盐酸氯丙嗪显色-分光光度法快速测定食盐中的碘含量

研究了在硫酸介质中,IO3-能与盐酸氯丙嗪发生氧化显色反应,且显色的程度和IO3-的量成正比例关系,据此建立了分光光度法测定食盐中碘含量的分析方法。显色物质的最大吸收波长为526nm,线性回归方程为y=1.214x+0.011 8,相关系数为0.998 9,表观摩尔吸光系数为5.2×104 L/(mol·cm),碘浓度在0~24μg/10mL范围内有良好的线性关系,相对标准偏差为1.2%~2.2%,加标回收率为97.5%~102.0%,实验表明,方法操作简单,灵敏度高、选择性好,适用于食盐中碘含量的测定。     

紫尿酸–Fe(Ⅲ)分光光度法测定盐酸羟胺

在碱性介质及溴化十六烷基吡啶存在条件下,盐酸羟胺与Fe(Ⅲ)–紫尿酸体系发生显色反应形成离子缔合物,该离子缔合物在635 nm波长处有一个吸收峰,其表观摩尔吸光系数ε=2.05×104 L/(mol·cm),据此建立了测定盐酸羟胺的间接分光光度法。盐酸羟胺的质量浓度在0~2.4 mg/L范围内与吸光度与呈良好的线性,线性相关系数r=0.999 8,方法的检出限为0.01 mg/L。将该方法用于盐酸羟胺的测定,其测定结果与国标法测定结果相吻合,加标回收率为95.0%~104.0%,测定结果的相对标准偏差为0.51%~1.29%(n=5)。该方法灵敏度高,操作简便,可用于盐酸羟胺含量测定。     

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。     

钒酸铵氧化-分光光度法测定盐酸氯丙嗪

在磷酸介质中,钒酸铵与盐酸氯丙嗪反应生成红色氧化产物,其最大吸收波长为524nm;据此建立了测定盐酸氯丙嗪含量的钒酸铵氧化-分光光度法,并将其用于直接测定药物制剂中的盐酸氯丙嗪.结果表明,当盐酸氯丙嗪的浓度处于10.0～100mg/L和100～360mg/L范围内时,被测定体系的吸光度与盐酸氯丙嗪的浓度之间呈良好的线性关系;线性回归方程分别为A=-0.061 69+0.010 05c(mg/L,r=0.998 8)、A=0.494+0.004 43c(mg/L,r=0.998 8),检出限为1.96mg/L,相对标准偏差为0.29%,回收率为94.9%～102.9%.     

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%.     

邻二氮菲分光光度法测定盐酸氯丙嗪

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0.040～15.00 mg/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=2.8×104 L.mol-1.cm-1,检出限为0.020 mg/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。     

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%。     

荧光分光光度法直接测定盐酸异丙嗪片剂及注射液的含量

以０．０００１ｍｏｌ／Ｌ盐酸的溶剂,３０３ｎｍ为激发波和ｎｍ为发射波和散荧光分光光度法直接测定盐酸异丙嗪片剂及注射液中盐酸异丙嗪的含量。盐酸异丙嗪在０．１～１０．０μｇ／ｍＬ浓度范围呈良好线性。片剂及注射液的测定平均变异系数分别为０．３１％和０．４５％,回收率分别为９９．９％和９９．６％。     

结晶紫分光光度法测定蛋白质的含量

在pH=4.0的Tris-HC l缓冲溶液中,结晶紫与蛋白质结合形成稳定的深红色配合物,该配合物的最大吸收波长为575 nm,表观摩尔吸光系数为3.25×105L/(mol.cm),蛋白质含量在0.0~80.0μg/mL范围内服从朗伯比耳定律,检出限为6.47μg/mL,回收率为97%~101%。将该法用于豆浆、牛奶等总蛋白质含量的测定,测定结果与凯氏法测定结果基本一致。     

紫尿酸光度法同时测定铁和钴

利用铁、钴配阴离子在365nm处的吸光度具有良好的加和性,建立了同时测定铁、钴的紫尿酸光度法。铁,钴量均在0～50.0μg/29ml范围内符合比耳定律。方法用于自来水中铁、钴的同时测定,结果分别与邻菲罗啉光度法和亚硝基R盐光度法一致,回收率分别为96％～102％和98％～104％。     

共振瑞利散射光谱法对盐酸异丙嗪与盐酸氯丙嗪的同时测定

钼酸铵(AM)与盐酸氯丙嗪(CPZ)及盐酸异丙嗪(PZ)均能反应形成离子缔合物,引起共振瑞利散射(RRS)的显著增强,并出现新RRS光谱.2种反应产物具有相似的RRS光谱特征,其最大散射峰均在365 nm处,且在一定范围内散射增强(Δ_(IRRS))与药物的质量浓度成正比,但RRS强度随药物质量浓度的线性增幅存在显著差异.结合两组分RRS光谱强度的加和性,可建立双组分信号响应的两条同原射线的计量分析法.方法对CPZ 和PZ的检出限分别为4.5、7.7 μg/L,线性范围均为0.03～2.4 mg/L.将该方法用于血清、尿样和非那根止咳糖浆中CPZ和PZ的同时测定,取得满意结果.     

