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1.
It is the first time that boron is determined in the presence of a little methanol by discoloring spectrophotometry in this paper. A russety product can be formed by the reaction between glycine (Gly) and sodium 1,2-naphthoquinone-4-sulfonate (NQS) in alkaline solution. When boron is added to the solution, the system will be discolored, and the addition of a little methanol will improve the discoloration. Beer's law is obeyed in the range of boron concentrations of 0.86-43.24 μg ml−1 at the maximal discoloring wavelength of 382 nm. The equation of linear regression is A = −0.07581-86.79186C (mol l−1), with a linearly correlation coefficient of 0.9979. The detection limit is 0.80 μg ml−1 and R.S.D. is 4.2%. The method is successfully applied to the determination of boron in pharmaceutical and biological samples. The average recoveries are in the range of 98.2-104.1%. Analytical results obtained with this novel method are satisfactory. 相似文献
2.
José A. Murillo Pulgarín Luisa F. García Bermejo Pablo Fernández López 《Analytica chimica acta》2005,546(1):60-67
The chemiluminescent behaviour of captopril when reacted with a common oxidant, potassium permanganate in different acidic media is described, using the stopped-flow technique in a continuous-flow system. A 22 bit analogue-to-digital converter that acquires analogue signals at −10 and +10 V and allows the power supply to the peristaltic pump to be interrupted is used in the time-resolved chemiluminescence manifold to ensure rapid, efficient mixing of chemiluminescent reagent and sample immediately before reaching the detector; this results in high precision and detectability, particularly with fast, short-lived emissions.The optimum chemical conditions for the chemiluminescence emission were investigated. It was found that a weak CL emission was emitted during the oxidation of this drug with potassium permanganate in acidic solution. The effect of common emission enhancers such as formic acid, formaldehyde, glutaraldehyde, acetaldehyde, quinine, fluorescein, rhodamine B and rhodamine 6G was studied. The parameters selected were 4.0 mol L−1 sulphuric acid, 0.25 mmol L−1 permanganate and 0.75 mol L−1 formaldehyde.Four quantitative parameters adjustable via software settings, two of them typically kinetic parameters, such as rate of the light-development reaction and rate of the light-decay reaction, and the other conventional parameters, such as maximum emission intensity and total emission area, were used to obtain linear calibration graphs with each measurement parameter. The detection limits ranged from 0.011 to 0.026 μg mL−1 and R.S.D. values (n = 10) of 1.21-3.93 at a 0.50 μg mL−1 and 2.01-3.41 at a 1.60 μg mL−1 concentration levels were obtained. The method was satisfactorily applied to the determination of captopril in pharmaceutical preparations. 相似文献
3.
In the present work, a new ligandless-dispersive liquid-liquid microextraction (LL-DLLME) method has been developed for preconcentration trace amounts of copper as a prior step to its determination by flame atomic absorption spectrometry. In the proposed approach 1,2-dicholorobenzene and ethanol were used as extraction and dispersive solvents, respectively. Some factors influencing on the extraction efficiency of copper and its subsequent determination were studied and optimized, such as the extraction and dispersive solvent type and volume, pH of sample solution, extraction time and salting out effect. Under the optimal conditions, the calibration curve was linear in the range of 1.0 ng mL−1-0.6 μg mL−1 of copper with R2 = 0.9985. Detection limit was 0.5 ng mL−1 in original solution (3Sb/m) and the relative standard deviation for seven replicate determination of 0.2 μg mL−1 copper was ±1.4%. The proposed method has been applied for determination of copper in standard and water samples with satisfactory results. 相似文献
4.
