Spectrophotometric determination of chlorpromazine hydrochioride by 1,10-phenanthroline

在HAc-NaAc缓冲介质中,盐酸氯丙嗪(CPZ)能定量使Fe(Ⅲ)还原为Fe(Ⅱ),还原生成的Fe(Ⅱ)与邻二氮菲反应生成稳定的红色络合物,并且在一定范围内,CPZ的浓度和生成的红色络合物的吸光度呈良好的线性关系.据此,提出邻二氮菲-Fe(Ⅲ)体系测定盐酸氯丙嗪的新方法.在优化的实验条件下,盐酸氯丙嗪的质量浓度在0.040～15.00mg/L范围内与吸光度呈现良好的线性关系,线性相关系数R=0.9995,摩尔吸光系数ε=2.8×104L·mol-1·cm-1,检出限为0.020mg/L.11次重复测定的相对标准偏差小于2.9％.该方法用于药物中盐酸氯丙嗪的测定,结果满意.     

铁氰化钾-Fe(Ⅲ)分光光度法测定盐酸氯丙嗪

建立了以铁氰化钾-Fe(Ⅲ)体系测定盐酸氯丙嗪的新方法.研究表明,盐酸氯丙嗪可以使Fe(Ⅲ)还原为Fe(Ⅱ),还原生成的Fe(Ⅱ)可以与K3[Fe(CN)6]反应生成可溶性普鲁士蓝KFe[Fe(CN)6].盐酸氯丙嗪的质量浓度在0.21-32.00μg/mL范围内与吸光度呈现良好线性关系,线性回归方程A=0.01854+0.07652p(μg/mL),相关系数R=0.9992,摩尔吸光系数ε=2.5×10(4)·L·mol-1·cm-1,检出限0.12μg/mL.方法用于测定药物和血清中盐酸氯丙嗪含量,回收率为98.1%～101.3%.     

分光光度法测定固相表面酰肼活化基团

建立了一种测定固相表面酰肼基团含量的方法.运用Fe(Ⅲ)-邻二氮菲显色体系,通过固相表面具有较强还原性的酰肼基团将Fe(Ⅲ)还原为Fe(Ⅱ),生成的Fe(Ⅱ)可与邻二氮菲生成稳定的桔红色络合物,从而利用分光光度法测定溶液体系吸光度来表征固相表面酰肼基团的含量.该方法在0～0.02 μmol/mL范围内呈良好线性关系,线...     

Fe(Ⅲ)分光光度法测定盐酸氯丙嗪

建立了以Fe(Ⅲ)为氧化剂分光光度法测定盐酸氯丙嗪的方法。在盐酸介质中,Fe(Ⅲ)将盐酸氯丙嗪氧化形成一种红色化合物,该化合物的最大吸收波长位于525 nm,其摩尔吸光系数ε=1.05×104 L/(mol·cm)。盐酸氯丙嗪的质量浓度在0~20.0 mg/L范围内与体系的吸光度呈良好的线性关系,线性相关系数r=0.999 2,加标回收率为94.0%~100.4%,测定结果的相对标准偏差为0.55%~1.42%(n=6)。该法灵敏度较高、选择性及重现性良好,可用于药品和血清中盐酸氯丙嗪的测定。     

邻菲口罗啉-Fe(Ⅱ)体系光度法间接测定头孢噻肟钠

基于头孢噻肟钠在0.3 mol/L NaOH溶液中沸水浴降解产物具有还原性,在酸性介质中可将Fe(Ⅲ)还原为Fe(Ⅱ),邻菲口罗啉能与所生成的Fe(Ⅱ)显色生成红色络合物,最大吸收波长λ=508 nm;表观摩尔吸光系数ε=1.1×104L.mol-1.cm-1;头孢噻肟钠在0.4~80μg/mL范围内呈良好的线性关系;线性回归方程为A=-0.00204 0.01989ρ(μg/mL);线性相关系数r=0.9998;检出限为0.18μg/mL;RSD为1.2%(5.0μg/mL,n=11);平均回收率为99%。初步探讨了反应机理,并优化了对头孢噻肟钠的测定条件。     

