Food safety problems caused by excessive nitrite addition have been frequently reported and the detection of nitrite in food is particularly important. The standing time during the pretreatment of primary sample has a...Food safety problems caused by excessive nitrite addition have been frequently reported and the detection of nitrite in food is particularly important. The standing time during the pretreatment of primary sample has a great influence on the concentration of nitrite tested by spectrophotometric method. In this context, three kinds of food samples are prepared, including canned mustard, canned fish and home-made pickled water. A series of standing times are placed during the sample pretreatments and the corresponding nitrite contents in these samples are detected by spectrophotometric method based on N-ethylenediamine dihydrochloride. This study aims to find out a reasonable standing time during the pretreatment of food sample, providing influence factor for precise detection of nitrite.展开更多
In this study, the simple DPPH UV-spectrophotometric analytical procedures were optimized and validated for the estimation of antioxidant properties in aerated, semi-aerated and non-aerated tea products as per the AOA...In this study, the simple DPPH UV-spectrophotometric analytical procedures were optimized and validated for the estimation of antioxidant properties in aerated, semi-aerated and non-aerated tea products as per the AOAC guidelines. The method was found to be simple, rapid, accurate and economical in estimating antioxidant properties in the different tea products. A (0.0100 ± 0.0001) g well ground tea sample was extracted directly in 80% v/v methanol in distilled water. The precision of the method had an RSD% of 1.695 with a linear relation equation of Y = 200.7X + 5.25 (r2 = 0.997). The method proved to be a reliable and effective tool in analysis of anti-oxidant properties in varied tea cultivars and their processed products.展开更多
Based upon the standard deviations for the intercept and the slope of a linear regression line, as well as by differentiating both Beer's law and a linear relationship between transmittance and concentration at high ...Based upon the standard deviations for the intercept and the slope of a linear regression line, as well as by differentiating both Beer's law and a linear relationship between transmittance and concentration at high transmission, it is proved that the relative spectrophotometric error of a measurement becomes greater as the sample concentration only decreases. Further, it is demonstrated that the present knowledge with regard to the error in absorption spectrophotometry is necessary to be reexamined. The total scale of transmittance can literally be used for measurements, unfolding workable dynamic ranges about two orders of magnitude lower than usually and thus absorption spectrophotometry can efficiently compete with other methods of analysis with respect to detection limits.展开更多
A new catalytic spectrophotometric method was developed for the determination of trace amount of Se(Ⅳ) in microemulsion medium. The method is based on the catalytic effect of traces of Se(Ⅳ) on the oxidation of ...A new catalytic spectrophotometric method was developed for the determination of trace amount of Se(Ⅳ) in microemulsion medium. The method is based on the catalytic effect of traces of Se(Ⅳ) on the oxidation of 2',4'-dichlorophenylfluomne (p-CPF) by potassium bromate with HNO3 as an activator in the presence of nonionic microemulsion medium. Under optimum conditions, the calibration graph is linear in the range of 0.4-15 μg·L^-1 of Se(Ⅳ) at 480 nm. The detection limit achieved is 9.86 × 10^-10μg·L^-1. Samples were dissolved and the obtained trace Se(Ⅳ) was separated and enriched by sulphydryl dextrane gel (SDG). The method has been applied for determination of trace selenium with satisfactory results.展开更多
A novel method for on-site determination of trace iron was developed using membrane preconcentration and spectrophotometric detection. Fe(II)-ferrozine complex was reacted with cetyltrimethylammonium bromide (CTAB...A novel method for on-site determination of trace iron was developed using membrane preconcentration and spectrophotometric detection. Fe(II)-ferrozine complex was reacted with cetyltrimethylammonium bromide (CTAB) to form a Fe(II)-ferrozine-CTAB paired compound, which was collected on a membrane by filtration under vacuum. The membrane was immersed in 2 mL of ethanol-nitric acid and the absorbance of the solution measured for quantitative analysis. Various factors affecting the iron collection and determination were investigated. With different sample preconcentration volumes, the range of determination was broadened to 0.5-120 ~tg/L. The detection limit of this method reached 0.19 ktg/L and the recoveries were between 97.2 and 109% when the concentration enrichment was about 45. The relative standard deviation (n = 7) was 1.9% for samples containing 10 ~g/L Fe. Twelve seawater samples were analyzed on-site using the proposed method, and two were also analyzed in inductively coupled plasma mass spectrometry. No significant difference was shown between the two methods by the Student's t-test. The method has also been used on-site for iron enrichment experiments with phytoplankton and concluded to be simple, accurate and inexpensive.展开更多