A new reversed-phase high performance liquid chromatography with resonance Rayleigh scattering detection (HPLC-RRS) was developed for simultaneous separation and determination of four tetracycline antibiotics (TCs). A good chromatographic separation among the compounds was achieved using a Synergi Fusion-RP column (150 mm × 4.6 mm; 4 μm) and a mobile phase consisting of methanol-acetonitrile-oxalic acid (5 mM) at the flow rate of 0.8 mL min−1. Column temperature was 30 °C. The RRS signal was detected at λex = λem = 370 nm. The recoveries of sample added standard ranged from 95.3% to 103.5%, and the relative standard deviation was below 2.79%. A detection limit of 2.12-5.12 μg mL−1 was reached and a linear range was found between peak height and concentration in the range of 10.36-518.0 μg mL−1 for oxytetracycline (OTC), 12.11-605.5 μg mL−1 for tetracycline (TC), 11.79-589.5 μg mL−1 for chlortetracycline (CTC) and 10.32-516.0 μg mL−1 for doxycycline (DC). The linear regression coefficients were all above 0.999. The method has been applied successfully to the determination of OTC, TC, CTC, DC in pharmaceutical formulations and in honey. The method was simple, rapid and showed a better linear relation and high repeatability. 相似文献
5.
Four simple, rapid, accurate, precise, reliable and economical spectrophotometric methods have been proposed for simultaneous determination of salbutamol sulphate (SS), bromhexine hydrochloride (BH) and etofylline (ET) in pure and commercial formulations without any prior separation or purification. They were first derivative zero crossing spectrophotometry (method 1), simultaneous equation method (method 2), derivative ratio spectra zero crossing method (method 3) and double divisor ratio spectra derivative method (method 4). The ranges for SS, BH and ET were found to be 1-35 μg mL−1, 4-40 μg mL−1 and 5-80 μg mL−1. For methods 1 and 2, the values of limit of detection (LOD) were 0.2314 μg mL−1, 0.4865 μg mL−1 and 0.2766 μg mL−1 and the values of limit of quantitation (LOQ) were 0.7712 μg mL−1, 1.6217 μg mL−1 and 0.9221 μg mL−1 for SS, BH and ET, respectively. For method 3, LOD values were 0.3297 μg mL−1, 0.2784 μg mL−1 and 0.7906 μg mL−1 and LOQ values were 0.9325 μg mL−1, 0.9282 μg mL−1 and 2.6352 μg mL−1 for SS, BH and ET, respectively. For method 4, LOD values were 0.3161 μg mL−1, 0.2495 μg mL−1 and 0.2064 μg mL−1 and LOQ values were 0.9869 μg mL−1, 0.8317 μg mL−1 and 0.6879 μg mL−1 for SS, BH and ET. The precision values were less then 2% R.S.D. for all four methods. The common excipients and additives did not interfere in their determinations. The results obtained by the proposed methods have been statistically compared by means of Student t-test and by the variance ratio F-test. 相似文献
6.
In this work, chemiluminescence (CL) behaviors of two selected phenothiazines, namely promazine and fluphenazine hydrochloride, were investigated for their simultaneous determination using oxidation of Ru(bipy)32+ by Ce4+ ions in acidic media. This method is based on the kinetic distinction of the CL reactions of fluphenazine and promazine with Ru(bipy)32+ and Ce4+ system in a sulfuric acid medium. Least square support vector regression models were constructed for relating concentrations of both compounds to their CL profiles. The parameters of the model consisting of σ2 and γ were optimized using all possible combinations of σ2 and γ to select the model with the minimum root mean square cross validation. Under optimized conditions, the univariate calibration curve was linear over the concentration ranges of 0.4-30.0 μg mL−1 and 0.07-5.0 μg mL−1 with detection limits of 0.1 μg mL−1 and 0.04 μg mL−1 for promazine and fluphenazine, respectively. The influence of potential interfering substances on the determination of promazine and fluphenazine were studied. The proposed method was used for simultaneous determination of both compounds in synthetic mixtures and in spiked human plasma. 相似文献
7.
