FLAME ATOMIC ABSORPTION DETERMINATION OF COPPER IN CEREALS FOOD SAMPLES WITH THE PRECONCENTRATION OF POTASSIUM TETRATITANATE WHISKER

A simple and reliable method has been developed for separation and preconcentration of trace amounts of copper ions in cereals food for subsequent measurement by flame atomic absorption spectrometry （FAAS）. The Cu^2＋ ions are adsorbed selectively and quantitatively during the passage. The retained copper ions were desorbed from the potassium tetratitanate whisker with 10.0mL of 2mol/L sulphuric acid solutions as eluent and were determined by FAAS. The linear range was 0.05μg/mL-0.20μg/mL in the original solution with a correlation coefficient of 0.9998. The detection limit of the proposed method is 2. lng/mL in the original solution （3σ, n=9）. Determination of copper in standard ions showed that the proposed method has good accuracy （recovery was more than 95%）. The method was successfully applied for recovery and determination of copper in cereals food samples     

STUDY ON THE DETERMINATION OF TRACE Fe(Ⅲ) BY THIN LAYER RESIN PHASE SPECTROPHOTOMETRY

A method to determine Fe(Ⅲ) by thin layer resin phase spectrophotometry has been developed in this paper. The colored complex formed by Fe(Ⅲ) and 1,2-benzendiol is concentrated on the 717# resin, then Fe(Ⅲ) can be determined directly by making thin layer. The method is sensitive with a apparent molar absorption of 4.8×104L/mol. cm, which is 16 times higher than that of liquid phase spectrophotometry, most coexisting ions do not influence the determination. The detection limit for Fe(Ⅲ) is 1.47μg/L with the precision of 3.3% [n=6, 7μg/50mL Fe(Ⅲ)]. The calibration curve is linear in the range of 0～25μg/50mL. The preposed method was applied to the determination of Fe(Ⅲ) in water sample with satisfactory results.     

Simultaneous determination of cefuroxime axetil and ornidazole in tablet dosage form using reversed-phase high performance liquid chromatography

 A simple, accurate and sensitive reversed-phase high performance liquid chromatographic (RP-HPLC) method for the simultaneous determination of cefuroxime axetil and ornidazole in combined tablet dosage form has been developed. The method was performed with a HiQ-SiL C18 column (250 mm×4.6 mm) and photodiode array (PDA) detector, using 0.01 mol/L potassium dihydrogen orthophosphate-methanol (56∶44, v/v) as the mobile phase and tinidazole as the internal standard. Beer’s law obeys in the concentration ranges of 5-25 μg/mL and 10-50 μg/mL for cefuroxime axetil and ornidazole, respectively. The method has been successfully validated statistically and applied for the analysis of the drugs in pharmaceutical formulation.     

Determination of resveratrol in red wine by solid phase extraction-flow injection chemiluminescence method

A sensitive flow injection chemiluminescence method has been developed for the detection of resveratrol in red wine based on the fact that resveratrol can greatly enhance chemiluminescence reaction between KMnO_4 and HCHO in sulfuric acid medium. Analytes were pre-concentrated on solid sorbents (C_(18) solid-phase extraction cartridges).Under the optimum conditions,the proposed method allows the measurement of resveratrol over the range of 1.32×10~(-8) to 1.32×10~(-5) mol/L with a detection limit of 3.30×10~(-9) mol/L,and the relative standard deviation for 1.32×10~(-5) mol/L resveratrol (n=11) is 3.8%.This method has been successfully applied for the determination of the resveratrol in red wine.Furthermore,the possible reaction mechanism was also discussed.     