This research studied a new spectrophotometric method for measuring the chemical oxygen demand (COD) of seawater. In this method, the COD was measured using a spectrophotometer instead of titrating with sodium thios...This research studied a new spectrophotometric method for measuring the chemical oxygen demand (COD) of seawater. In this method, the COD was measured using a spectrophotometer instead of titrating with sodium thiosuiphate. The measuring wavelength was selected to be 470 nm, and the COD of three standard glucose solutions (COD = 0.5, 1.5 and 2.5 mgL^-1, respectively) and two seawater samples (from the South Yellow Sea and Jiaozhou Bay) were measured using the spectrophotometric method and titrimetric method respectively. The results showed that the spectrophotometric method was somewhat better than the titrimetric method. The relative standard deviation (RSD) of the spectrophotometric method was less than 2.7%, and the recovery of seawater samples ranged from 96.3% to 103.8%. In addition, the spectrophotometric method has other advantages such as expeditiousness, operation simplicity, analysis automatization, etc. Therefore the spectrophotometric method can be used to measure the COD of seawater with satisfactory results.展开更多
The new catalytic kinetic spectrophotometric method for Au(III) determination was developed and validated. It was based on the catalytic effect of gold on the oxidation of sudan red III by ammonium peroxodisulfate ...The new catalytic kinetic spectrophotometric method for Au(III) determination was developed and validated. It was based on the catalytic effect of gold on the oxidation of sudan red III by ammonium peroxodisulfate ((NH4)2S2O8) with nitrilo triacetic acid as an activator in microemulsion and H2SO4 medium. Under optimum conditions, there was the linearity of the calibration curve in the concentration range from 0 to 20 μg/L Au(Ⅲ) at 520 nm. The relative standard deviation was 3.0% with a correlation coefficient of 0.9986. The detection limit achieved was 9.75 × 10^-5 μg/mL. A new method using a column packed with sulfhydryl dextrose gel (SDG) as a solid-phase extractant has been developed for the preconcentration and separation of Au(Ⅲ) ions. The method has been applied to the determination of trace gold with satisfactory results.展开更多
A new analytical method using Back-Propagation (BP) artificial neural network and kinetic spectrophotometry for simultaneous determination of iron and magnesium in tap water, the Yellow River water and seawater is est...A new analytical method using Back-Propagation (BP) artificial neural network and kinetic spectrophotometry for simultaneous determination of iron and magnesium in tap water, the Yellow River water and seawater is established. By conditional experiments, the optimum analytical conditions and parameters are obtained. Levenberg-Marquart (L-M) algorithm is used for calculation in BP neural network. The topological structure of three-layer BP ANN network architecture is chosen as 15-16-2 (nodes). The initial value of gradient coefficient μ is fixed at 0.001 and the increase factor and reduction factor of μ take the default values of the system. The data are processed by computers with our own programs written in MATLAB 7.0. The relative standard deviation of the calculated results for iron and manganese is 2.30% and 2.67% respectively. The results of standard addition method show that for the tap water, the recoveries of iron and manganese are in the ranges of 98.0%-104.3% and 96.5%-104.5%, and the RSD is in the range of 0.23%-0.98%; for the Yellow River water (Lijin district of Shandong Province), the recoveries of iron and manganese are in the ranges of 96.0%-101.0% and 98.7%-104.2%, and the RSD is in the range of 0.13%-2.52%; for the seawater in Qingdao offshore, the recoveries of iron and manganese are in the ranges of 95.3%-104.8% and 95.3%-104.7%, and the RSD is in the range of 0.14%-2.66%. It is found that 21 common cations and anions do not interfere with the determination of iron and manganese under the optimum experimental conditions. This method exhibits good reproducibility and high accuracy in the determination of iron and manganese and can be used for the simultaneous determination of iron and manganese in tap water and natural water. By using the established ANN- catalytic spectrophotometric method, the iron and manganese concentrations of the surface seawater at 11 sites in Qingdao offshore are determined and the level distribution maps of iron and manganese are drawn.展开更多