A novel method to determine isoniazid with high sensitivity and good selectivity has been established by using potassium ferricyanide as spectroscopic probe reagent. In the presence of potassium ferricyanide, it has been demonstrated that iron(III) is reduced to iron(II) by isoniazid at pH 4.0. In addition, the in situ formed iron(II) reacts with potassium ferricyanide to give soluble prussian blue. The absorbance of soluble prussian blue is measured at the absorption maximum of 735 nm, and the amount of isoniazid can be calculated based on this absorbance. A good linear relationship of the concentration of isoniazid versus absorbance is observed with a linear range of 0.040-8.00 μg mL−1. The linear regression equation is A = −0.00286 + 0.28588C (μg mL−1) with a correlation coefficient of 0.9992. The detection limit (3σ/k) is 0.037 μg mL−1, and its relative standard deviation (R.S.D.) is 0.35% (n = 11). Moreover, the apparent molar absorption coefficient of indirect determination of isoniazid is 3.92 × 104 L mol−1 cm−1. The parameters with regard to determination are optimized, and the reaction mechanism is discussed. This method has been successfully applied to the determination of isoniazid in pharmaceutical samples and saliva samples of patients. 相似文献
8.
The directly suspended droplet microextraction (DSDME) technique coupled with the capillary gas chromatography-flame ionization detector (GC-FID) was used to determine BTEX compounds in aqueous samples. The effective parameters such as organic solvent, extraction time, microdroplet volume, salt effect and stirring speed were optimized. The performance of the proposed technique was evaluated for the determination of BTEX compounds in natural water samples. Under the optimal conditions the enrichment factors ranged from 142.68 to 312.13, linear range; 0.01-20 μg mL−1, limits of detection; 0.8-7 ng mL−1 for most analytes. Relative standard deviations for 0.2 μg mL−1 of BTEX in water were in the range 1.81-2.47% (n = 5). The relative recoveries of BTEX from surface water at spiking level of 0.2 μg mL−1 were in the range of 89.87-98.62%. 相似文献
9.
This study presents a novel separation, preconcentration and determination of basic fuchsin (BF) in an aqueous solution by sodium dodecyl sulfate (SDS)-bounded iron oxide nanoparticles (S-IONPs). It is shown that the novel magnetic nano-adsorbent is quite efficient for the adsorption and desorption of BF at 25 °C. Different parameters such as pH, temperature, ionic strength and composition of desorbent solvent were optimized. The effect of some co-existing ions on the determination was investigated. The nanoparticles were analyzed by transmission electron microscopy (TEM) and the sizes of S-IONPs were in the range of 20-100 nm. The method showed good linearity for the determination of BF in the range of 10-300 ng mL−1 with a regression coefficient of 0.9989. The limit of detection (LOD) (signal-to-noise ratio of 3:1) was 0.0073 μg L−1 and the relative standard deviation (RSD) for 0.03 μg mL−1 and 0.2 μg mL−1 of BF were 4.53% and 4.73%, respectively. The BF was determined successfully in spiked samples of Karoon River water. 相似文献
10.
A quantitative method of capillary electrophoresis with sample stacking induced by moving reaction boundary (MRB) was developed for sensitive determination of oxymatrine (OMT) and matrine (MT) in rat plasma. The experimental conditions were optimized firstly. Below are the optimized experimental conditions: 20 mM sodium formate solution (HCOONa, adjusted to pH 10.70 by ammonia) as sample solution, 3 min 14 mbar sample injection, 40 mM formic buffer (HCOOH-HCOONa, pH 2.60) as stacking buffer, 7 min 14 mbar injection of stacking buffer, 100 mM HCOOH-HCOONa (pH 4.80) as separation buffer, 73 cm capillary (effective length 64 cm), 21 kV voltage, 210 nm wavelength. Under the optimized conditions, higher than 60-fold sensitivity improvement of the stacking was simply achieved as compared with capillary zone electrophoresis, and the detectable limits obtained for OMT and MT were 0.26 and 0.19 μg mL−1, respectively. Then, numerous demonstrations were carefully performed for the methodological validations of OMT and MT in rate plasma, including high specificity of method, good linearity (r = 0.9993 for OMT, r = 0.9991 for MT), fair wide linear concentration range (1.30-65.00 μg mL−1 for OMT, 0.84-42.00 μg mL−1 for MT), low limit of detection (1.03 μg mL−1 for OMT, 0.38 μg mL−1 for MT), less than 5% intra- and inter-day variance value, and higher than 96% recovery of OMT and MT in plasma. The developed method could be used for the trace analyses of OMT and MT in plasma and was finally used for the investigation on pharmacokinetic study of OMT in rat plasma. 相似文献
11.
