Rapid and Simple Method for Simultaneous Determination of Escin and Diethylamine Salicylate in Pharmaceutical Preparations by Partial Least-Squares Multivariate Calibration

A partial least-squares calibration (PLS) method has been developed for simultaneous quantitative determination of escin (ES) and diethylamine salicylate (DAS) in pharmaceutical preparations. The resolution of these mixtures has been accomplished without prior separation or derivatisation, by using partial least-squares (PLS-2) regression analysis of electronic absorption spectral data. The experimental calibration matrix was constructed with 9 samples. The concentration ranges considered were 10, 20, 30 (ES) and 40, 50, 60 (DAS) μg cm⁻³. The absorbances were recorded between 200 and 325 nm every 5 nm. Proposed method was compared with conventional spectrophotometric method. The results show that PLS-2 is a simple, rapid, and accurate method applied to the determination of these compounds in pharmaceuticals.     

多元校正-光度法同时测定食品中的香兰素和乙基麦芽酚

香兰素、乙基麦芽酚在紫外区均有吸收,其吸收光谱严重重叠。在pH=2．87的B-R缓冲溶液中对香兰素和乙基麦芽酚两组分混合溶液进行光度测定,所得重叠光谱数据分别用经典最小二乘法(CLS)、偏最小二乘法(PLS)、主成分回归法(PCR)处理,并用于食品样品的测定,获得了较好的定量分析结果。香兰素和乙基麦芽酚的线性范围均为1．0～20．0mg／L;检出限分别为0．478mg／L和0．559mg／L。     

Simultaneous Determination of Theobromine and Caffeine in Cocoa by Partial Least-Squares Multivariate Spectrophotometric Calibration

Abstract

The use of partial least - squares multivariate spectrophotometric calibration for the simultaneous determination of theobromine and caffeine in cocoa is presented. The results show that these components in a molar ratio of about 6 : 1 in cocoa have been determined simultaneously with standard deviations of about 0.05 and 0.02 for theobromine and caffeine, respectively.     

多元校正分光光度法同时测定兔血清内的氨甲苯酸和酚磺乙胺

氨甲苯酸和酚磺乙胺在紫外区均有吸收,但吸收光谱重叠而形成干扰,较难直接进行分析。本文采用紫外分光光度法对氨甲苯酸和酚磺乙胺两组分混合溶液进行测定,并将所得光谱数据用化学计量学多元校正方法处理。本法测定氨甲苯酸和酚磺乙胺的的线性范围均为2.0~20.0μg/mL。用拟定的方法测定了兔血清中的氨甲苯酸和酚磺乙胺,并与高效液相色谱法的结果进行了比较,两者无显著性差异。     

Simultaneous Determination of Anthocyanin and Ponceau 4R in Drink Powders by Derivative Spectrophotometry and Partial Least-Squares Multivariate Spectrophotometric Calibration

Summary.  Two methods for the simultaneous determination of anthocyanin and ponceau 4R in drink powders by second derivative spectrophotometry and by partial least-squares multivariate spectrophotometric calibration are described. The procedures do not require any separation step. The methods were applied to determine both colorants in commercial gelatin powders; the results obtained are compared. Received September 7, 2000. Accepted (revised) November 20, 2000     

Carbon‐based Nanosensors for Salicylate Determination in Pharmaceutical Preparations