New simple and sensitive spectrophotometric determination of fluoride in drinking groundwater has been developed using aluminium-resorcin blue complex. The method is based on the reaction of fluoride with the coloured...New simple and sensitive spectrophotometric determination of fluoride in drinking groundwater has been developed using aluminium-resorcin blue complex. The method is based on the reaction of fluoride with the coloured complex to produce colourless aluminium fluoride complex and releasing of the free ligand. The relationship of the reaction of flu-oride with the complex is sixth-order polynomial function. The reaction reaches equilibrium at fluoride concentration of 0.054 mM. The equilibrium constant (Keq) was calculated as 1.12 × 1014. Beer-Lambert law is obeyed in the range 0.0 - 0.024 mM of fluoride (0.0 - 1.0 mg·L-1). The molar absorptivity at 502 nm is 6.45 × 103 L·mol-1·cm-1. Fluoride concentration higher than 1.0 mg·L-1 can be measured after proper dilution. The sensitivity, detection limit, quantitation limit, and the percentage recovery of 0.75 mg·L-1 fluoride for the method were found to be 0.357 μg·ml-1., 0.07 mg·L-1, 0.2 mg·L-1, and 101.1 respectively.展开更多
By the use of CPB, Cd(Ⅲ) forms a highly sensitive complex with 5-Br-PADAP in aqueous solution, molar absorptivity εis 1. 21 ×105 1. mol-1. cm-1.Trace amount of sulphide can be determined from its effect on the...By the use of CPB, Cd(Ⅲ) forms a highly sensitive complex with 5-Br-PADAP in aqueous solution, molar absorptivity εis 1. 21 ×105 1. mol-1. cm-1.Trace amount of sulphide can be determined from its effect on the complex of Cd (Ⅲ)-5-Br-PADAP-CPB, sulphide in the range 0~3. 2 ×10-6mol dm-3 causes a decrease in absorption, that is a linear function of the concentration, For 13ng cm-3 sulphide, common metal ions such as Na+, K+, Ca2+, Mg2+, Al3+ and anions such as CO (24μg cm-3). S2O (22μg cm-3). PO (20μg cm-3) etc. do not interfere. A method for the indirect determination of sulphide in beer and in dustrial waste water with good selectivity and accuracy is described.展开更多
A highly simple, rapid, sensitive and selective method is developed for spectrophotometric determination of gabapentin in pure form as well as in pharmaceutical formulations. The method is based on the formation of a ...A highly simple, rapid, sensitive and selective method is developed for spectrophotometric determination of gabapentin in pure form as well as in pharmaceutical formulations. The method is based on the formation of a yellow Schiff base derived from the condensation of gabapentin drug (1-amino methyl) cyclo hexane acetic acid and 2,5-dihydroxybenzaldehyde (DHBA) exhibiting a maximum absorbance at 445 nm. The composition, molar absorptivity and effect of different excipient have been determined spectrophotometrically. Under optimized experimental conditions, Beer’s law is obeyed in the concentration range 2.57 - 37.25 μg/ml. The method is validated with respect to accuracy, precision, limit of detection and limit of quantification. The Sandell sensitivity, correlation coefficient and regression equation are calculated. The equilibrium constant and free energy change using Benesi-Hildebrand plot are also determined. The Schiff base derived from condensation of gabapentin with DHBA is also synthesized and characterized. The condensation reaction mechanism has been proposed.展开更多
In the framework of fighting against the poor quality medicines sold in developing countries using classical analytical methods easily accessible in those countries, four UV-Visible spectrophotometric methods for one ...In the framework of fighting against the poor quality medicines sold in developing countries using classical analytical methods easily accessible in those countries, four UV-Visible spectrophotometric methods for one antimalarial (quinine) and two antibiotics (amoxicillin and metronidazole) have been developed and validated according to the total error strategy using the accuracy profiles as a decision tool. The dosing range was 2 - 10 μg/mL (for quinine sulfate in tablet), 4 - 12 μg/mL (for quinine bichlorhydrate in oral drop-metronidazole benzaote in oral suspension) and 15 - 35 μg/mL (for amoxicillin trihydrate in capsule). The validated methods were then applied in determining the content of some analogous medicines sold in the Democratic Republic of Congo. Thus, the proposed UV-Visible spectrophotometric methods are simple and suitable to quantify quinine, amoxicillin and metronidazole in different pharmaceutical forms.展开更多