紫尿酸显色分光光度法测定盐酸氯丙嗪片剂含量

建立了以紫尿酸为显色剂测定盐酸氯丙嗪的光度法。在弱酸性条件下,Fe(Ⅲ)被盐酸氯丙嗪定量还原成Fe(Ⅱ),Fe(Ⅱ)在碱性条件下与紫尿酸反应形成不稳定的蓝色配阴离子,该配阴离子与盐酸氯丙嗪形成稳定的蓝色离子缔合物,该离子缔合物的最大吸收波长位于635 nm,其表观摩尔吸光系数ε=2.62×104 L/(mol·cm),盐酸氯丙嗪质量浓度在0.5~10.0 mg/L范围内与体系的吸光度呈良好的线性关系,线性相关系数为0.999 2。测定结果的相对标准偏差为1.02%~2.65%(n=5),加标回收率为91.0%~95.0%。该法灵敏度较高、选择性及重现性良好,可用于片剂中盐酸氯丙嗪含量的测定。     

FeCl3-铁氰化钾体系分光光度法测定酚磺乙胺

采用铁氰化钾-FeCl3体系分光光度法测定酚磺乙胺。研究表明,酚磺乙胺可使Fe(Ⅲ)还原为Fe(Ⅱ),还原生成的Fe(Ⅱ)可以与K3[Fe(CN)6]反应生成可溶性普鲁士蓝KFe[Fe(CN)6],其最大吸收波长位于710 nm处。酚磺乙胺的质量浓度在0.064～9.6 mg/L范围内与吸光度呈现良好线性关系,线性回归方程A=0.03242+0.08244ρ(mg/L),相关系数r=0.9994,摩尔吸光系数ε=2.17×104L/(mol·cm),检出限0.047 mg/L;相对标准偏差(3.20 mg/L,n=11)为2.4%。方法用于测定药物注射液中酚磺乙胺含量,回收率为98.3%～102.9%。     

邻菲啰啉-Fe(Ⅱ)体系光度法间接测定头孢噻肟钠

基于头孢噻肟钠在0.3 mol/L NaOH溶液中沸水浴降解产物具有还原性,在酸性介质中可将Fe(Ⅲ)还原为Fe(Ⅱ),邻菲罗啉能与所生成的Fe(Ⅱ)显色生成红色络合物,最大吸收波长λ=508 nm;表观摩尔吸光系数ε=1.1×104 L·mol-1·cm-1;头孢噻肟钠在0.4～80 μg/mL范围内呈良好的线性关系;线性回归方程为A=-0.00204 0.01989ρ(μg/mL);线性相关系数r=0.9998;检出限为0.18 μg/mL;RSD为1.2%(5.0 μg/mL,n=11);平均回收率为99%.初步探讨了反应机理,并优化了对头孢噻肟钠的测定条件.     

邻菲哕啉-Fe(Ⅱ)光度法间接测定盐酸吡硫醇

在酸性介质中,盐酸吡硫醇可将Fe(Ⅲ)还原为Fe(Ⅱ),邻菲啰啉能与Fe(Ⅱ)显色,最大吸收波长为508 nm,通过测定Fe(1Ⅰ)的量间接的测定了盐酸吡硫醇的量.建立了测定盐酸吡硫醇质量浓度的新方法.盐酸吡硫醇在0.010～6.0 μg/mL范围内与吸光度呈良好的线性关系,线性回归方程为△A=-0.00373+0.1...     

铁氰化钾-Fe(Ⅲ)体系测定盐酸异丙肾上腺素

本文建立了以铁氰化钾-Fe(Ⅲ)体系测定盐酸异丙肾上腺素的方法。研究表明,在pH 3.0,盐酸异丙肾上腺素可使Fe(Ⅲ)还原为Fe(Ⅱ),生成的Fe(Ⅱ)可以与K_3[Fe(CN)_6]反应生成可溶性普鲁士蓝(KFe~(Ⅲ)[Fe~(Ⅱ)(CN)_6)。盐酸异丙肾上腺素的浓度在0.03~5.00μg·m L~(-1)范围内与吸光度呈现良好线性关系,线性回归方程A=0.017+0.57779C(μg·m L~(-1)),相关系数R=0.9997,检出限为0.025μg·m L~(-1),相对标准偏差R.S.D.=1.05%(n=11),间接测定盐酸异丙肾上腺素的摩尔吸光系数ε=1.4×105L·mol~(-1)·cm~(-1)。本方法成功用于药物制剂和生物样品中盐酸异丙肾上腺素含量的测定,结果满意。     