Anastasios Economou Demetrius G ThemelisGeorgios Theodoridis Paraskevas D Tzanavaras 《Analytica chimica acta》2002,463(2):249-255
This work reports a novel flow injection (FI) method for the determination of captopril, 1-[(2S)-3-mercapto-2-methylpropionyl]-l-proline (CPL), based on the enhancement CPL affords on the chemiluminescence (CL) reaction between luminol and hydrogen peroxide. For this purpose alkaline luminol and hydrogen peroxide solutions were mixed online, the sample containing CPL was injected into an aqueous carrier stream, mixed with the luminol-hydrogen peroxide stream and pumped into a glass flow cell positioned in front of a photomultiplier tube (PMT). The increase in the CL intensity was recorded in the form of FI peaks, the height of which was related to the CPL mass concentration in the sample. Different chemical and instrumental parameters affecting the CL response were investigated. Under the selected conditions, the log-log calibration curve was linear in the range 5-5000 μg l−1 of CPL, the limit of detection was 2 μg l−1 (at the 3σ level), the R.S.D., sr was 3.1% at the 100 μg l−1 level (n=8) and the sampling rate was 180 injections h−1. The method was applied to the determination of CPL in pharmaceutical formulations with recoveries in the range 100±3%. 相似文献
12.
Jingyan You Shiqian GaoHaiyan Jin Wenjing LiHanqi Zhang Aimin Yu 《Journal of chromatography. A》2010,1217(12):1875-1881
An on-line method, based on coupling dynamic ultrasonic extraction (DUE), continuously sampling the suspension of sample and solvent, high performance liquid chromatographic separation with diode array detection, has been developed for the determination of the flavonoids, including baicalin, baicalein and wogonin, from the root of Scutellaria baicalensis Georgi. Variables influencing the DUE were evaluated by orthogonal test. The extraction yields of baicalin, baicalein and wogonin in the roots of S. baicalensis Georgi obtained from five different cultivated areas are 73.8–131.5 μg mg−1 (RSD ≤ 6.24%), 6.8–15.9 μg mg−1 (RSD ≤ 5.36%) and 4.4–14.3 μg mg−1 (RSD ≤ 5.30%), respectively. The limits of detection for baicalin, baicalein and wogonin are 0.30, 0.37 and 0.41 μg mL−1, respectively. Linearity is from 0.55 to 109 μg mL−1 for baicalin, from 0.51 to 105 μg mL−1 for baicalein and from 0.53 to 102 μg mL−1 for wogonin. Compared with off-line continuous flow-DUE, the proposed method would be more convenient for the determination of the analytes and the rapid optimization of the extraction process. The extraction yields of flavonoids obtained by the proposed method are comparable with those obtained by dynamic microwave assisted extraction, static ultrasonic extraction and reflux extraction. The result indicated that the proposed method is suitable to determine the active components in Chinese herbal medicine. 相似文献
13.
In this article, a new ligandless dispersive liquid-liquid microextraction method has been developed for preconcentration of trace quantities of silver as a prior step to its determination by flame atomic absorption spectrometry. In the proposed approach, carbon tetrachloride and ethanol were used as extraction and dispersive solvents. Several factors that may be affected on the extraction process, like, extraction solvent, disperser solvent, the volume of extraction and disperser solvent, pH of the aqueous solution and extraction time were optimized. Under the optimal conditions, the calibration curve was linear in the range of 5.0 ng mL−1 to 2.0 μg mL−1 of silver with R2 = 0.9995 (n = 9) and detection limit based on three times the standard deviation of the blank (3Sb) was 1.2 ng mL−1 in original solution. The relative standard deviation for eight replicate determination of 0.5 μg mL−1 silver was ±1.5%. The high efficiency of dispersive liquid-liquid microextraction to carry out the determination of silver in complex matrices was demonstrated. The proposed method has been applied for determination of trace amount of silver in standard and water samples with satisfactory results. 相似文献
14.