A new simple spectrophotometric method was developed for the determination of binary mixtures without prior separation.The method is based on the generation of ratio spectra of compound X by using a standard spectrum ...A new simple spectrophotometric method was developed for the determination of binary mixtures without prior separation.The method is based on the generation of ratio spectra of compound X by using a standard spectrum of compound Y as a divisor.The peak to trough amplitudes between two selected wavelengths in the ratio spectra are proportional to concentration of X without interference from Y.The method was demonstrated by determination of two drug combinations.The first consists of the two antihyperlipidemics:atorvastatin calcium(ATV) and ezetimibe(EZE),and the second comprises the antihypertensives:candesartan cilexetil(CAN) and hydrochlorothiazide(HCT).For mixture 1,ATV was determined using 10 μg/mL EZE as the divisor to generate the ratio spectra,and the peak to trough amplitudes between 231 and 276 nm were plotted against ATV concentration.Similarly,by using 10 μg/mL ATV as divisor,the peak to trough amplitudes between 231 and 276 nm were found proportional to EZE concentration.Calibration curves were linear in the range 2.5-40 mg/mL for both drugs.For mixture 2,divisor concentration was 7.5 μg/mL for both drugs.CAN was determined using its peak to trough amplitudes at 251 and 277 nm,while HCT was estimated using the amplitudes between 251 and 276 nm.The measured amplitudes were linearly correlated to concentration in the ranges 2.5-50 and 1-30 μg/mL for CAN and HCT,respectively.The proposed spectrophotometric method was validated and successfully applied for the assay of both drug combinations in several laboratory-prepared mixtures and commercial tablets.展开更多
Solid liquid extraction of copper ion (I) with 2, 9-dimethyl-1, 10-phenanthroline (neo-cuproine, DMP) into molten naphthalene followed by chloroform spectrophotometric determination has been studied experimentally. Th...Solid liquid extraction of copper ion (I) with 2, 9-dimethyl-1, 10-phenanthroline (neo-cuproine, DMP) into molten naphthalene followed by chloroform spectrophotometric determination has been studied experimentally. The ternary complex Cu(I)-DMP-ClO4 was extracted quantitatively into molten naphthalene in the range of pH from 5 to 6 at 85 C-. Absorbance was spectrophotometrically determined at 459 nm against the reagent blank after the solid naphthalene layer was anhydrously dissolved in chloroform. Beer's law is obeyed over a concentration range of 0.5-70 mug/mL. The molar absorptivity and Sandell's sensitivity are 1.0x10(4) L/(mol(.)cm) and 0.0099 mug(.)cm(2) respectively. In addition, the various conditions on determination and the interference of coexisted ions were discussed, and the method was applied to the determination of copper ion both in tea samples and cadmium sulfate reagents. The results are in good agreement with those obtained by ICP AES method.展开更多
A novel,safe,economic and sensitive method of spectrophotometric estimation has been developed using Azeoptropic mixture (water∶methanol:60∶40,v/v) for the quantitative determination of Lornoxicam,a practically wate...A novel,safe,economic and sensitive method of spectrophotometric estimation has been developed using Azeoptropic mixture (water∶methanol:60∶40,v/v) for the quantitative determination of Lornoxicam,a practically water-insoluble drug.Hence,Lornoxicam stock solution was prepared in Azeoptropic mixture.Lornoxicam showed maximum absorbance at 383 nm.Beer's law was obeyed in the concentration range 4-24 μg/mL with regression coefficient of 0.999.The method was validated in terms of linearity (R2=0.999),precision (CV for intra-day and inter-day was 0.28 0.68 and 0.12-0.92,respectively),accuracy (98.03-100.59% w/w) and specificity.This method is simple,precise,accurate,sensitive and reproducible and can be used for the routine quality control testing of the marketed formulations.展开更多
This work reports the spectrophotometric simultaneous determination of zinc(Ⅱ), manganese(Ⅱ) and iron(Ⅱ) in pharmaceutical preparation, using orthogonal signal correctionpartial least squares (OSC-PLS). All...This work reports the spectrophotometric simultaneous determination of zinc(Ⅱ), manganese(Ⅱ) and iron(Ⅱ) in pharmaceutical preparation, using orthogonal signal correctionpartial least squares (OSC-PLS). All the factors affecting on the sensitivity were optimized and the linear dynamic range for determination of these metals was found. The PLS modeling was used for the multivariate calibration of the spectrophotometric data. The OSC was used for preprocessing of data matrices and the prediction results of model. The experimental calibration matrix was designed by measuring the absorbance over the range 450-570 nm for 21 samples of 0.05-1.05, 0.10-1.10 and 0.05-1.05μg·mL^-1 of zinc(Ⅱ), manganese(Ⅱ) and iron(Ⅱ), respectively. The RMSEP for zinc(Ⅱ), manganese(Ⅱ) and iron(Ⅱ) using OSC-PLS were 0.0164, 0.0132, 0.0146, respectively. The proposed method was successfully applied the determination of zinc(Ⅱ), manganese(Ⅱ) and iron(Ⅱ) in pharmaceutical preparations.展开更多
The method for the sepration and determination of trace Cr(VI) exiting in mass Cr(III) has been researched. The method is highly sensitive and less interference, but is simple and useful for analysis trace Cr(VI).
