硝普钠显色测定药物样品中甲巯咪唑

在溶液中NaOH浓度为6.7×10-3mol/L及0℃(冰水浴)条件下,反应时间为30 min,硝普钠与甲巯咪唑生成化学计量比为1碱性条件下硝普钠与甲巯咪唑反应生成化学计量比为1∶1的绿色产物,其最大吸收波长为610 nm。甲巯咪唑在4.8~48 mg/L浓度范围内与吸光度呈良好线性关系,线性回归方程为A=-0.0617 0.01329C(mg/L),相关系数r=0.9991;检出限为0.47 mg/L;相对标准偏差RSD=0.2%。本法成功用于测定片剂药品中甲巯咪唑的含量,平均回收率大于97.2%。     

A Novel Visible Spectrophotometric Method for the Determination of Methanol Using Sodium Nitroprusside as Spectroscopic Probe

A novel, rapid and reliable method has been established for the determination of methanol using sodium nitroprusside as a spectroscopic probe. This method indicates that the sodium nitroprusside can react with the methanol to form a colored product in the basic solution. The absorbance of the product is measured at the maximal absorption wavelength of 481 nm, and the amount of methanol can be calculated based on this absorbance. A good linear relationship of the concentration of methanol versus absorbance is observed with a linear range of 0.02‐6.0 mg mL^?1. The linear regression equation is A = 0.02484 + 0.29457C (mg mL^?1), with a correlation coefficient of 0.9991. The detection limit (3σ/k) is 0.012 mg mL^?1, while its R.S.D. is 1.5% and the recovery rate is 97.5‐102.5%. The parameters with regard to determination are optimized, and the reaction mechanism is discussed. This method has been successfully applied to determine methanol in variety of samples. Analytical results obtained by this new method were very gratifying.     

硝普钠分光光度法测定头孢他啶

建立了硝普钠分光光度法测定头孢他啶的方法。实验结果表明,在碱性条件下,头孢他啶与硝普钠以1∶2的化学计量比反应形成一种红褐色产物,其最大吸收波长为528 nm。 头孢他啶在2.50~810 mg/L浓度范围内与吸光度呈良好线性关系,线性回归方程为A=0.02704+0.00218ρ(mg/L),线性相关系数r＝0.9987,表观摩尔吸收系数ε528=1.2×103 L/(mol·cm),检测限(3σ/k)为1.38 mg/L。 本方法操作简便、快速,成功用于药品中头孢他啶含量的测定。     

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。     

Rapid and Convenient Method for the Determination of Sodium Nitroprusside in Aqueous Solution

Abstract

We propose a rapid and convenient method for the determination of sodium nitroprusside in aqueous solution. In alkaline medium and in the presence of dimethylsulfoxide, the concentration of the nitrite ions coming from the nitroprusside corresponds with the initial quantity of this compound.     

A Simple Sensitive Spectrophotometric Method for the Determination of Ce4+ Using Variamine Blue as a Chromogenic Reagent

A rapid and sensitive spectrophotometric method is described for the determination of trace amounts of cerium using Variamine Blue (VB) as a chromogenic reagent. The proposed method is based on the reaction of cerium with potassium iodide in acidic medium to liberate iodine, which oxidizes Variamine Blue to give a violet colored species with an absorption maximum at 560nm. Beers law was obeyed in the range 2–10µg mL^–1 of cerium. The molar absorptivity and Sandells sensitivity are found to be 1.65×10⁴L mol^–1cm^–1 and 8.48×10^–3µgcm^–2, respectively. The proposed method has been successfully applied to the determination of cerium in alloy and synthetic mixtures.     

在丙酮增敏作用下硝普钠分光光度法测定盐酸吗啉胍

摘要：建立了可见分光光度法测定盐酸吗啉胍的新方法。研究表明,当NaOH浓度为0.13mol/L,在丙酮存在下硝普钠与盐酸吗啉胍反应生成紫色N-亚硝基类化合物,其最大吸收波长为508nm,表观摩尔吸光系数2.5×10³ L/（mol•cm）。盐酸吗啉胍浓度在0.38×10^-6~3.0×10^-4 g/mL范围内与吸光度呈现良好线性关系,线性回归方程A = 0.02292 + 0.01213c (10^-6 g/mL),线性相关系数r=0.9998,检测限(3σ/k)为0.25×10^-6 g/mL,RSD = 0.21%。本方法可用于药物样品和血清中盐酸吗啉胍含量的测定。     