Thiourea derivative‐based carbon paste electrode (TUD1‐CPE) was constructed as a potentiometric sensor for the determination of salicylate anion in pharmaceutical formulations, Aspocid® and Aspirin®. The optimized CPE contained 45.5 % graphite, 0.5 % reduced graphene oxide (rGO), 46.0 % nitrophenyl octyl ether (NPOE) plasticizer, 5.0 % TUD1 ionophore, and 3.0 % tridodecylmethyl ammonium chloride as additive. The incorporation of NPOE of high dielectric constant, and rGO in electrode caused better performance of the sensor; Nernstian response of 59.0 mV decade^?1 in the concentration range of 10^?1–10^?5 mole L^?1, a detection limit of 1×10^?5 mole L^?1 in a very short response time of 6 seconds. The prepared sensor showed high selectivity against similar anions (i. e. , benzoate, I^?, SCN^?). Selectivity was confirmed by calculating the formation constant (K_β) using sandwich membrane method, where K_β for TUD1‐salicylate is 10^0.43. Theoretical calculations at DFT‐B3LY/6‐31G** level of theory were performed to find interaction mechanism, Energies of HOMO and LUMO orbitals, non‐linear optical (NLO) properties (the electronic dipole moment (μ), first‐order hyperpolarizability (β), the hyper‐Rayleigh scattering (β_HRS) and the depolarization ratio (DR)), and other global properties; these calculations showed lower values of β and DR, higher value of β_HRS, and the shortest lengths of the four N?H bonds between TUD1 and salicylate which confirm their strong complexation and salicylate‐selectivity. Also, all the studied anion‐TUD1 exhibited relatively high NLO properties, and these results were considered as a preliminary study for investigating new types of NLO bearing materials. The sensors were applied successfully for the determination of salicylate anion in Aspocid® and Aspirin®.     

Simultaneous Determination of Acetaminophen and Phenobarbital in Suppositories by Partial Least-Squares Spectrophotometric Calibration

Abstract

The use of partial least-squares spectrophotometric calibration for the simultaneous determination of suppositories in a multicomponent formulation is presented. This method is applied to the deternination of acetaminophen and phenobarbital in suppository preparations. The results show that these components in a molar ratio of about 61:1 in suppositories have been determined simultaneously with high precision.     

校正变换矩阵法及其在多组分直接同时测定中的应用

将目标变换因子分析中自由浮动技术引入多元校准中，提出了一种新的多组分同时校准法———校正变换矩阵法。该法用于四组分氨基酸人工混合样品分析，结果令人满意，通过与传统目标变换因子分析法比较研究，表明该法用于组分光谱严重共线的波长范围时，其校准能力大大优于传统目标变换法。     

Simultaneous Determination of Quercetin and Luteolin in Dried Flowers by Multivariate HPLC-ECD Calibration

Two calibration models, partial least squares (PLS) and principal component regression (PCR), were applied to the simultaneous determination of quercetin and luteolin by high performance liquid chromatography (HPLC) with electrochemical detection (ECD). The proposed methods were successfully applied to the analysis of dried flower samples. It was found that the relative standard errors of prediction (RSEP) for the validation set of PLS of quercetin and luteolin was 1.31 and 2.23%, and the RSEP of PCR was found to be 3.56 and 4.32%, respectively. Several dried flower samples were analysed and the recoveries were in the range of 95.9–103.3%.     

A Partial Least-Squares Multivariate Calibration Method for the Simultaneous Spectrophotometric Determination of Spironolactone,Canrenone and Hydrochlorothiazide

Abstract

An application of a partial least squares calibration method for the simultaneous spectrophotometric determination of spironolactone, canrenone and hydrochlorothiazide is suggested. The use of the PLS for the multicomponent spectrophotometric determination is demonstrated on the analysis of several synthetic mixtures. It was shown that is possible to resolve complex mixtures of     

Simultaneous Determination of Sunset Yellow and Ponceau 4R in Gelatin Powder by Derivative Spectrophotometry and Partial Least-Squares Multivariate Spectrophotometric Calibration

ABSTRACT

Two methods for the simultaneous determination of Sunset Yellow and Ponceau 4R in gelatin powders by first derivative spectrophotometry and by partial least-squares multivariate spectrophotometric calibration are described. These procedures do not require any separation step. These methods were applied to determine both colorants in commercial gelatin powders and the results obtained were compared. A good statistical agreement was obtained between the results.     

多变量校正方法在电分析化学多组分同时测定中的应用

评述了多变量校正方法在电分析化学中的应用进展,着重介绍了多变量校正方法的原理及其在电分析化学多组分同时测定中的应用。     

多元校正-速差动力学分光光度法同时测定三组分有机磷农药

速差动力学分析结合化学计量学对动力学数据进行解析计算, 可扩大动力学分析的范围, 提高分析的准确度. 本文利用对硫磷、甲基对硫磷和杀螟硫磷在碱性介质中能与氧化剂过氧化氢发生氧化反应生成对硝基苯酚的性质, 引入多元校正方法中的经典最小二乘法(CLS)、偏最小二乘法(PLS)和主成分回归法(PCR)对动力学数据进行解析, 实现了三组分人工合成样品的同时测定.     