盐酸氯丙嗪与Fe(Ⅲ)的显色反应及测定

研究了在盐酸介质中,三价铁离子能将盐酸氯丙嗪氧化成一种红色的物质,且氧化的程度与盐酸氯丙嗪的量呈正比关系,据此建立了测定盐酸氯丙嗪的分光光度分析方法。实验中最大吸收波长为530nm,摩尔吸光系数为5.13×103 L/(mol·cm),盐酸氯丙嗪的量在5~250μg/10mL范围内与吸光度A有良好的线性关系,方法用于盐酸氯丙嗪药物的测定,其相对标准偏差为0.11%~0.19%,加标回收率为95.0%~97.0%。     

Spectrophotometric determination of phenylephrine hydrochloride in pharmaceuticals by flow injection analysis exploiting the reaction with potassium ferricyanide and 4-aminoantipyrine

This paper presents a method for the determination of phenylephrine hydrochloride in pharmaceuticals by spectrophotometric flow injection analysis exploiting the reaction with potassium ferricyanide and 4-aminoantipyrine, which leads to the formation of a condensation product with strong absorptivity at 500 nm. The linear dynamic range was between 0.95 and 9 mg/L, with a limit of detection of 0.2 mg/L and a sampling throughput of 120 samples per hour. The method was applied to eyewashes and nasal decongestant liquid medicines.     

多壁碳纳米管修饰电极检测盐酸氯丙嗪的研究

制备了多壁碳纳米管修饰玻碳电极,采用循环伏安法(CV)研究了盐酸氯丙嗪在修饰电极上的电化学特性,发展了一种新的检测盐酸氯丙嗪的电化学分析方法。在最佳实验条件下,用循环伏安法检测盐酸氯丙嗪,其响应电流与盐酸氯丙嗪的浓度在8.0×10-5~1.0×10-3mol/L范围内有很好的线性关系,线性方程为Ip(A)=0.0106c(mol/L)-8×10-8(R2=0.999,n=6),检出限为6.2×10-6mol/L(S/N=3)。方法可用于盐酸氯丙嗪片的测定。     

铬天青S–盐酸氯丙嗪–溴化十六烷基三甲铵光度法测定水样中的铁

采用铁(Ⅲ)–铬天青S–盐酸氯丙嗪–溴化十六烷基三甲铵(CTMAB)四元配合物光度法测定水样中铁的含量。在pH 5.50的HAc–NaAc缓冲介质中,在铁(Ⅲ)–铬天青S–盐酸氯丙嗪显色反应中,加入CTMAB,四元配合物的表观摩尔吸光系数为9.85×10~4 L/(mol·cm),是三元配合物灵敏度的两倍。结果表明,配合物在657nm波长处有最大吸收,Fe(Ⅲ)的质量浓度在0~20μg/(25 mL)范围内与吸光度呈良好的线性关系,线性相关系数为0.999 6,方法的检出限为1.84×10~(–3) mg/L。样品加标回收率为97.3%~98.8%,测定结果的相对标准偏差为1.9%~3.2%(n=5)。该方法灵敏度高,精密度与准确度好,便于在实验室推广应用。     

Determination of Iron(II) in Pharmaceuticals Using Chlorpromazine Hydrochloride as a Redox Indicator

Abstract

Titrimetric method for the determination of (1–100) mg/L iron(II) as pure solutions and in its dosage forms was investigated and found to offer an improvement in ease, speed and accuracy. This method is based on the direct visual titration of iron(II) with ceric amnonium sulphate and employs chlorpromazine hydrochloride in a mixture of sulphuric and phosphoric acids as a redox indicator.

An interference study is carried out for the differant acids and cations. Data obtained for sevceral pharmaceuticals are reported and compared with those obtained potentiometrically. Formal redox potential was determined to be 285 mv.     

