主成分分析-紫外光谱法同时测定四种维生素B

采用主成分分析法(PCA)完成对多组分样品分析的建模及解析研究,用于处理紫外光谱数据,实现了维生素B_1、B_2及B_6及烟酰胺四组分的同时测定,结果可靠,操作简便。     

Simultaneous Determination of Adrenaline and Noradrenaline by First Derivative Spectrophotometry in a Fia Assembly

Abstract

This article deals with the design of an unsegmented-flow injection manifold for the simultaneous determination of adrenaline and noradrenaline two structurally related compounds with overlapping spectra. An FIA manifold is proposed for the simultaneous determination in which the sample solution is directly injected into a carrier-reagent stream of aqueous NaOH. The selected wavelengths (first derivative) were 394 and 342 nm, for noradrenaline and adrenaline, respectively with an integration time of 0.4 s. The calibration graphs are linear over the range 2.0–30 ppm for both drugs. The method is applied to different synthetic mixtures of both drugs.     

Determination of Ranitidine Hydrochloride in Pharmaceutical Preparations by Ultraviolet and Visible Spectrophotometry

Abstract

Ranitidine hydrochloride in tablets (T) and injections (I) was determined by ultraviolet spectrophotometry (UVS) at 313 nm and visible spectrophotometry (VISS) at 615 nm, after reaction with 3-methyl-2-benzothiazolinone hydrazone hydrochloride (MBTH) and ferric chloride. For UVS, Beer's law was obeyed in the range 5.0 – 18.0 μg/mL. The coefficients of variation (CV) for the samples T were 0.36% and 0.71% and for the samples I were 0.51% and 0.24%. The recovery average (RA) was 99.88%. For UVS, Beer's law was observed in the range 1.44 – 5.76 μg/mL. The CV for T were 0.72% and 0.59%, and for I were 0.53% and 0.61%. The RA was 99.39%. The precision and accuracy of the two methods were compared.     

一阶导数分光光度法直接测定肉制品中硝酸盐及亚硝酸盐的含量

本文研究了硝酸盐及亚硝酸盐的一阶导数光谱，选择亚硝酸盐的一阶导数光谱与基线相交点２０７ｎｍ，作为硝酸盐的测定波长；选择硝酸盐在２０７ｎｍ、２２０ｎｍ处导数值相等，作为双波长法测定亚硝酸盐的测定波长。结果表明，硝酸盐及亚硝酸盐在１～１５μｇ／ｍＬ浓度范围内线性关系良好，合成样分析，加标回收试验，样品测定同标准比色法对照均获得满意结果。     

Simultaneous Determination of Two Synthetic Dyes Erytrosine and Sunset Yellow in a Pharmaceutical Syrup By First Derivative Visible Spectrophotometry

ABSTRACT.

A rapid first derivative spectrophotometric method for simultaneous determination of two synthetic dyes, erytrosine (E 127) and sunset yellow (E 110), in a mixture is proposed. The procedure does not require any separation step. The method was applied for determining the two compounds in a pharmaceutical syrup. Good linearity, accuracy, precision and selectivity were found, and the method is proposed for routine quality control purposes.     

First Derivative Spectrophotometric Determination of Certain Drugs in Two-Component Mixtures

Abstract

Four two-component mixtures have been assayed using both Vierordt's and first derivative spectrophotometric methods. Such mixtures are acepifylline and phenobarbitone, phenylbutazone and amidopyrine, procaine and caffeine, and sulphamethoxazole and trimethoprim. These selected applications illustrate the relative ease and simplicity offered by first derivative spectrophotometry for the assay of two component mixtures with spectral interferences from matrix formulations.     

Simultaneous Determination of Cobalt and Nickel Using Morpholinedithiocarbamate (MDTC) as Reagent by First and Second Derivative Spectrophotometry

A selective and sensitive derivative method has been proposed for the simultaneous determination of trace amounts of Co(II) and Ni(II) with morpholinedithiocarbamate (MDTC) in the presence of sodium lauryl sulphate (SLS). The molar absorption coefficients of the 1:2 complex of Co(II) and Ni(II) at 326 nm and 322 nm are 2.248 × 10⁴ and 2.505 × 10⁴ L mol^?1 cm^?1 for zero order. The analytical sensitivity for the second derivative of Co(II) and Ni(II) complexes are 0.0044 μg mL^?1 and 0.0060 μg mL^?1. The developed derivative procedure, using the zero‐crossing technique, has been successfully applied for the analysis of Co(II) and Ni(II) simultaneously in different alloy samples.     

Simultaneous Determination of Perphenazine and Amitriptyline by Derivative Spectrophotometry

Abstract

Two methods have been developed for the simultaneous determination of Amitryptiline and Perphenazine: the zero-crossing (I) and the derivative ratio spectrum (II) methods and both use the derivative spectrophotometry.