A rapid, acetonitrile-free, HPLC method for determination of melamine in infant formula 总被引:3,自引:0,他引:3
Gopalakrishnan Venkatasami 《Analytica chimica acta》2010,665(2):227-12011
A simple, precise, accurate and validated, acetonitrile-free, reverse phase high performance liquid chromatography (HPLC) method is developed for the determination of melamine in dry and liquid infant formula. The separation is performed on a Kromasil C18 column (150 mm × 3.2 mm I.D., 5 μm particle size) at room temperature. The mobile phase (0.1% TFA/methanol 90:10) is pumped at a flow rate of 0.3 mL min−1 with detection at 240 nm. Melamine elutes at 3.7 min. A linear response (r > 0.999) is observed for samples ranging from 1.0 to 80 μg mL−1. The method provides recoveries of 97.2-101.2% in the concentration range of 5-40 μg mL−1, intra- and inter-day variation in <1.0% R.S.D. The limit of detection (LOD) and limit of quantification (LOQ) values are 0.1 μg mL−1 and 0.2 μg mL−1, respectively. 相似文献
15.
A simple, inexpensive and reagent-less colorimetric micro flow analysis (μFA) system was implemented in a polymethyl methacrylate (PMMA) micro fluidic manifold. A T-shaped micro channel on a PMMA chip was fabricated by laser ablation and topped with molded polydimethylsiloxane (PDMS). The fabricated μFA system was integrated with the optical components as detector and applied to the determination of iron in water samples. It is based on the measurement of Fe(III)-nitroso-R salt complex at 720 nm formed by the reaction between Fe(III) and nitroso-R salt in an acetate buffer solution pH 5. The proposed μFA consumed very small amount of reagent and sample, it released waste of less than 2.0 mL h−1. The relative standard deviation (R.S.D.) was less than 2% (n = 11) with the recovery of 98.7 ± 0.12 (n = 5). The linear range for the determination of iron in water samples was over the range of 0.05-4.0 μg mL−1 with a correlation coefficient (r2) of 0.9994. The limit of detection (3σ) and limit of quantitation (10σ) were 0.021 μg mL−1 and 0.081 μg mL−1, respectively with a sample throughput of 40 h−1. 相似文献
16.
A simple and rapid reversed-phase HPLC-UV method was developed for the determination of triterpenic acids in the crude extract of Prunellae Spica. Five triterpenic acids were extracted and isolated from P. Spica as marker compounds for use in the quality control of herbal medicines. Various solvent extraction techniques were evaluated, and the greatest efficiency was observed with sonication in 100% ethanol. Elemental compositions of the five marker compounds were determined by high-resolution mass spectroscopy. The dynamic range of the HPLC-UV method depended on the specific analyte, and acceptable quantitation was obtained between 10 and 250 μg mL−1 for oleanolic acid, between 10 and 300 μg mL−1 for ursolic acid, between 3 and 75 μg mL−1 for 2α,3α,24-trihydroxyolean-12en-28oic acid, between 5 and 100 μg mL−1 for euscaphic acid, and between 5 and 100 μg mL−1 for 2α,3α-dihydroxyurs-12en-28oic acid. The method was deemed satisfactory by inter- and intra-day validation and exhibited both high accuracy and precision (relative standard deviation <9.4%). Overall limits of quantitation and detection were approximately 0.5-2.5 μg mL−1 at a signal-to-noise ratio (S/N) of 3 and were about 3.0-10.0 μg mL−1 at a S/N of 10. In addition, principal component analysis (PCA) was performed on the analytical data of 15 different P. Spica samples in order to classify samples collected from different regions. 相似文献
17.