Electrochemical Behavior of Mitoxantrone and Its Determination at a Pt／C Implanted Modified Microelectrode

In a 0.02 mol/L Na2HPO4-KH2PO4(PBS) buffer solution(pH=6.82), the electrochemical behavior of mitoxantrone was studied by linear-sweep voltammetry and cyclic voltammetry at a Pt/C ion implantation modified microelectrode. A sensitive reduction peak was observed. The peak potential was -0.72 V(vs.SCE), the peak current was proportional to the concentration of mitoxantrone within the ranges of 7.0×10-8-9.0×10-7 mol/L and 1.0×10-6-2.4×10-5 mol/L, with a detection limit of 4.0×10-8 mol/L. The linear correlation coefficients were 0.9994 and 0.9992, respectively. This method has been applied to the direct determination of mitoxantrone in simulated urine. The recoveries were in the range from 96.2% to 105.9%. The reduction process was a quasi-reversible one with adsorptive characteristics at the Pt/C microelectrode. The electrode reaction rate constant ks and the electron transfer coefficient α of the system were determined to be 4.5 and 0.65 s-1, respectively. The experiments showed that Pt element had surely been implanted into the surface of the carbon fiber, and the atomic Pt improved the electrocatalytic activity. The Pt/C microelectrode had a good stability and reproducibility.     

Trace determination of cobalt ion by using malic acid-malonic acid double substrate oscillating chemical system

A novel kinetic method for determination of trace amounts of cobalt ion was proposed and validated. The method is based on adding malic acid into classical Belousov-Zhabotinskii （B-Z） oscillating chemical system to form a double substrate one. The results showed that when the concentration of cobalt ion was in the range of 5.27× 10^-8 to 5.37 × 10^-12 mol L^-1, the change of the oscillating period was directly proportional to the negative logarithm of cobalt ion concentration. The sensitivity and precision of the developed method were quite satisfactory. The limit of detection was down to 5.20 × 10^-13 mol L^-1 which was a highest sensitivity found for determination of metal ions using oscillating chemical reaction so far. Some factors influencing the determination were also examined. The method has been successfully used to determine cobalt ion in vitamin B12 injection.     

Spectrophotometric Study on the Interaction of Water with Chloranilic Acid and its Analytical Application

The reaction between chloranilic acid and water in alcohol was studied spectrophotometrically. The conditions of reaction were investigated in detail. The stable purple complex with an absorption wavelength at 530 nm was produced from the reaction between chloranilic acid and water. As a method for determination of H2O, Beer‘s law was obeyed in range of 0-6.0 % or 0-8.0 % (V/V) with the detection limit of 0.13 %. The relative standard deviation (RSD) was less than 2 %. The proposed method has been applied to determination of tracea mount of water in ethanol, flour and food flavoring, respectively. The recoveries of water in samples were 97～102%.     

STUDY ON THE DETERMINATION OF TRACE Fe（III） BY THIN LAYER RESIN PHASE SPECTROPHOTOMETRY

A method to determine Fe（Ⅲ） by thin layer resin phase spectrophotometry has been developed in this paper. The colored complex formed by Fe（Ⅲ） and 1,2-benzendiol is concentrated on the 717^# resin, then Fe（Ⅲ） can be determined directly by making thin layer. The method is sensitive with a apparent molar absorption of 4.8×10^4L/mol.cm, which is 16 times higher than that of liquid phase spectrophotornetry, most coexisting ions do not influence the determination. The detection limit for Fe（Ⅲ） is 1.47μg/L with the precision of 3.3% [n=6, 7μg/50mL Fe（Ⅲ）]. The calibration curve is linear in the range of 0-25μg/50mL. The preposed method was applied to the determination of Fe（Ⅲ） in water sample with satisfactory results.     

Preconcentration of chlorophenols in water samples using threedimensional graphene-based magnetic nanocomposite as absorbent

In this paper, a novel magnetic solid-phase extraction method using three-dimensional graphene-based magnetic nanocomposite as adsorbent for the preconcentration of several chlorophenols from water samples prior to high-performance liquid chromatography analysis was developed. Various experimental parameters were investigated. Under the optimum conditions, the enrichment factors of the method were in the range of 186–312, and the limit of detection(S/N = 3) was 0.10 ng/mL. The recoveries of the method were in the range between 85.1% and 101.2%. The developed method has been successfully applied to the determination of chlorophenols in environmental water samples.     