The Use of Internal Standard Method for Dertvative-Spectrophotometric Determination of Chlorpromazine Hydrochloride

ABSTRACT

The use of 1, 10-phenantroline as internal standard (IS) is proposed for spectrophotometric determination of chlorpromazine hydrochloride in pharmaceutical formulations. The spectra of both compounds: analyte and internal standard are partially overlapped, so the Savitzky-Golay alghoritm was used to obtain separated signals of analyte and IS. The best parameters to generate the second-derivative spectra were: ∠λ = 10 nm (5 experimental points) and second polynomial degree. For quantification of chlorpromazine in pharmaceuticals, the zero-crossing technique was used. The values of the second-derivative peaks were measured for chlorpromazine at 256 nm and at 236 nm for IS. Analytical characteristic for proposed method was evaluated (r²=0.9990, detection limit=3.97 ng/ml). The obtained analytical results were in good agreement with results obtained using the UV-spectrophotometric Blazek method.     

A Novel Method for the Determination of Streptomycin Using Sodium Nitroprusside as a Chromogenic Reagent by Spectrophotometry

Abstract

A rapid and simple spectrophotometric method for the determination of streptomycin has been developed and validated. The method was based on the reaction of streptomycin with sodium nitroprusside in the alkaline medium forming a red product measured at the maximum absorption of 495 nm. The stoichiometric ratio of the product is 1:1. Beer's law is obeyed in a range of 1.87 µg mL^?1 ～ 279.8 µg mL^?1 of streptomycin and ?₄₉₅ is 6.0 × 10³ L·mol^?1 cm^?1.Under the optimum condition, the equation of linear regression is A = 0.00742 + 0.05683 C (× 10⁵ mol·L^?1), with a linear correlation coefficient of 0.9990. The detection limit (3σ/k) is 0.96 µg mL^?1, the relative standard deviation (RSD) is 2.40%, and the average recovery rate is 98.3%–102.7%. Every parameter has been optimized, and the reaction mechanism has been studied. The proposed method has been successfully applied to the determination of streptomycin for injections and tablets of pharmaceutical preparation. Analytical results obtained by this new method were very gratifying.     

稳定回归法用于复方氯丙嗪片的测定

本文应用稳定回归法用于紫外重叠光谱的分析。以复方氯丙嗪为例,不经分离,测定了盐酸氯丙嗪和盐酸异丙嗪的含量。与最小二乘回归法比较,提高了测定结果的准确度和精密度。结果满意。     

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.     

Spectrophotometric Determination of Chlorpromazine and Levomepromazine Hydrochlorides In Injectables and Drops By Reaction With Ferric Ion

Abstract

The principal aim of this research was the standardization of a spectrophotometric method using the reaction with ferric ion for quantitative determination of these substances in pharmaceutical preparations. By reaction with ferric ion chlorpromazine gave a pink compound with maximum absorption at 525 nm. the violet product obtained by the reaction with ferric ion and levomepromazine had a maximum at 565 nm. Beer's law was obeyed in a wide range of concentrations for both compounds. the method was applied to simulated and commercially available samples. the efficiency of the method was confirmed by recovery tests.     

紫外分光光度法同时测定面粉中过氧化苯甲酰及其还原产物苯甲酸的含量

建立了一种测定面粉中过氧化苯甲酰及其还原产物苯甲酸含量的紫外分光光度法。采用无水乙醇作参比,在同一样品溶液中分别于233 nm和226 nm处同时测定过氧化苯甲酰及其还原产物苯甲酸的含量,由于两组分同时测定时相互影响,通过建立线性方程组的方法消除被测组分间的相互干扰,过氧化苯甲酰在8.26×10-6~4.95×10-6mol/L和苯甲酸在1.64×10-5~9.84×10-5mol/L范围内服从比耳定律。该法操作简便、快速,不经提取分离同时测定面粉中过氧化苯甲酰及其还原产物苯甲酸含量获得了较满意的结果。     

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。