A new method for the determination of cerium subgroup rare earths was studied and reported ill this paper. It was found that cerium subgroup rare earth elements react with DBMCSA in 0.6 mol/L hydrochloric acid medium ...A new method for the determination of cerium subgroup rare earths was studied and reported ill this paper. It was found that cerium subgroup rare earth elements react with DBMCSA in 0.6 mol/L hydrochloric acid medium to form stable blue complexes. The absorbances of equal amounts of cerium subgroup rare earths are close to each other at their maximum adsorptive wavelength (641 nm). Beer's law is obeyed for 0-20 mu g of I ars earths in 25 mi of solution. The method has been applied to the determination of the total amount of cerium subgroup rare earths in steel and cast iron samples with satisfactory results.展开更多
Aluminium has been determined by β-correction spectrophotometer with phenylfluorone (PF)and a non-ionic surfactant, emulsifying OP in PH 8 ammoniacal buffer solution. β-correction spectrophotometric method can elimi...Aluminium has been determined by β-correction spectrophotometer with phenylfluorone (PF)and a non-ionic surfactant, emulsifying OP in PH 8 ammoniacal buffer solution. β-correction spectrophotometric method can eliminate completely the effect of excess PF to increase the analytical sensitivity and decrease error. The results have Shown that Beer's law was obeyed over the concentration range 0-15μg Al (Ⅲ)/25ml and the relative standard deviation was less than 3.3%.展开更多
At present, there is no method for identifying meat frozen in a thermal state acceptable for production control. The role of free nucleotides in the processes of refrigeration and storage of meat, affecting the struct...At present, there is no method for identifying meat frozen in a thermal state acceptable for production control. The role of free nucleotides in the processes of refrigeration and storage of meat, affecting the structural and mechanical properties of muscle tissue, the formation of taste and its biological value is known. In this article we compared methods for identifying the thermal state of meat based on the determination of the composition and content of free nucleotides by high-performance liquid chromatography (HPLC) and spectrophotometry [SF]. High-purity reference substances were used: free nucleotides—ATP, ADP, AMP, IMP and nucleosides-inosine and hypoxanthine. It has been experimentally established that the characteristic peaks of the absorption spectra for extracts of free nucleotides of meat frozen depended from thermal state of meat. The content of ATP is 21.8 times higher in meat frozen in a fresh state, and the amount of IMF is 12.3 times lower than in meat frozen after cooling. The results of studies of meat frozen using the HPLC method and the developed SF method show the adequacy of the data obtained by both methods. SF-method based on the determination of the optical density of the extracts of free nucleotides is recommended to justify the choice of technological process meat defrost modes.展开更多
文摘Food safety problems caused by excessive nitrite addition have been frequently reported and the detection of nitrite in food is particularly important. The standing time during the pretreatment of primary sample has a great influence on the concentration of nitrite tested by spectrophotometric method. In this context, three kinds of food samples are prepared, including canned mustard, canned fish and home-made pickled water. A series of standing times are placed during the sample pretreatments and the corresponding nitrite contents in these samples are detected by spectrophotometric method based on N-ethylenediamine dihydrochloride. This study aims to find out a reasonable standing time during the pretreatment of food sample, providing influence factor for precise detection of nitrite.
文摘In this study, the simple DPPH UV-spectrophotometric analytical procedures were optimized and validated for the estimation of antioxidant properties in aerated, semi-aerated and non-aerated tea products as per the AOAC guidelines. The method was found to be simple, rapid, accurate and economical in estimating antioxidant properties in the different tea products. A (0.0100 ± 0.0001) g well ground tea sample was extracted directly in 80% v/v methanol in distilled water. The precision of the method had an RSD% of 1.695 with a linear relation equation of Y = 200.7X + 5.25 (r2 = 0.997). The method proved to be a reliable and effective tool in analysis of anti-oxidant properties in varied tea cultivars and their processed products.
文摘Based upon the standard deviations for the intercept and the slope of a linear regression line, as well as by differentiating both Beer's law and a linear relationship between transmittance and concentration at high transmission, it is proved that the relative spectrophotometric error of a measurement becomes greater as the sample concentration only decreases. Further, it is demonstrated that the present knowledge with regard to the error in absorption spectrophotometry is necessary to be reexamined. The total scale of transmittance can literally be used for measurements, unfolding workable dynamic ranges about two orders of magnitude lower than usually and thus absorption spectrophotometry can efficiently compete with other methods of analysis with respect to detection limits.
文摘A new catalytic spectrophotometric method was developed for the determination of trace amount of Se(Ⅳ) in microemulsion medium. The method is based on the catalytic effect of traces of Se(Ⅳ) on the oxidation of 2',4'-dichlorophenylfluomne (p-CPF) by potassium bromate with HNO3 as an activator in the presence of nonionic microemulsion medium. Under optimum conditions, the calibration graph is linear in the range of 0.4-15 μg·L^-1 of Se(Ⅳ) at 480 nm. The detection limit achieved is 9.86 × 10^-10μg·L^-1. Samples were dissolved and the obtained trace Se(Ⅳ) was separated and enriched by sulphydryl dextrane gel (SDG). The method has been applied for determination of trace selenium with satisfactory results.