Chromatographic separation of cerium(Ⅲ) in L-valine medium using poly[dibenzo-18-crown-6]

A column chromatographic method has been developed for the separation and determination of cerium(Ⅲ) using poly[dibenzo-18-crown-6]. The separation was carried out in L-valine medium. The adsorption of cerium(Ⅲ) was quantitative from 1×10-1 to 1×10-4 mol/L L-valine. Amongst the various eluents, 1.0-8.0 mol/L hydrochloric acid, 1.0-8.0 mol/L hydrobromic acid, 1.0-8.0 mol/L perchloric acid, 1.0-2.0 mol/L sulfuric acid and 4.0-5.0 mol/L acetic acid, were found to be the efficient eluents for cerium(Ⅲ). The capacity of poly[dibenzo-18-crown-6] for cerium(Ⅲ) was (0.428±0.01) mmol/g. The method was applied to the separation of cerium(Ⅲ) from associated elements link uranium(Ⅵ) and thorium(Ⅳ). It was also applied for the determination of cerium(Ⅲ) in geological samples. The method is simple, rapid and selective with good reproducibility (approximately±2% ).     

Analysis of Vitamin K3 by a Fluorescent Spectroelectrochemistry Method

A simple and sensitive spectroelectrochemistry method for the determination of vitamin K 3 was developed by combining electrolysis and fluoremetry. This method was based on that vitamin K 3 was reduced at a glassy carbon electrode, and its product with characteristic fluorescence at 420 nm was determined with excitation wavelength at 309 nm. Under optimized electrochemical reaction conditions and fluorescent experiment parameters, the fluores-cence intensity was proportional to the concentration of vitamin K 3 in a range from 3.50×10 ?7 to 1.05×10 ?5 mol/L with a correlation coefficient of 0.9991, and detection limit was estimated to be 7.50×10 ?8 mol/L at a signal/noise ra-tio of 3. The relative standard deviation was less than 4.3%(n=5) and the recovery was in a range of 97%―105% for the determination of vitamin K 3 in pharmaceutical preparations. The result is satisfactory for the determination of vi-tamin K 3 as comparison to that from HPLC method.     

方波伏安法测定新型修饰多壁碳纳米管糊电极对肼的电催化氧化(英文)

The application of p-aminophenol as a suitable mediator, as a sensitive and selective voltammetric sensor for the determination of hydrazine using square wave voltammetric method were described. The modified multiwall carbon nanotubes paste electrode exhibited a good electrocatalytic activity for the oxidation of hydrazine at pH = 7.0. The catalytic oxidation peak currents showed a linear dependence of the peaks current to the hydrazine concentrations in the range of 0.5–175 μmol/L with a correlation coefficient of 0.9975. The detection limit (S/N = 3) was estimated to be 0.3 μmol/L of hydrazine. The relative standard deviations for 0.7 and 5.0 μmol/L hydrazine were 1.7 and 1.1%, respectively. The modified electrode showed good sensitivity and selectivity. The diffusion coefficient (D = 9.5 × 10–4 cm2/s) and the kinetic parameters such as the electron transfer coefficient (α = 0.7) of hydrazine at the surface of the modified electrode were determined using electrochemical approaches. The electrode was successfully applied for the determination of hydrazine in real samples with satisfactory results.     

Determination of chloride ion by electrochemiluminescence and investigation of the mechanism

The electrochemiluminescence (ECL) of luminol in aqueous alkaline solution was studied.Trace amounts of chloride showed significant effect on the efficiency of light emission of luminol as a posi-tive trigonometrical wave pulse was exerted on the solution. The detection limit for the chloride is5.0 ×10~(-6) mol/L and the linear calibration range extends up to 1.0 ×10~(-2) mol/L; the relative standarddeviation for 1.0 ×10~(-5) mol / L chloride is 5%. The influencing factors for chloride determination arealso discussed. The possible mechanism for the electrochemiluminescence reaction may be due to theoxidation of chloride ion in the solution to ClO~-, and the latter acts on luminol and then gives outluminescence. The method has been applied to determine the total chloride in tap water with satisfactoryresults.     

