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61.
Determination of trace elements in biological materials using tetramethylammonium hydroxide for sample preparation 总被引:1,自引:0,他引:1
Patrícia Martins Dirce Pozebon Valderi L. Dressler Gisele A. Kemieciki 《Analytica chimica acta》2002,470(2):62-204
A method to prepare milk powder, bovine liver and bovine muscle samples for analysis by electrothermal atomic absorption spectrometry (ETAAS) is proposed. Samples are mixed with a small amount of tetramethylammonium hydroxide (TMAH) and a stable and homogeneous slurry is produced in ca. 2 h with heating at 60–70 °C. After such sample preparation and dilution with water, trace elements are determined in certified reference materials. Pyrolysis and atomisation temperatures are optimised for each element, and several modifiers are investigated. External calibration is used for every analyte. Limits of detection (LODs), precision and accuracy are reported for Cd, Pb, Ni, Cr, Cu and Ag and compared with those obtained after conventional acid digestion. The main advantages of the proposed method are the simplicity of sample preparation and the longer lifetime of the graphite tube. 相似文献
62.
Square-wave voltammetric determination of cefoperazone in a bacterial culture,pharmaceutical drug,milk, and urine 总被引:1,自引:0,他引:1
Use of square-wave voltammetry (SWV) for determination of cefoperazone (CFPZ) in some buffers, bacterial culture, urine, and milk is described. CFPZ provides a specific voltammetric signal which is affected by pH and solution components. Determination of CFPZ in Britton–Robinson buffer, pH 4.4, is sensitive with a low detection limit (about 0.5 nmol L–1). In a more complex medium (bacterial 2YT medium, pH 7.2) the detection limit was approximately 1.5 mol L–1. We provide evidence that SWV is a suitable and quick method for CFPZ determination in a culture of living bacteria without separation of biomass. We have found big differences between methicillin-resistant Staphylococcus aureus (MRSA) and methicillin-sensitive Staphylococcus aureus (MSSA) in cultivation in the presence of CFPZ, depending on time. When CFPZ is cleaved by penicillinase, a new SWV peak b appears at more positive potentials. This peak rises both with increasing concentration of enzyme and with cleavage time while the original CFPZ peak is simultaneously decreasing. We determined the concentration of CFPZ in the drug Pathozone by the standard addition method and achieved good agreement with the declared value of CFPZ in the drug. With a simple pretreatment procedure it is possible to determine CFPZ in milk; for urine no pretreatment was required. Using SWV we could detect CFPZ concentrations as low as 500 nmol L–1 in bovine milk and human urine. 相似文献
63.
Othman A. Farghaly 《Microchemical Journal》2003,75(2):119-131
Tap water samples (Assiut city, lie in the middle north of upper Egypt, approx. 370 km from Cairo, January-March, 2002) were taken from the eight sampling sites of different locations at Assiut city. The samples are analyzed to determine the total content of cadmium, copper, lead and zinc by differential pulse anodic stripping voltammetry (DPASV) while nickel and cobalt are determined by a new simple differential pulse adsorptive stripping voltammetry (DPAdSV), using dimethylglyoxime (DMG) as the complexing agent. This method uses sodium sulfite as the supporting electrolyte, which facilitates the removal of oxygen interference without the traditional necessity of purging with inert gas. The effect of various parameters was studied using DPASV (for Cd, Pb, Cu and Zn) and AdSV (for Ni and Co) methods. Subsequently, under the so found experimental conditions, the stability of calibration curves and the detection limits (μg/l) have been determined. The data achieved (for all metals utility) are comparable to those measured by the graphite furnace atomic absorption spectrophotometric (GF-AAS) method. The effects of the interferences between these metal ions have been investigated. Moreover, the effect of storage was discussed and the obtained results were compared favorably with standard official methods. Statistical analysis of the database exhibits applicability and the accuracy of the techniques. The results obtained from the two techniques (Voltammetry and GF-AAS) are in very good agreements in the most tap water samples. 相似文献
64.
Determination of linuron in soil by stripping voltammetry with a carbon fiber microelectrode 总被引:1,自引:0,他引:1
A carbon fiber microelectrode was used for the electroanalytical determination of Linuron (LIN) in soil extracts. The microelectrode was subjected to an electrochemical pretreatment in order to improve the herbicide adsorption on the electrode surface. With this preconcentration step, detection limits of 80 ng ml−1 and determination limits of 260 ng ml−1 were reached. Optimal conditions with respect to accumulation time and potential, scan rate and pH were established. The LIN was determined in a soil sample with the method proposed and the results found were comparable to those obtained by HPLC. 相似文献
65.
66.
InteractionbetweenMetalinMetalloEnzymeandSmallBiologicalMolecules¥HuJie-Han;ShuZan-Yong;TaoLi-Mei;ChengGuo-Bao(DalianInstitut... 相似文献
67.
68.
水中酚类化合物的液-液-液微萃取/ 高效液相色谱联用分析研究 总被引:3,自引:3,他引:3
建立了液-液-液微萃取/高效液相色谱联用(LLLME/HPLC)测定环境水中痕量酚类化合物2-甲基苯酚、2-硝基苯酚、2,4-二氯苯酚的分析方法,研究了有机相溶剂种类及其体积、料液相pH值与离子强度、接受相的体积、组成及浓度和搅拌速率、萃取时间等因素对分析物萃取效率的影响。实验结果表明,该方法对酚类化合物的富集倍数可达到404~747倍,方法的线性范围为0.2~300μg/L,RSD(n=6)为6.8%~11.4%。测定加标自来水、江水以及生活污水样品的回收率为83%~110%。 相似文献
69.
以芳香基三唑类杀菌剂三唑酮为先导物设计并合成了5个含N,N-二烷基二硫代氨基甲酸酯的芳香三唑类化合物, 通过元素分析、红外光谱、核磁共振氢谱和质谱对其结构进行了表征. 用X射线单晶衍射测定了[α-(4-甲氧基苯甲酰基)-2-(1,2,4-三唑-1-基)]乙基-N,N-二甲基二硫代氨基甲酸酯的晶体结构, 晶体属于三斜晶系, 空间群, 晶胞参数为: a=0.73482(15) nm, b=1.1051(2) nm, c=1.1209(2) nm, α=90.32(3)°, β=101.97(3)°, γ=105.13(3)°, V=0.8578(3) nm3,
Z=2, Dc=1.357 g/cm3, F(000)=368, µ=0.324 mm-1. 生物测试结果显示这5种有机化合物都具有杀菌性和植物生长调节活性 相似文献
70.
Chandra S Gupta LK 《Spectrochimica acta. Part A, Molecular and biomolecular spectroscopy》2005,62(4-5):1089-1094
Nickel(II) complexes, having the general composition Ni(L)2X2, have been synthesized [where L: isopropyl methyl ketone semicarbazone (LLA), isopropyl methyl ketone thiosemicarbazone (LLB), 4-aminoacetophenone semicarbazone (LLC) and 4-aminoacetophenone thiosemicarbazone (LLD) and X=Cl-, 1/2SO(4)2-]. All the Ni(II) complexes reported here have been characterized by elemental analyses, magnetic moments, IR, electronic and mass spectral studies. All the complexes were found to have magnetic moments corresponding to two unpaired electrons. The possible geometries of the complexes were assigned on the basis of electronic and infrared spectral studies. Newly synthesized ligand and its nickel(II) complexes have been screened against different bacterial and fungal growth. 相似文献