In pH 4.2-4.8 HAc-NaAc buffer solution, folic acid (FA) could react with uranium (VI) to form a 2:1 anionic chelate which further reacted with some basic triphenylmethane dyes (BTPMD) such as Ethyl Violet (EV), Methyl Violet (MV) and Crystal Violet (CV) to form 1:2 ion-association complexes. As a result, not only the absorption spectra were changed, but also the intensities of resonance Rayleigh scattering (RRS) were enhanced greatly and the new RRS spectra were observed. The maximum RRS wavelengths were located at 328 nm for EV system, 325 nm for MV system and 328 nm for CV system. The fading degree (ΔA) and RRS intensities (ΔI) of three systems were different. Under given conditions, the ΔA and ΔI were all directly proportional to the concentration of FA. The linear ranges and the detection limits of RRS methods were 0.0039-5.0 μg mL−1 and 1.2 ng mL−1 for EV system, 0.0073-4.0 μg mL−1 and 2.2 ng mL−1 for MV system, 0.014-3.5 μg mL−1 and 4.7 ng mL−1 for CV system. The RRS methods exhibited higher sensitivity, so they are more suitable for the determination of trace FA. The optimum conditions, the influencing factors and the effects of coexisting substances on the reaction were investigated. The method can be applied to the determination of FA in serum and urine samples with satisfactory results. The structure of the ternary ion-association complex and the reaction mechanism were discussed in this work. 相似文献
18.
Beatrice Campanella Massimo Onor Marco Carlo Mascherpa Alessandro D’Ulivo Carlo Ferrari Emilia Bramanti 《Analytica chimica acta》2013
We developed a flow injection (FI) method for the determination of thiomersal (sodium ethylmercurithiosalicylate, C9H9HgNaO2S) based on the UV/microwave (MW) photochemical, online oxidation of organic mercury, followed by cold vapor generation atomic fluorescence spectrometry (CVG-AFS) detection. Thiomersal was quantitatively converted in the MW/UV process to Hg(II), with a yield of 97 ± 3%. This reaction was followed by the reduction of Hg(II) to Hg(0) performed in a knotted reaction coil with NaBH4 solution, and AFS detection in an Ar/H2 miniaturized flame. The method was linear in the 0.01–2 μg mL−1 range, with a LOD of 0.003 μg mL−1. This method has been applied to the determination of thiomersal in ophthalmic solutions, with recoveries ranging between 97% and 101%. We found a mercury concentration in commercial ophthalmic solutions ranging between 7.5 and 59.0 μg mL−1. 相似文献
19.
A novel fluorescent probe for Cu2+ determination based on the fluorescence quenching of glyphosate (Glyp)-functionalized quantum dots (QDs) was firstly reported. Glyp had been used to modify the surface of QDs to form Glyp-functionalized QDs following the capping of thioglycolic acid on the core–shell CdTe/CdS QDs. Under the optimal conditions, the response was linearly proportional to the concentration of Cu2+ between 2.4 × 10−2 μg mL−1 and 28 μg mL−1, with a detection limit of 1.3 × 10−3 μg mL−1 (3δ). The Glyp-functionalized QDs fluorescent probe offers good sensitivity and selectivity for detecting Cu2+. The fluorescent probe was successfully used for the determination of Cu2+ in environmental samples. The mechanism of reaction was also discussed. 相似文献
20.
A new, simple and highly sensitive method for spectrofluorimetric determination of amiloride (AMI) and furosemide (FUR) in pharmaceuticals is presented. The proposed method is based on the separation of AMI from FUR by solid-phase extraction using a nylon membrane, followed by spectrofluorimetric determination of both drugs, on the solid surface and the filtered aqueous solution, respectively. AMI shows low native fluorescence, but its separation-preconcentration by immobilization (solid-phase extraction) on nylon membrane surface provides a considerable enhancement in fluorescence intensity. The fluorescence determination is carried out at λex = 237, λem = 415 nm for FUR; and λex = 365, λem = 406 nm for AMI. The calibration graphs are linear in the range 3.20 × 10−4 to 0.8 μg mL−1and 1.33 × 10−3 to 4.0 μg mL−1, for AMI and FUR, respectively, with a detection limit of 9.62 × 10−5 and 4.01 × 10−4 μg mL−1 (S/N = 3). The commonly found excipients in commercial pharmaceutical formulations do not interfere. The developed method is successfully applied to the determination of both drugs in pharmaceutical formulations. 相似文献