基金Supported by State Key Laboratory of Marine Environmental Science(MEL)Funds(No.MELRI1001)
文摘A novel method for on-site determination of trace iron was developed using membrane preconcentration and spectrophotometric detection. Fe(II)-ferrozine complex was reacted with cetyltrimethylammonium bromide (CTAB) to form a Fe(II)-ferrozine-CTAB paired compound, which was collected on a membrane by filtration under vacuum. The membrane was immersed in 2 mL of ethanol-nitric acid and the absorbance of the solution measured for quantitative analysis. Various factors affecting the iron collection and determination were investigated. With different sample preconcentration volumes, the range of determination was broadened to 0.5-120 ~tg/L. The detection limit of this method reached 0.19 ktg/L and the recoveries were between 97.2 and 109% when the concentration enrichment was about 45. The relative standard deviation (n = 7) was 1.9% for samples containing 10 ~g/L Fe. Twelve seawater samples were analyzed on-site using the proposed method, and two were also analyzed in inductively coupled plasma mass spectrometry. No significant difference was shown between the two methods by the Student's t-test. The method has also been used on-site for iron enrichment experiments with phytoplankton and concluded to be simple, accurate and inexpensive.
文摘This research studied a new spectrophotometric method for measuring the chemical oxygen demand (COD) of seawater. In this method, the COD was measured using a spectrophotometer instead of titrating with sodium thiosuiphate. The measuring wavelength was selected to be 470 nm, and the COD of three standard glucose solutions (COD = 0.5, 1.5 and 2.5 mgL^-1, respectively) and two seawater samples (from the South Yellow Sea and Jiaozhou Bay) were measured using the spectrophotometric method and titrimetric method respectively. The results showed that the spectrophotometric method was somewhat better than the titrimetric method. The relative standard deviation (RSD) of the spectrophotometric method was less than 2.7%, and the recovery of seawater samples ranged from 96.3% to 103.8%. In addition, the spectrophotometric method has other advantages such as expeditiousness, operation simplicity, analysis automatization, etc. Therefore the spectrophotometric method can be used to measure the COD of seawater with satisfactory results.
文摘The new catalytic kinetic spectrophotometric method for Au(III) determination was developed and validated. It was based on the catalytic effect of gold on the oxidation of sudan red III by ammonium peroxodisulfate ((NH4)2S2O8) with nitrilo triacetic acid as an activator in microemulsion and H2SO4 medium. Under optimum conditions, there was the linearity of the calibration curve in the concentration range from 0 to 20 μg/L Au(Ⅲ) at 520 nm. The relative standard deviation was 3.0% with a correlation coefficient of 0.9986. The detection limit achieved was 9.75 × 10^-5 μg/mL. A new method using a column packed with sulfhydryl dextrose gel (SDG) as a solid-phase extractant has been developed for the preconcentration and separation of Au(Ⅲ) ions. The method has been applied to the determination of trace gold with satisfactory results.
文摘A new analytical method using Back-Propagation (BP) artificial neural network and kinetic spectrophotometry for simultaneous determination of iron and magnesium in tap water, the Yellow River water and seawater is established. By conditional experiments, the optimum analytical conditions and parameters are obtained. Levenberg-Marquart (L-M) algorithm is used for calculation in BP neural network. The topological structure of three-layer BP ANN network architecture is chosen as 15-16-2 (nodes). The initial value of gradient coefficient μ is fixed at 0.001 and the increase factor and reduction factor of μ take the default values of the system. The data are processed by computers with our own programs written in MATLAB 7.0. The relative standard deviation of the calculated results for iron and manganese is 2.30% and 2.67% respectively. The results of standard addition method show that for the tap water, the recoveries of iron and manganese are in the ranges of 98.0%-104.3% and 96.5%-104.5%, and the RSD is in the range of 0.23%-0.98%; for the Yellow River water (Lijin district of Shandong Province), the recoveries of iron and manganese are in the ranges of 96.0%-101.0% and 98.7%-104.2%, and the RSD is in the range of 0.13%-2.52%; for the seawater in Qingdao offshore, the recoveries of iron and manganese are in the ranges of 95.3%-104.8% and 95.3%-104.7%, and the RSD is in the range of 0.14%-2.66%. It is found that 21 common cations and anions do not interfere with the determination of iron and manganese under the optimum experimental conditions. This method exhibits good reproducibility and high accuracy in the determination of iron and manganese and can be used for the simultaneous determination of iron and manganese in tap water and natural water. By using the established ANN- catalytic spectrophotometric method, the iron and manganese concentrations of the surface seawater at 11 sites in Qingdao offshore are determined and the level distribution maps of iron and manganese are drawn.
文摘New simple and sensitive spectrophotometric determination of fluoride in drinking groundwater has been developed using aluminium-resorcin blue complex. The method is based on the reaction of fluoride with the coloured complex to produce colourless aluminium fluoride complex and releasing of the free ligand. The relationship of the reaction of flu-oride with the complex is sixth-order polynomial function. The reaction reaches equilibrium at fluoride concentration of 0.054 mM. The equilibrium constant (Keq) was calculated as 1.12 × 1014. Beer-Lambert law is obeyed in the range 0.0 - 0.024 mM of fluoride (0.0 - 1.0 mg·L-1). The molar absorptivity at 502 nm is 6.45 × 103 L·mol-1·cm-1. Fluoride concentration higher than 1.0 mg·L-1 can be measured after proper dilution. The sensitivity, detection limit, quantitation limit, and the percentage recovery of 0.75 mg·L-1 fluoride for the method were found to be 0.357 μg·ml-1., 0.07 mg·L-1, 0.2 mg·L-1, and 101.1 respectively.