茚三酮为显色剂分光光度法测定氨苄西林钠

采用分光光度法研究了氨苄西林钠与茚三酮间的显色反应。 确定了反应条件,建立了一种快速、简便测定氨苄西林钠的分光光度法。 实验表明,氨苄西林钠与茚三酮在pH=5.4的水溶液中,沸水浴1 h可以反应完全,产物在λmax=564 nm下,表观摩尔吸光系数为3.72×103 L/(mol·cm)。 氨苄西林钠质量浓度在10~90 mg/L范围内服从比耳定律, 相关系数为0.9981,当氨苄西林钠浓度为40 mg/L时,测定结果的相对标准偏差为1.5%(n=6),回收率在99.0%以上。     

Spectrophotometric Determination of Hydroxylamine,Glycine and Methionine by Using Sodium Nitroprusside as a Complexing Agent

Abstract

The spectrophotometric determination of hydroxylamine, glycine and methionine has been investigated. The high molar absorptivity of the investigated amino acids or hydroxylamine-nitroprusside complexes at the optimum conditions indicates that concentrations of 10^?4?10^?3 M of these compounds can be determined spectrophotometrically with fair accuracy. The effect of pH was studied and the optimum pH was chosen to give the highest sensitivity. The validity of this method is supported by the constancy of the absorptivity of the investigated compounds and the statistical data of regression analysis.     

食品中甜蜜素的紫外分光光度法测定

采用紫外分光光度法测定食品中的甜蜜素。该法在０．２～１．０ｇ／Ｌ甜蜜素范围内符合比尔定律,回收率为９５．０％～１０２．７％,相对标准偏差（ＲＳＤ）为２．６６％～５．４０％,食品中共存的苯甲酸、山梨酸、糖精钠在０～１０．０ｇ／Ｌ范围内,色 ０～２．０ｇ／Ｌ范围内不影响测定。方法简捷,准确。     

紫外分光光度法间接测定果冻中甜蜜素

提出了紫外分光光度法间接测定食品中甜蜜素的方法。考察了酸性介质的种类,亚硝酸钠与碘化钾浓度、用量及反应时间对测定的影响。在优化的试验条件下,甜蜜素在1.0～14.0mg·mL-1范围内遵守比耳定律,检出限(3S/N)为0.3mg·mL-1。用此方法测定果冻中甜蜜素含量,加标回收率为102.6%～103.3%,相对标准偏差(n=5)为0.7%～1.3%。     

Assay of Phenformin Hydrochloride in Pharmaceutics by Coupling with Sodium Nitroprusside

A novel and simple spectrophotometric method for the determination of phenformin hydrochloride using sodium nitroprusside as chromogenic reagent is developed in this paper. The experiment indicates that the sodium nitroprusside can react with the phenformin hydrochloride in a basic solution to form a product with colored N‐nitrosamines. The stoichiometric ratio of phenformin hydrochloride and sodium nitroprusside is 1:3 in the product. The maximal absorption wavelength (λ_max) of the product is 520 nm, ?₅₂₀ = 2.2 × 10³ Lmol^?1cm^?1. A Good linear relationship is obtained between the absorbance (A) and the concentration (C) of phenformin hydrochloride in a wide range of 0.20‐400 μg mL^?1. The equation of the linear regression is A = 0.03461 + 0.00907C (μg mL^?1) with a linear correlation coefficient of 0.9991. The detection limit is 0.13 μg mL^?1, and the relative standard deviation (R.S.D.) is 0.19%. The method is successfully applied to the determination of phenformin hydrochloride in tablet forms, and satisfactory recoveries are obtained.     

醌茜素显色分光光度法测定奋乃静

研究了奋乃静(Perphenazine,PPH)与醌茜素(Quinalizarin,QLZ)之间的荷移光谱及其性能。奋乃静作为电子给体,醌茜素作为电子受体,两者在乙醇-水介质中反应生成荷移络合物。该络合物的λmax=568nm,表观摩尔吸光系数是3.39×103 L.mol-1.cm-1,奋乃静药物质量浓度在0～35mg/L范围内服从比耳定律,相对标准偏差为1.23%(n=6),回收率为98.9%～102.4%。     

亚硝基铁氰化钠分光光度法测定药品“必理通”中对乙酰氨基酚含量

用亚硝基铁氰化钠分光光度法测定药品“必理通”中的对乙酰氨基酚含量。采用亚硝基铁氰化钠试液为显色剂,蒸馏水做溶剂,在波长为700nm下有最大吸收,利用分光光度计测定不同浓度溶液的吸光度,并绘制标准曲线进行分析。实验证明,对乙酰氨基酚在0．024mg／mL～0．168mg／mL浓度范围内,吸光度与样品浓度的线性关系良好,回收率在98．0％以上。此测定方法准确、快速、简便,是测定对乙酰氨基酚含量的最佳方法之一。     