衍生化-离子液体萃取分光光度法测定盐酸美西律

盐酸美西律与1,2-萘醌-4-磺酸钠在pH=9.0的介质中反应生成一种橙红色衍生物,该衍生物能被离子液体所萃取,其最大吸收波长发生较大幅度红移,吸光度显著增强。据此建立了高选择性的测定盐酸美西律的衍生化-离子液体萃取分光光度法。萃取后的衍生物在448 nm处的表观摩尔吸光系数ε为2.69×104L·mol-1·cm-1。盐酸美西律浓度在0.2～5.4μg·mL-1范围内符合比耳定律,相关系数为0.9994,检出限为0.067μg·mL-1。该方法已用于药物制剂及尿样中盐酸美西律的测定,其回收率分别为99.5%～100.7%和96.6%～101.5%。     

Sensitive determination of phenothiazines in pharmaceutical preparation and biological fluid by flow injection chemiluminescence method using luminol-KMnO4 system

A flow injection chemiluminescence method was described for the determination of four phenothiazine drugs, namely, chlorpromazine hydrochloride, perphenazine hydrochloride, fluphenazine hydrochloride and thioridazine hydrochloride. Strong Chemiluminescence (CL) signal was produced when above-mentioned drug was injected into the mixed stream of luminol with KMnO₄. The linear ranges of the method were 0.0020-1.0 μg/mL chlorpromazine hydrochloride, 0.0040-3.0 μg/mL perphenazine hydrochloride, 0.0020-5.0 μg/mL fluphenazine hydrochloride and 0.0050-1.0 μg/mL thioridazine hydrochloride. The detection limits were 0.4 ng/mL chlorpromazine hydrochloride, 0.7 ng/mL perphenazine hydrochloride, 2 ng/mL fluphenazine hydrochloride and 0.7 ng/mL thioridazine hydrochloride. The proposed method was applied to the determination of chlorpromazine hydrochloride in injections and in mental patient's urine samples and the satisfactory results were achieved. The possible CL reaction mechanism was also discussed briefly.     

A New Extraction Spectrophotometric Method for the Determination of Phenol in Water

The product of the reaction among phenol, sodium nitroprusside and hydroxylamine hydrochloride in an alkaline solution can be extracted by chloroform in the presence of cetylpyridinium bromide(CPB), on the basis of which a new extraction spectrophotometric method for the determination of phenol in water is developed. The optimum determination wavelength is 720 nm. The molar absorptivity is 1.05×105 mol-1·L·cm-1 and the detection limit is 4.0 μg/L. For 30.0 and 60.0 μg/L standard solutions, the relative standard deviations are 4.5% and 2.2%, respectively(n=6). F values of the statistical analysis show that there is no notable difference between the proposed method and 4-AAP method. The results of the standard addition method for the natural water samples are satisfactory.     

测定抗坏血酸的亚甲蓝褪色光度法

确定了亚甲蓝与抗坏血酸褪色反应的最佳条件,在 pH=2的缓冲溶液和对氨基苯磺酸存在的条件下,抗坏血酸能够很快还原亚甲蓝并使之褪色,褪色反应的体系具有很好的稳定性。该反应的摩尔吸光系数为 2.0× 103 L· mol－ 1· cm－ 1,线性范围 0.4～ 40.0 mg/L。该法具有优良的选择性,常见的能够与抗坏血酸共存的阴、阳离子和还原剂、表面活性剂不干扰测定,应用于药品、饮料、蔬菜中抗坏血酸的测定,获得满意结果。     

Sequential injection technique for the determination of chlorpromazine hydrochloride in pure form and pharmaceutical formulations

A simple, economical, and automated spectrophotometric method for the determination of chlorpromazine hydrochloride by sequential injection analysis using ammonium metavanadate as colorimetric reagent is proposed. The various chemical and physical conditions that affected the reaction have been thoroughly investigated. The calibration curve was linear within the range 10–100 μg/mL. The detection limit (S/N = 3) was 0.7 μg/mL and the limit of quantification (S/N = 10) was 2.3 μg/mL. The sampling frequency was 22 h⁻¹. The method has been used for the determination of chlorpromazine hydrochloride in pure form and pharmaceutical formulations. The t-test has revealed that there is no evidence of significant differences between the obtained results at the 95% confidence level. The method can be applied to the quantitative determination of chlorpromazine hydrochloride. It is also applicable in the quality control of chlorpromazine hydrochloride preparations. The text was submitted by the authors in English.