The methods have been applicable in the ranges of 1 to 30 μg·ml^?1 of Amitryptiline (I and II) and between 1 and 8 μg·ml^?1 and from 1 to 7 μg·ml^?1 of Perphenazine for the methods I and II respectively. The accuracy of the proposed methods have been studied and they have been used in the determination of Amitryptiline and Perphenazine in commercially available pharmaceuticals.     

Simultaneous Determination of Atenolol and Chlorthalidone in Pharmaceutical Preparations by Capillary-Zone Electrophoresis

Abstract

A capillary zone electrophoresis (CZE) method for the simultaneous determination of the β-blocker drugs atenolol and chlorthalidone in pharmaceutical formulations has been developed. The CZE separation was performed under the following conditions: capillary temperature, 25°C; applied voltage, 25 kV; 20 mM H₃PO₄–NaOH running buffer (pH 9.0); and detection wavelength, 198 nm. Phenobarbital was used as internal standard. The method was validated and showed not only good precision and accuracy but also good robustness. The method has been successfully applied to the simultaneous determination of both atenolol and chlorthalidone in pharmaceutical tablets.     

Rapid and Accurate Determination of Acetaminophen and Phenprobamate in Binary Mixtures by Derivative-Differential UV Spectrophotometry and Ratio-Spectra Derivative Spectrophotometry

ABSTRACT

Derivative-Differential UV spectrophotometry and ratio-spectra first derivative spectrophotometry are presented for the simultaneous determination of analgesic and myorelaxan mixtures, namely acetaminophen (A)- phenprobamate (P). Derivative-Differential UV spectrophotometry is based on pH changes. The other method depends on the application ratio-spectra first derivative spectrophotometry to resolve the interference due to spectral overlapping.

The proposed methods were applied to the determination of this compound in synthetic mixtures and in pharmaceutical preparations. The proposed methods, which give thoroughly comparable data, are simple and rapid, and allow one to obtain precise and accurate results.     

Solid Phase Spectrophotometry for the Determination of Cobalt in Pharmaceutical Preparations

 A new sensitive method exploiting solid-phase spectrophotometry is proposed for the determination of cobalt in pharmaceutical preparations. The chromogenic reagent 1-(2-thiazolylazo)-2-naphthol (TAN) was immobilized on C18 bonded silica loaded into a home-made cell with 1.5 mm of optical path for cobalt determination. Cobalt(II) reacts with TAN on C18 material, at pH 6.0–7.5, to give a coloured complex which has maximum absorption at 572 nm. In this way, the sample was passed through the cell and Co(II) ions were quantitatively retained on the solid-phase. After the direct measurement of light-absorption in the solid phase, only the cobalt was eluted with 0.1 mol L⁻¹ hydrochloric acid. The cell was washed with water and then another sample solution could be passed through the cell. The procedure allowed the determination of cobalt in the range of 10–160 μg L⁻¹ with coefficient of variation of 4.7% (n=10) and apparent molar absorptivity of 2.62 × 10⁶ L mol⁻¹ cm⁻¹ using sample volume of 3-mL. Received May 15, 2000. Revision August 28, 2000.     

Determination of Amoxycillin and Clavulanic Acid in Some Pharmaceutical Preparations by Derivative Spectrophotometry

 Derivative spectrophotometry was applied for the simultaneous determination of amoxycillin and clavulanic acid in pharmaceutical preparations: “Augmentin” inj. and tablets and “Amoksiklav” drops and tablets, in solutions after hydrolysis with sodium hydroxide. As the absorption spectra overlap strongly (amoxycillin λ_max = 247 nm and 290 nm, clavulanic acid λ_max = 258 nm) the first and the second derivative spectrophotometric procedure was elaborated for their determination. Amoxycillin was determined at λ = 257.9 nm (1-st derivative spectra) or λ = 273 nm (2-nd derivative) while clavulanic acid at λ = 280.3 nm (1-st derivative) or λ = 285 nm (2-nd derivative spectra). The Beer’s law is obeyed in the range of 0.004–0.04 mg/ml for amoxycillin and 0.002–0.02 mg/ml for clavulanic acid. Received December 6, 1999. Revision August 1, 2000.     

Application of Derivative and Ratio Spectra Derivative Spectrophotometry for the Determination of Pseudoephedrine Hydrochloride and Acrivastine in Capsules

Abstract

Two new spectrophotometric methods are used for the determination of acrivastine and pseudoephedrine hydochloride in their mixture without previous chemical separation. In the first, second derivative spectrophotometry, the measurements are made at 288.0 nm for acrivastine and at 270.2 nm for pseudoephedrine hydrochloride in the second derivative spectra of their solution in 0.1M NaOH. In the second, ratio spectra derivative spectrophotometry, the amplitudes are measured at 276.0 nm and 298.5 nm corresponding to two maximums for acrivastine, and at 252.6 nm and 268.3 nm corresponding to a maximum and a minumum, respectively, for pseudoephedrine hydrochloride in first derivative of their ratio spectra plotted by using of their solutions as divisor. The methods were successfully applied for the determination of these drugs in a commercial pharmaceutical formulation capsule.     

