Determination of various hemoglobin species with thermal-lens spectrometry

Desoxyhemoglobin, oxyhemoglobin, carboxyhemoglobin, methemoglobin, cyanohemoglobin, and hemichrome are determined using thermal-lens spectrometry, with the detection limits at the level of 10^?8 M/l (2–5 mcg/l depending on hemoglobin species). Signal behavior and detectability thresholds are in good agreement with theoretical modeling based on the approach proposed earlier by the authors to describe thermal-lens signal generation in complex (inhomogeneous) systems. The thermooptical response for all studied hemoglobin species depends on the power of laser radiation within the range of 1–50 mW (532, 514.5, and 488 nm). Under the conditions of a thermal-lens experiment, the total temperature growth (0.0001 K) due to heating of the studied solution as the radiation of the inducing laser is absorbed by hemoglobin is estimated. Due to the interference with oxyhemoglobin the error in determining desoxyhemoglobin using thermal-lens spectrometry (for a maximum radiation power of 532 nm, 210 mW) does not exceed 3% in the case when the ratio of the species is 10: 1. In the opposite case (determination of oxyhemoglobin in the presence of desoxyhemoglobin), the error does not exceed 5%, the ratio of test and interfering species being the same.     

Determination of copper with neocuproine by thermal-lens spectrometry

Conditions for the spectrophotometric determination of copper with 2,9-dimethyl-l,10-phenan-throline (neocuproine) in the presence of ascorbic acid in a water-ethanol solution (9 : 1) at pH 4.5–5.0 have been found. The detection limit is 3 x 10^-6 M. The concentration range is from 4.4 x 10^-6 to 3 x 10^-4 M. Conditions for the determination of copper(I) with neocuproine by thermal lens spectrometry have been proposed. The detection limit is 4 x 10^-7 M. The concentration range is from 7 x 10^-7 to 6 x 10^-5 M. Iron(II) at concentrations as high asn x 10^-4 M does not interfere with the determination of copper. Changes in the conditions for the photometric reaction associated with passing from spectrophotometric measurements to thermal lensing are discussed.     

Microchannel-assisted thermal-lens spectrometry for microchip analysis

We present a new method for homocysteine quantitation in human plasma based on in-capillary reaction of homocysteine with 2,2′-dipyridyl disulfide. Homocysteine is in this so-called thiol-exchange reaction quantitatively transformed in mixed disulfide concomitantly with formation of an equimolar amount of 2-thiopyridone that is further separated by micellar electrokinetic chromatography and determined specifically at 343 nm. The concentration of homocysteine is thus estimated indirectly from the result of 2-thiopyridone determination. The linear detection range for concentration versus peak area for the assay was from 0.03–3 mM (correlation coefficient 0.994) with a detection limit of 6 μM and a limit of quantitation 20 μM. The inter-day reproducibility of the peak area and the migration time were 1.37% and 0.05%, respectively. The method is simple, relatively rapid and can be easily automated. Moreover the common capillary electrophoresis apparatus with a UV detector can be used to distinguish between normal and pathological hyperhomocysteinemia plasma samples.     

Investigation of ionene adsorption on quartz surfaces by thermal-lens spectrometry

Thermal-lens spectrometry was used for the investigation of the adsorption of ionene to quartz surfaces. The thermooptical analysis of the surface makes it possible to distinguish the modified surface from a clean quartz surface and to provide sensitive direct concentration measurements of the light absorbing co-adsorbed substance. The co-adsorption of chromate ions and 2,10-ionene from aqueous solutions to quartz surfaces was investigated and the desorption procedure proposed.     

Determination of cinnarizine in pharmaceutical preparations by spectrophotometry, atomic absorption spectrometry and potentiometry

New methods are developed for the determination of cinnarizine in various dosage forms. They are based on the reaction of cinnarizinium cation with cobalt tetrathiocyanate anion, whereby a sparingly soluble blue 21 drug: reagent ion-pair complex is quantitatively formed. The complex is (a) extracted with nitrobenzene and spectrophotometrically measured at 622 nm; (b) extracted with nitrobenzene and nebulized in an air-acetylene flame for atomic absorption spectrometric monitoring of cobalt at 242.5 nm; and (c) dispersed in a PVC membrane plasticized with 2-nitrophenyloctyl ether and used as a sensor for direct potentiometric determination of the drug. Optimum reaction conditions and performances of the three analytical techniques are evaluated and compared. At the 25 mg level of cinnarizine, the three methods give results with equal accuracy and precision. The average recovery is 98–99% of the nominal and the mean standard deviation is 0.7%. No significant interferences are caused by drug excipients and diluents.     