Determination of catecholamines by ion chromatography coupled to acidic potassium permanganate chemiluminescence detection

A simple,fast,sensitive,highly selective and eco-friendly analytical method for the determination of catecholamines in human urine by ion chromatography（IC） with chemiluminescence（CL） detection was described in this paper.Using 12 mmol/L H₂SO₄ without any organic additive as eluent,three catecholamines including epinephrine（EP）,norepinephrine（NE） and dopamine（DA） were well separated on a cation-exchange column.The CL detection was based on the reaction of analytes with acidic potassium permanganate in the presence of formaldehyde as an enhancer.The absence of methanol and acetonitrile in eluent made the proposed method more sensitive and eco-friendly.Under the optimal conditions,the linear range of the proposed method was in the range of 0.02-0.5μg/mL.The limit of detection（LOD） was in the range of 0.6 and 5.1μg/L.The relative standard deviations （RSD） for 0.1μg/mL mixed standard solution were in the range of 0.8-1.9%（n = 11）.The method has been applied to the determination of catecholamines in human urine successfully.Excellent spiked recoveries were achieved for catecholamines ranged from 91.2%to 112.7%.     

Homogeneous and nanomolar detection of hydrazine by indigocarmine as a mediator at the surface of TiO2 nanoparticles modified carbon paste electrode

The homogeneous electrocatalytic oxidation of hydrazine（HZ） has been studied by indigocarmine（IND） as a mediator at the surface of TiO₂ nanoparticles modified carbon paste electrode（TNMCPE）.Cyclic voltammetry was used to study the electrochemical behavior of IND at different scan rates.The voltammetric response of the modified electrode was linear against the concentration of HZ in the ranges of 3.0×l0^-8-7.0×10⁶ mol/L with differential pulse voltammetry method.The detection limit（3σ） was determined as 27.3 nmol/L.To evaluate the applicability of the proposed method to real samples,the modified CPE was applied to the determination of HZ in water samples.     

AQUEOUS TWO-PHASE GAS FLOATATION SPECTROPHOTOMETRIC DETERMINATION OF TRACE TETRACYCLINE IN ENVIRONMENTAL WATER SAMPLE

A green method for separating and enriching trace tetracycline （TC） in environment water by Aqueous Two-phase Gas Floatation Spectrophotometry has been proposed, the principium was discussed. In this paper, the hydrophobic complex composed of Mg（II） and TC was floated into organic phase under the optimal conditions： pH=10, the floatation equipment is home-made, n-propyl alcohol as the organic solvent, sodium chloride as the separating phase reagent. The data were obtained by spectrophotometry after floatation; The linear regression equation is A=2.33×10^5C（mol/L）＋0.2179, linear range is from 3.77×10^-7mol/L to 6.32×10^-5 mol/L, respectively, with thecorrelation coefficient （r） better than 0.9997, relative recoveries is 99.7% to 100.3%, limit of detection was 4.29×10^-5mol/L, The method can be applied to analyse the trace TC in water sample, the result is better.     

Iodide analysis by ion chromatography on a new stationary phase of polystyrene-divinylbenzene agglomerated with polymerized-epichlorohydrin-dimethylamine