文摘By the use of CPB, Cd(Ⅲ) forms a highly sensitive complex with 5-Br-PADAP in aqueous solution, molar absorptivity εis 1. 21 ×105 1. mol-1. cm-1.Trace amount of sulphide can be determined from its effect on the complex of Cd (Ⅲ)-5-Br-PADAP-CPB, sulphide in the range 0~3. 2 ×10-6mol dm-3 causes a decrease in absorption, that is a linear function of the concentration, For 13ng cm-3 sulphide, common metal ions such as Na+, K+, Ca2+, Mg2+, Al3+ and anions such as CO (24μg cm-3). S2O (22μg cm-3). PO (20μg cm-3) etc. do not interfere. A method for the indirect determination of sulphide in beer and in dustrial waste water with good selectivity and accuracy is described.
文摘A highly simple, rapid, sensitive and selective method is developed for spectrophotometric determination of gabapentin in pure form as well as in pharmaceutical formulations. The method is based on the formation of a yellow Schiff base derived from the condensation of gabapentin drug (1-amino methyl) cyclo hexane acetic acid and 2,5-dihydroxybenzaldehyde (DHBA) exhibiting a maximum absorbance at 445 nm. The composition, molar absorptivity and effect of different excipient have been determined spectrophotometrically. Under optimized experimental conditions, Beer’s law is obeyed in the concentration range 2.57 - 37.25 μg/ml. The method is validated with respect to accuracy, precision, limit of detection and limit of quantification. The Sandell sensitivity, correlation coefficient and regression equation are calculated. The equilibrium constant and free energy change using Benesi-Hildebrand plot are also determined. The Schiff base derived from condensation of gabapentin with DHBA is also synthesized and characterized. The condensation reaction mechanism has been proposed.
文摘In the framework of fighting against the poor quality medicines sold in developing countries using classical analytical methods easily accessible in those countries, four UV-Visible spectrophotometric methods for one antimalarial (quinine) and two antibiotics (amoxicillin and metronidazole) have been developed and validated according to the total error strategy using the accuracy profiles as a decision tool. The dosing range was 2 - 10 μg/mL (for quinine sulfate in tablet), 4 - 12 μg/mL (for quinine bichlorhydrate in oral drop-metronidazole benzaote in oral suspension) and 15 - 35 μg/mL (for amoxicillin trihydrate in capsule). The validated methods were then applied in determining the content of some analogous medicines sold in the Democratic Republic of Congo. Thus, the proposed UV-Visible spectrophotometric methods are simple and suitable to quantify quinine, amoxicillin and metronidazole in different pharmaceutical forms.
文摘A new simple spectrophotometric method was developed for the determination of binary mixtures without prior separation.The method is based on the generation of ratio spectra of compound X by using a standard spectrum of compound Y as a divisor.The peak to trough amplitudes between two selected wavelengths in the ratio spectra are proportional to concentration of X without interference from Y.The method was demonstrated by determination of two drug combinations.The first consists of the two antihyperlipidemics:atorvastatin calcium(ATV) and ezetimibe(EZE),and the second comprises the antihypertensives:candesartan cilexetil(CAN) and hydrochlorothiazide(HCT).For mixture 1,ATV was determined using 10 μg/mL EZE as the divisor to generate the ratio spectra,and the peak to trough amplitudes between 231 and 276 nm were plotted against ATV concentration.Similarly,by using 10 μg/mL ATV as divisor,the peak to trough amplitudes between 231 and 276 nm were found proportional to EZE concentration.Calibration curves were linear in the range 2.5-40 mg/mL for both drugs.For mixture 2,divisor concentration was 7.5 μg/mL for both drugs.CAN was determined using its peak to trough amplitudes at 251 and 277 nm,while HCT was estimated using the amplitudes between 251 and 276 nm.The measured amplitudes were linearly correlated to concentration in the ranges 2.5-50 and 1-30 μg/mL for CAN and HCT,respectively.The proposed spectrophotometric method was validated and successfully applied for the assay of both drug combinations in several laboratory-prepared mixtures and commercial tablets.
基金This research was financially supported by the project KJCXGC-01 of Northwest Normal University, China.