Determination of ethambutol in pharmaceutical preparations by atomic absorption spectrometry,spectrophotometry and potentiometry

Simple methods are described for the determination of ethambutol in pharmaceutical preparations. They are based on the reaction of the drug with copper phosphate suspension in a borate buffer of pH 9.2, whereby a blue 11 water-soluble copper-ethambutol complex is quantitatively formed. Four portions of the reaction solution are used for (i) measurement of copper by atomic-absorption spectrometry at 324.7 nm; (ii) potentiometric titration with EDTA with use of a solid-state copper ion-selective electrode; (iii) visual titration with EDTA (copper-PAN indicator); and (iv) spectrophotometric measurement of the copper-ethambutol complex at 640 nm. The results obtained are in good agreement and are better than those of the British Pharmacopoeia (BP) method.     

Determination of boron in silicon-doped gallium arsenide by electrothermal atomic absorption spectrometry and ultraviolet-visible spectrophotometry

Two methods have been developed for the determination of boron impurities in silicon-doped gallium arsenide (GaAs) for electronics. The first method employs the electrothermal atomic absorption spectrometry (ETAAS), the second, the UV-Vis molecular absorption spectrophotomety. In both cases the GaAs sample is decomposed with aqua regia (1+1). To prevent Ga(III) interference on the ETAAS determination of boron, a double extraction of the chlorogallic acid (HGaCl4) in diethyl ether is performed. To improve the overall ETAAS performance, the graphite tubes were pre-treated with iridium(III) and tungsten(IV). A mixed chemical modifier containing Ni(II), Sr(II) and citric acid was also used. The characteristic mass (m0) is 301 +/- 47 pg and the detection limit (3sB) is 2.4 microg g(-1). The classic UV-Vis spectrophotometric procedure using curcumin was also extended to the determination of boron in GaAs. By masking Ga(III) with EDTA and a preliminary extraction of boron with 2-ethyl-hexane 1,3-diol, performed on a semi-micro scale, a detection limit of 0.6 microg g(-1) was achieved. Both methods were applied to the analysis of two Si-doped GaAs samples which were suspected of being boron-contaminated. Results are compared with those obtained by direct analysis of the decomposed sample solution using the inductively coupled plasma atomic emission spectrometry (ICP-AES).     

Determination of chloramphenicol in pharmaceutical preparations by the cadmium ion-selective electrode, spectrophotometry and atomic-absorption spectrometry

New simple methods are described for the determination of chloramphenicol and its esters in pure powders, suppositories, injections, eye-drops, capsules and oral suspensions. These are based on reduction with cadmium metal whereby 6 equivalents of cadmium ions per mole and the corresponding amino-derivative are released. Four portions of the reduction products are used for (i) measurement of the cadmium ions by atomic-absorption spectrometry at 228.8 nm; (ii) potentiometric titration with EDTA, with use of the cadmium ion-selective electrode; (iii) visual titration with EDTA, with Eriochrome Black T as indicator, (iv) diazotization and coupling with N-(1-naphthyl)ethylenediamine and measuring the resultant colour at 550 nm. The results obtained by these procedures are in good agreement, and compare favourably with those of the official methods.     

曙红分光光度法测定沙拉沙星

在pH 3.0的Clark-Lubs缓冲溶液存在下,盐酸沙拉沙星溶液在可见光区无吸收,当将其加入曙红溶液中,发现曙红吸收峰有明显位移,且吸光度增加,说明盐酸沙拉沙星与曙红反应生成络合物。盐酸沙拉沙星在4.0-220.0mg/L的范围内与吸光度呈良好的线性关系,方法检出限为117.6μg/L。用于片剂中盐酸沙拉沙星的测定,6次平行测定相对标准偏差为1.4%-3.9%,回收率为92.8%-105.8%。     

乙酰乙酸乙酯分光光度法测定甲醛的研究

乙酰乙酸乙酯在弱酸性溶液中与甲醛及铵离子反应,生成2,6-二甲基-1,4-二氢-3,5-吡啶二乙酸乙酯,该化合物在375nm处有最大吸收,以甲醛计的摩尔吸光系数为5.533×103mol·cm-1·L-1;利用该反应建立了测定食品中微量甲醛的新方法,甲醛质量浓度在0.08～4.0mg/L成线性关系。并用质谱分析了产物,证实在水溶液中该反应遵循汉秋希吡啶合成法的原理。     

Differential kinetic determination of cobalt and vanadium with thermal-lens monitoring

On the example of a model indicator reaction of oxidation of cobalt (II) and vanadium (IV) ions by a complex of iron (III) with 1,10-phenantroline, resulting in the formation of tris-(1,10-phenantroline) iron (II), an application of thermal-lens detection of analytical signal with differential kinetic methods is reported. For the simultaneous differential kinetic determination of cobalt (II) and vanadium (IV) with thermal-lens signal detection (514.5 nm, 35.5 mW), the achieved limit of detection (LOD) is 2 ng/ml for both metals, matching the respective values for individual determination. In comparison to spectrophotometric techniques, the effect of synergy, which reduces the sensitivity of detection in the system, is found to be negligible. In general, the sensitivity of differential kinetic determination of cobalt (II) and vanadium (IV) with thermal-lens registration of signal is superior to the analogous procedure with spectrophotometric control of the reaction velocity by two orders of magnitude.     