A new stationary phase for iodide ion analysis has been developed. The cationic polymerepichlorohydrin-dimethylamine(PEPI-DMA) was served as modifier in synthesizing polyelectrolyte sorbents and the macroporous polystyrene-divinylbenzene(PS-DVB) resin was used as support. The positively charged polymer(PEPI-DMA) was electrostatically bonded to a negatively charged particle(PS-DVB sulfonated). The new stationary phase was characterized by scanning electron microscopy(SEM), Fourier transform infrared(FTIR), elemental analysis, chemical adsorption and desorption measurements. The chromatographic evaluation of the new stationary phase was performed using various anions with a conductivity detector. The new stationary phase was also applied to the determination of iodide directly with a DC amperometric detector using a platinum working electrode and an Ag/Ag Cl reference electrode. The chromatographic conditions were optimized and the eluent solution contained 5 mmol/L HNO3 and 15 mmol/L Na NO3 at a flow rate of 1.0 m L/min and column temperature of 30 8C. The applied voltage of the DC amperometric detector was 0.9 V. Under the optimum conditions, the linear range of the method was 0.2–50 mg/L for iodide ion with a correlation coefficient of 0.9990. The detection limit was 0.05 mg/L(calculated at S/N = 3) and the relative standard deviations(RSD, n = 6) were all less than 1% for retention time, peak area and peak height. This method was also utilized for the determination of iodide ions in samples of povidone iodine solution and kelp samples with satisfactory results.     

Determination of Melatonin in Rat Pineal Gland and Drug with Flow-Injection Chemiluminescence

A flow-injection chemiluminescence （CL） method for the determination of melatonin based on the CL reaction of melatonin with hydrogen peroxide and sodium hypochlorite （NaOCl） in a basic alkaline solution was developed. The possible CL mechanism has been discussed, and a proposal for the reaction pathway was given that singlet oxygen was clarified to be produced in this reaction system and was responsible for the CL emission. Under the optimized conditions, the linear concentration range of application was 1.0×10^-7-2.5 × 10^-4 moloL-I with a de- tection limit of 5.0 ×10^-8 moloL-1 （S/N= 3）. The relative standard deviation for eight repeated measurements of 1.0×10^-6 mol·L^-1 melatonin was 2.8%. The interferences of several important biological substances, some indole compound, cations and anions were studied. No interference was found for the anions, glucose, starch, most of cations and low concentration （less than 3.0 × 10^-6 mol·L^-1） of some biological substances and indole compound. The method was applied to the determination of melatonin in rat pineal gland and drug with satisfactory results. The sample throughput was 90 injections per hour.     

A quantitative colorimetric assay of H2O2 and glucose using silver nanoparticles induced by H2O2 and UV

A simple spectrophotometric assay of H2O2 and glucose using Ag nanoparticles has been carried out. Relying on the synergistic effect of H2O2 reduction and ultraviolet （UV） irradiation, Ag nanoparticles with enhanced absorption signals were synthesized. H2O2 served as a reducing agent in the Ag nanoparticles formation in which Ag＋ was reduced to Ago by O2- generated via the decomposition of H2O2 in alkaline media. On the other hand, photoreduction of Ag＋ to Ago under UV irradiations also contributed to the nanoparticles formation. The synthesized nanoparticles were characterized by TEM, XPS, and XRD. The proposed method could determine H2O2 with concentrations ranging from 5.0× 10^-7 to 6.0× 10^-5 tool/ L The detection limit was estimated to be 2.0 × 10^-7 mol/L. Since the conversion of glucose to gluconic acid catalyzed by glucose oxidase was companied with the formation of H2O2, the sensing protocol has been successfully utilized for the determination of glucose in human blood samples. The results were in good agreement with those determined by a local hospital. This colorimetric sensor thus holds great promises in clinical applications.     

阿莫西林与维多利亚蓝B的显色反应及应用

The color reaction of amoxicillin with victoria blue B was studied.A novel visible spectrophotometric method for the determination of amoxicillin has been established.Under pH 8.50～10.5 condition,victoria blue B reacteds with amoxicillin to form red ion association complex.The maximum absorption wavelength was at 630nm and the apparent molar absorptivity(ε) was 2.67×10~4 L·mol~(-1)·cm~(-1) and the linear ranges was 0～5.5 mg·L~(-1).Amoxicillin obey Beer's law in definite concentration range.The optimum reaction conditions and the methodological precision were studied simultaneity.The method was simple and rapid and sensitive for the determination of amoxicillin.This method has been applied to the determination of amoxicillin is in the city sell amoxicillin medicament is in point and average recovery at 98.2%～101.0%.