Direct Sensitive Spectrophotometric Determination of Glyphosate by Using Ninhydrin as a Chromogenic Reagent in Formulations and Environmental Water Samples

A simple, sensitive, and rapid spectrophotometric method for the assay of glyphosate (= N‐(phosphonomethyl)glycine) in various formulations (Roundup, Excel Mera 71) and environmental water samples is described. The method is based on the reaction of glyphosate with ninhydrin in presence of sodium molybdate in neutral aqueous medium at 100° to give a Ruhemann's purple product having the VIS absorption maximum at 570 nm (Scheme, Fig. 1). The product is stable for 10 h. Beer's law is obeyed in the concentration range of 0.1–3.5 μg ml^?1. The molar absorptivity and Sandell's sensitivity are 3.2816 ? 10⁴ l mol^?1 cm^?1 and 5.2 ng cm^?2, respectively (Table 1). The method is highly reproducible, as confirmed by the relative‐standard‐deviation (r.s.d.) values (1.70%; Table 2). Recovery studies establish that this method is accurate (Table 5) and can be successfully employed for the determination of glyphosate.     

超高灵敏卟啉试剂导数分光光度法直接测定矿样中的痕量铜

用ｍｅｓｏ－四－（对－三甲铵苯基）卟啉作显色剂，以四阶导数光谱技术进行测定，提出了测量痕量铜的新方法。在ｐＨ４．４的ＨＡｃ－ＮａＡｃ介质中，在盐酸羟胺催化和乙醇增稳增敏作用下，于沸水浴中加热１ｍｉｎ，显色反应即呆完成。其四阶导数光谱表观摩尔吸光系数ε＇达１．００×１０＾７Ｌ·ｍｏｌ＾－１·ｃｍ＾－１，最低检出限为０．０６２μｇ／Ｌ，分别是常规光度法的２１．２和１２．３倍。同时，绝大多数离子不干扰测     

1,2-萘醌-4-磺酸钠体系分光光度法测定磺胺甲噁唑

采用1,2-萘醌-4-磺酸钠体系分光光度法测定磺胺甲噁唑(SMZ)。磺胺甲噁唑与1,2-萘醌-4-磺酸钠在pH=10.0的缓冲溶液中发生亲核取代反应生成橙红色的产物,组成比为1:1,最大吸收波长λ=476 nm;表观摩尔吸光系数ε=6.44×103L/(mol.cm);SMZ浓度在0.2~60 mg/L范围内呈良好的线性关系;线性回归方程为A=0.02452 0.02301C(mg/L),线性相关系数r=0.9991;检出限为0.08 mg/L;RSD为0.25%(20 mg/L,n=11);平均回收率为98.7%以上。优化了对磺胺甲噁唑的测定条件。初步探讨了反应机理,应用拟定的方法测定磺胺甲噁唑的含量,与药典法相比,结果满意。     

光谱法测定复方双氯灭痛注射液含量

本实验对复方双氯灭痛注射液中扑热息痛和双氯灭痛两种主要成分分别采用双波长紫外分光光度法及紫外差示分光光度法进行含量测定。可在不用分离的情况下连续测定两种成分的含量。实验结果:扑热息痛的直线回归方程C=31.34A+0.078,R=0.9999,回收率100.69%,CV%=0.91。双氯灭痛的直线回归方程C=24.94A—0.202,R=0.9997,回收率为100.91%,CV%=0.77。本法具有方法简便,结果准确,重现性好,实用等优点。     

二乙基二硫代氨基甲酸钠流动注射萃取分光光度法测定矿石中微量铜的研究

本文对二乙基二硫代氨基甲酸钠(铜试剂)-四氯化碳流动注射莘取分光光度法测定矿石中微量铜进行了研究。与手工萃取法相比,本法最大特点是大量Mn~(2+)无干扰。方法操作简便、快速、可靠、毒性小;进样频率为20次/小时,RSD为3.5％。线性范围为O～1.28μg/ml。方法用于测定矿石中微量铜,结果满意。     

Spectrophotometric Study and Potentiometric Titration between Sulphite and Nitrite Ions Using Acktaldehyde Complex of Nitroprusside as a Carrier

Abstract

A complex between sodium nitroprusside (NP) and acetaldehyde of 1:1 in aqueous solution of pH 10 has been prepared and used as an analytical reagent for the spectrophotometric determination of sulphite and nitrite ions. Nitrite ion can be titrated against sulphite ion and vise versa in equivalent amounts with high accuracy in the presence of the acetaldehyde complex of nitroprusside as a carrier using a potentiometric titration technique.