.46-101.54%, precision values were 0.38 (intra-day) and 1.22% (inter-days), and LOD and LOQ were found to be 0.05 and 0.17 μg mL−1, respectively. The working mobile phase elevated the ascorbic acid retention time to ≈3.5 min at a flow rate of 1.0 mL min−1 and provided resolution of the active from the nicotinic acid (internal standard), degradation product (oxalic acid) and other excipients from the pharmaceutical/cosmetic preparations. 相似文献
The voltammetric behaviors of uric acid (UA) and L ‐ascorbic acid (L ‐AA) were studied at well‐aligned carbon nanotube electrode. Compared to glassy carbon, carbon nanotube electrode catalyzes oxidation of UA and L ‐AA, reducing the overpotentials by about 0.028 V and 0.416 V, respectively. Based on its differential catalytic function toward the oxidation of UA and L ‐AA, the carbon nanotube electrode resolved the overlapping voltammetric response of UA and L ‐AA into two well‐defined voltammetric peaks in applying both cyclic voltammetry (CV) and differential pulse voltammetry (DPV), which can be used for a selective determination of UA in the presence of L ‐AA. The peak current obtained from DPV was linearly dependent on the UA concentration in the range of 0.2 μM to 80 μM with a correlation coefficient of 0.997. The detection limit (3δ) for UA was found to be 0.1 μM. Finally, the carbon nanotube electrode was successfully demonstrated as a electrochemical sensor to the determination of UA in human urine samples by simple dilution without further pretreatment. 相似文献
The present work describes oxidation of ascorbic acid (AA) at octacyanomolybdate‐doped‐glutaraldehyde‐cross‐linked poly‐L ‐lysine (PLL‐GA‐Mo(CN) film modified glassy carbon electrode in 0.1 M H2SO4. The modified electrode has been successfully prepared by means of electrostatically trapping Mo(CN) mediator in the cationic film of glutaraldehyde‐cross‐linked poly‐L ‐lysine. The dependence of peak current of modified electrode in pure supporting indicates that the charge transfer in the film was a mixed process at low scan rates (5 to 200 mV s?1), and kinetically restrained at higher scan rates (200 to 1000 mV s?1). Cyclic voltammetry and rotating disk electrode (RDE) techniques are used to investigate the electrocatalytic oxidation of ascorbic acid and compared with its oxidation at bare and undoped PLL‐GA film coated electrodes. The rate constant of catalytic reaction k obtained from RDE analysis was found to be 9.5×105 cm3 mol?1 s?1. The analytical determination of ascorbic acid has been carried out using RDE technique over the physiological interest of ascorbic acid concentrations with a sensitivity of 75 μA mM?1. Amperometric estimation of AA in stirred solution shows a sensitivity of 15 μA mM?1 over the linear concentration range between 50 and 1200 μM. Interestingly, PLL‐GA‐Mo(CN) modified electrode facilitated the oxidation of ascorbic acid but not responded to other electroactive biomolecules such as dopamine, uric acid, NADH, glucose. This unique feature of PLL‐GA‐Mo(CN) modified electrode allowed for the development of a highly selective method for the determination of ascorbic acid in the presence of interferents. 相似文献
The exploitation of multifunctional nanocomposites is highly desired in environmental monitoring,biosensors,and medical diagnosis.In this paper,a simple approach has been proposed to fabricate MoS2 decorated N-doped carbon nanotubes(NCNTs@MoS2)hybrid composites as efficient peroxidase-like mimics.The combination of the MoS2 and N-doped carbon nanotubes(NCNTs)brings about an enhanced synergistic effect,leading to remarkably decent intrinsic peroxidase-mimic activities than that of the single components.Due to the high catalytic efficiency of the resultant NCNTs@MoS2 hybrid nanotubes as peroxidase-like mimics,a co nvenient colorimetric approach for the sensitive determination of H2 O2 and ascorbic acid have been developed with a detection limit of about 0.14μmol/L and 0.12μmol/L,respectively.The work offers a new strategy for the fabrication of peroxidase-like nanomaterials with excellent catalytic activity,which indicates great promising applications in sensitive detections in real samples. 相似文献
Forty synthetic food colors were determined in drinks and candies by reversed-phase high-performance liquid chromatography with photodiode array detection. The following food colors were analyzed within 19 min using a short analytical column (50 mm × 4.6 mm i.d., 1.8 μm) at 50 °C with gradient elution: Ponceau 6R, Tartrazine, Fast yellow AB, Amaranth, Indigotine, Naphthol yellow S, Chrysoine, Ponceau 4R, Sunset yellow FCF, Red 10B, Orange G, Acid violet 7, Brilliant black PN, Allura red AC, Yellow 2G, Red 2G, Uranine, Fast red E, Green S, Ponceau 2R, Azorubine, Orange I, Quinoline yellow, Martius yellow, Ponceau SX, Ponceau 3R, Fast green FCF, Eosine, Brilliant blue FCF, Orange II, Orange RN, Acid blue 1, Erythrosine, Amido black 10B, Acid red 52, Patent blue V, Acid green 9, Phloxine B, Benzyl violet 4B, and Rose bengal. The recoveries of these compounds added to soft drinks and candies at 5 μg/g ranged from 76.6 to 115.0%, and relative standard deviations (R.S.D.s) were within 6.0%. The limits of detection and the limits of quantitation were 0.03 and 0.1 μg/g, respectively. 相似文献