Determination of chlorprothixene and amitryptyline hydrochlorides by UV-derivative spectrophotometry and UV-solid-phase spectrophotometry

Two methods for spectrophotometric determination of chlorprothixene and amitryptyline hydrochlorides were proposed. One of them is based on spectral analysis of their derivative spectra. The measurement of the value at 316.0 nm of first derivative was used for construction of calibration graph for chlorprothixene. The Beer law was obeyed in the concentration range 0.5-50.0 microg ml(-1). The amplitude of the second derivative at 261.4 nm was used for determination of amitryptyline in the range 0.5-75.0 microg ml(-1). The second proposed method is utilized the use of solid sorbent for simultaneous preconcentration and assay of studied compounds. For this purpose the filtration gel Sephadex G100 was applied. The elaborated solid-phase spectrophotometric method was used for determination of chlorprothixene at 268.0 nm in the range 2.5-75.0 microg ml(-1) and amitryptyline at 238.0 nm in the concentration range 10.0-75.0 microg ml(-1).     

Determination of plasma ethambutol with liquid chromatography and ultraviolet spectrophotometry

The method presented here is based on the ability of ethambutol to give chelates with divalent cationic metals. With copper salts, the chelate presents a characteristic ultraviolet absorbance at 270 nm, making it possible to titrate ethambutol extracted from plasma with chloroform in alkaline medium. The column which was used contained silica (LiChrosorb Si 60, 5 microns) and the mobile phase was a mixture of equal parts of water and acetonitrile, containing copper sulphate and ammonia. The internal standard was a lower homologue of ethambutol with the same chelating ability. The detection limit was 0.15 mg/l. No interference with other antitubercular agents was observed.     

分光光度法测定薯蓣皂苷元

采用高氯酸反应使薯蓣皂苷元显色 ,对影响显色反应的主要因素进行了考察 ,于 41 0nm波长处对穿山龙中薯蓣皂苷元的含量进行测定 ,测定结果与高效液相色谱法相近。方法的线性范围为 3.1 2～2 1 .84μg mL ,适用于薯蓣皂苷元提取过程中的常规检测     

Reaction of phenyldichlorophosphine with diacetyl

Conclusions Phenyldichlorophosphine reacts with diacetyl to form 5-methyl-2-phenyl-4-chloro-2-oxo-1,2-oxaphosphol-4-ene. Hydrolysis of this compound gives phenyl-(-chloro--oxo)butylphosphinic acid, and alcoholysis gives the ester of this acid.Translated from Izvestiya Akademii Nauk SSSR, Seriya Khimicheskaya, No. 2, pp. 466–468, February, 1969.     

Determination of amitriptyline,imipramine and orphenadrine in antidepressant drugs by potentiometry,spectrophotometry and atomic absorption spectrometry

Methods are described for the determination of amitriptyline, imipramine and orphenadrine in some antidepressant drugs. They are based on a prior reaction with ammonium reineckate to form 11 water-insoluble drugreineckate ion-pair complexes. These complexes are (i) used as ion-exchangers in liquid-membrane electrodes responsive to the drug cations, (ii) extracted with nitrobenzene or dissolved in acetonitrile and spectrophotometrically measured at 525 nm and (iii) dissolved in 90% acetone followed by nebulization in an air-acetylene flame for atomic absorption spectrometric measurements of Cr at 358.6 nm. The reaction and monitoring conditions are optimized to permit determination of as little as 10 g/ml of the drugs. Determination of the drugs in some pharmaceutical preparations shows an average recovery of 98.8% of the nominal and a mean standard deviation of 0.8%. The results compare favorably with data obtained by the United States and British Pharmacopoeia methods.     

固绿FCF分光光度法测替米沙坦的含量

在pH6.2的Britton-Robinson缓冲介质中,替米沙坦(TMST)与生物染色剂固绿FCF(FGF)反应,形成离子缔合物,溶液颜色发生明显改变,最大正、负吸收波长分别位于598、632 nm,从而建立光度法测定替米沙坦.在598、632 nm处,替米沙坦分别在0～1.35×10-5mol/,L、0～1.05×...     

紫外光谱法测定乙酸乙烯酯中的对苯二酚

采用紫外光谱法测定乙酸乙烯酯中对苯二酚含量时,乙酸乙烯酯中的有机杂质会对测试结果产生影响.其中乙醛、丙酮对测试结果的影响程度基本呈线性递增关系,而醋酸甲酯、醋酸乙酯对测试结果不会产生影响.