文摘Solid liquid extraction of copper ion (I) with 2, 9-dimethyl-1, 10-phenanthroline (neo-cuproine, DMP) into molten naphthalene followed by chloroform spectrophotometric determination has been studied experimentally. The ternary complex Cu(I)-DMP-ClO4 was extracted quantitatively into molten naphthalene in the range of pH from 5 to 6 at 85 C-. Absorbance was spectrophotometrically determined at 459 nm against the reagent blank after the solid naphthalene layer was anhydrously dissolved in chloroform. Beer's law is obeyed over a concentration range of 0.5-70 mug/mL. The molar absorptivity and Sandell's sensitivity are 1.0x10(4) L/(mol(.)cm) and 0.0099 mug(.)cm(2) respectively. In addition, the various conditions on determination and the interference of coexisted ions were discussed, and the method was applied to the determination of copper ion both in tea samples and cadmium sulfate reagents. The results are in good agreement with those obtained by ICP AES method.
文摘A novel,safe,economic and sensitive method of spectrophotometric estimation has been developed using Azeoptropic mixture (water∶methanol:60∶40,v/v) for the quantitative determination of Lornoxicam,a practically water-insoluble drug.Hence,Lornoxicam stock solution was prepared in Azeoptropic mixture.Lornoxicam showed maximum absorbance at 383 nm.Beer's law was obeyed in the concentration range 4-24 μg/mL with regression coefficient of 0.999.The method was validated in terms of linearity (R2=0.999),precision (CV for intra-day and inter-day was 0.28 0.68 and 0.12-0.92,respectively),accuracy (98.03-100.59% w/w) and specificity.This method is simple,precise,accurate,sensitive and reproducible and can be used for the routine quality control testing of the marketed formulations.
文摘This work reports the spectrophotometric simultaneous determination of zinc(Ⅱ), manganese(Ⅱ) and iron(Ⅱ) in pharmaceutical preparation, using orthogonal signal correctionpartial least squares (OSC-PLS). All the factors affecting on the sensitivity were optimized and the linear dynamic range for determination of these metals was found. The PLS modeling was used for the multivariate calibration of the spectrophotometric data. The OSC was used for preprocessing of data matrices and the prediction results of model. The experimental calibration matrix was designed by measuring the absorbance over the range 450-570 nm for 21 samples of 0.05-1.05, 0.10-1.10 and 0.05-1.05μg·mL^-1 of zinc(Ⅱ), manganese(Ⅱ) and iron(Ⅱ), respectively. The RMSEP for zinc(Ⅱ), manganese(Ⅱ) and iron(Ⅱ) using OSC-PLS were 0.0164, 0.0132, 0.0146, respectively. The proposed method was successfully applied the determination of zinc(Ⅱ), manganese(Ⅱ) and iron(Ⅱ) in pharmaceutical preparations.
文摘The method for the sepration and determination of trace Cr(VI) exiting in mass Cr(III) has been researched. The method is highly sensitive and less interference, but is simple and useful for analysis trace Cr(VI).
文摘A new method for the determination of cerium subgroup rare earths was studied and reported ill this paper. It was found that cerium subgroup rare earth elements react with DBMCSA in 0.6 mol/L hydrochloric acid medium to form stable blue complexes. The absorbances of equal amounts of cerium subgroup rare earths are close to each other at their maximum adsorptive wavelength (641 nm). Beer's law is obeyed for 0-20 mu g of I ars earths in 25 mi of solution. The method has been applied to the determination of the total amount of cerium subgroup rare earths in steel and cast iron samples with satisfactory results.
文摘Aluminium has been determined by β-correction spectrophotometer with phenylfluorone (PF)and a non-ionic surfactant, emulsifying OP in PH 8 ammoniacal buffer solution. β-correction spectrophotometric method can eliminate completely the effect of excess PF to increase the analytical sensitivity and decrease error. The results have Shown that Beer's law was obeyed over the concentration range 0-15μg Al (Ⅲ)/25ml and the relative standard deviation was less than 3.3%.
文摘At present, there is no method for identifying meat frozen in a thermal state acceptable for production control. The role of free nucleotides in the processes of refrigeration and storage of meat, affecting the structural and mechanical properties of muscle tissue, the formation of taste and its biological value is known. In this article we compared methods for identifying the thermal state of meat based on the determination of the composition and content of free nucleotides by high-performance liquid chromatography (HPLC) and spectrophotometry [SF]. High-purity reference substances were used: free nucleotides—ATP, ADP, AMP, IMP and nucleosides-inosine and hypoxanthine. It has been experimentally established that the characteristic peaks of the absorption spectra for extracts of free nucleotides of meat frozen depended from thermal state of meat. The content of ATP is 21.8 times higher in meat frozen in a fresh state, and the amount of IMF is 12.3 times lower than in meat frozen after cooling. The results of studies of meat frozen using the HPLC method and the developed SF method show the adequacy of the data obtained by both methods. SF-method based on the determination of the optical density of the extracts of free nucleotides is recommended to justify the choice of technological process meat defrost modes.