多元校正紫外光度法同时测定甲硝唑与维生素B6

本文报道多元校正紫外光度法同时测定甲硝唑和维生素B6。首先在0．1mol／LHCl溶液中对甲硝唑和维生素B6两组分混合溶液进行分光光度法测定,然后将所得的重叠光谱数据经计算机采集后,分别用化学计量学方法中的偏最小二乘法（PLS）和主成分回归法（PCR）进行处理,并用于药物样品的测定,获得了较好的定量分析结果。该法甲硝唑和维生素B6的线性范围分别为1．0～28．0mg／L和1．0～28．0mg／L,检出限分别为0．568mg／L和0．364mg／L。     

Simultaneous Polarographic Determination of Lead (II) and TIN (II) by Multivariate Calibration

ABSTRACT

The polarographic waves of lead (II) and tin (II) overlap due to their similar reductive potentials and it is difficult to determine these two components simultaneously without a pre-separation. In this paper, differential pulse polarography (DPP) combined with multivariate calibration approaches, such as classical least squares (CLS), principal component regression (PCR) and partial least squares (PLS), were successfully applied to the resolution of overlapping polarographic waves of these two components in the concentration range of 0.05-3.50 mg 1^?1. Satisfactory quantitative results were obtained.     

Simultaneous Spectrophotometric Determination of Hydrochlorothiazide and Pharmaceutical Preparations

Abstract

We developed three methods for the simultaneous determination of amiloride (AMI) and hydrochlorothiazide (HCT): zero-crossing, derivative quotient spectra with normalized divisor and multiple linear regression (MULTIC) methods. The two first methods use the derivative spectrophotometry, and the last one uses the absorbance measurement. The three methods were used to determine both compounds in synthetic mixtures and pharmaceutical preparations with errors less than 5% and 15%, respectively.     

多元校正滴定法测定酒石酸美托洛尔

以氢离子选择性电极为工作电极,盐酸或氢氧化钠为滴定剂,用多元校正滴定法对酒石酸美托洛尔片的含量进行了测定。探讨了盐酸或氢氧化钠测定酒石酸美托洛尔的可行性,比较了过滤和不过滤两种方法配制试液的测定结果。本法测定结果与中国药典(1995)中非水滴定法的对照偏差在1%之内;采用过滤和不过滤两种方法配制的试液测定结果之间的偏差在0.2%之内。     

Simultaneous Spectrophotometric Determination of Rare-Earth and Transition Elements Using Partial Least-Squares (PLS) Multivariate Calibration

A spectrophotometric method for the simultaneous determination of rare-earth and transition elements in synthetic superconductors, [(La_{1 – x} Eu _x )_1.82Sr_0.18CuO₄], by the use of 2-(5-bromo-2-pyridylazo)-5-diethylaminophenol (5-Br-PADAP) as chelating agent was developed. The influence of chemical variables affecting the reaction was studied. A partial least-squares (PLS) multivariate calibration procedure was used to assess the data obtained from several calibration solutions measured over the wavelengths range 400–700 nm. The concentration range for Cu was (1–12) × 10^–6 mol/L, while the range for the rare-earth elements La and Eu was (2–8) × 10^–6 mol/L. The relative errors in the determinations were less than 5% in most cases.     

Determination of Boanmycin in Pharmaceutical Preparations by a Simple and Rapid Ion-pair LC Method

An ion-pair HPLC method with UV detection is described for the determination of boanmycin in freeze-dried pharmaceutical preparations. Chromatographic separation was achieved on a 5 μm Agilent Eclipse XDB-C₁₈ column (150 × 4.6 mm). The mobile phase contained methanol, acetonitrile, 055 M sodium hexanesulfonate and 0.08 M acetic acid in water. UV detection was at 291 nm. The assay was validated over a linear concentration range from 0.05 to 120 μg mL^?1. The method was applied to determine the content of BAM in freeze-dried powders.