Difference spectrophotometric determination of some pharmaceutically important thioxanthene derivatives in dosage forms

A Spectrophotometric method is described for the rapid determination of four thioxanthene derivatives, namely chlorprothixene, thiothixene, flupenthixol hydrochloride and clopenthixol hydrochloride. The method is based on measuring the first derivative spectrum (D ₁) of the oxidized drug relative to a solution of the underivatized drug. At the wavelength of maximum difference in first derivative (range 285–315 nm), only the oxidation products have an appreciable difference in first derivative and the oxidizing agent has no absorbance. The oxidation products (assumed to be the thioxanthone sulphoxides) are formed rapidly at room temperature by the addition of peroxyacetic acid, prepared by the slow reaction of hydrogen peroxide and glacial acetic acid. The first derivative of the absorbance is proportional to the concentration of the drugs in solution over the ranges 2–14 g ml^–1 for chloroprothixene, 2–20 g ml^–1 for clopenthixol hydrochloride, 2–24 g ml^–1 for thiothixene and 4–40 g ml^–1 for flupenthixol hydrochloride. The method is specific for the intact drug and can be adopted in the presence of oxidative and photochemical decomposition products and tablet excipients. The recoveries ranged from 99.7 ± 1.3 to 100.2 ± 1.5%. The validity of the method was tested by analysing synthetic samples of thioxanthenes and some dosage forms containing the drugs; the results were in accordance with those given by the official methods.     

以四(对羟基苯基)卟啉作显色剂组合导数分光光度法同时测定锌、镉的研究

本文利用“组合导数分光光度法”,在碱性介质中,以四(对-羟基苯基)卟啉作显色剂,以咪唑作催化剂,对锌、镉的同时测定进行了详细研究。该法使测定锌的表观摩尔吸光系数提高到10~6L·mol~(-1)·cm~(-1),同时解决了重叠谱带相互干扰的问题。对合成样品进行分析,结果令人满意。     

Determination of Mefenamic Acid and Paracetamol by First Derivative Spectrophotometry

Abstract

A direct and simple first derivative spectrophotometric method has been developed for the determination of mefenamic acid and paracetamol in pharmaceutical formulations. A methanolic hydrochloric acid solution was used as solvent for extracting the drugs from the formulations and subsequently the samples were evaluated directly by derivative spectrophotometry. Simultaneous determination of both drugs can be carried out using the zero-crossing and the graphical methods. The methods do not require simultaneous equations to be solved. The calibration graphs were linear in the ranges from 1.8 × 10^?6 to 1.6 × 10^?4 M of mefenamic acid and from 4.1×10^?6 to 1.4 × 10^?4 M of paracetamol. The ingredients commonly found in commercial pharmaceutical formulations do not interfere. The proposed method was applied to the determination of these drugs in tablets.     

Simultaneous Determination of Atrazine and Chlorpyrifos in Pesticide Formulations,in Soils and Waters by Derivative Spectrophotometry and Ratio Spectra Derivative

Abstract

A new method is described to analyse a binary mixture of atrazine and chlorpyrifos, using first-derivative spectrophotometry for atrazine and first derivative of the ratio spectra for chlorpyrifos. The procedure does not require any separation step. Calibration graphs were linear up to 15 μg.mL^?1 of atrazine and to 10 μg.mL^?1 of chlorpyrifos. The method has been applied to determine both compounds in pesticide formulations, in soils and waters.     

Determination of Procaine Penicillin G and Penicillin G by Second Derivative Spectrophotometry in Pharmaceutical Products

Abstract

“Zero-crossing” derivative spectrophotometry has been used for determining binary mixtures of penicillin G and procaine penicillin G.

The procedure is rapid, simple, nondestructive, and does not require resolutions of equations.

Calibration graphs are linear between 2.0 and 50.0 μg mL^?1 of the penicillin G at 226.0 nm, and between 2.0 and 100.0 μg mL^?1 of procaine penicillin G at 319.0 nm, in the presence of each other. A complete and exhausive statistical analysis of the experimental data was realized to demonstrate the validity of method. The method was successfully applied to assay commercial injections of these drugs.     

微波消解-零交截距导数分光光度法同时测定催化剂中钴和镍

采用微波法消解催化剂 ,研究确定了微波消解催化剂的最佳工作条件。应用零交截距导数分光光度法解决了 PAR- CO2 +、PAR- Ni2 +体系中 Co2 +、Ni2 +的同时测定。钴和镍的线性范围分别为 0～ 30 μg/ 2 5m L和 0～ 2 5μg/ 2 5m L,催化剂样品中钴和镍测定结果的相对标准偏差 (n=5)分别≤ 1 .5%和≤ 1 .0 % ,与标准值相对误差分别≤± 1 .5%和≤± 2 .1 %。本方法测定催化剂中钴和镍 ,酸用量少 ,降低了环境污染