Multivariate Spectrophotometric Methods Research Articles

Simultaneous spectrophotometric determination of Celecoxib and Diacerein in bulk and capsule by absorption correction method and chemometric methods

Two methods, absorption correction and multivariate spectrophotometric methods were developed for simultaneous estimation of Celecoxib (CEL) and Diacerein (DIA) in combined dosage form. Absorption correction method involves direct estimation of DIA at wavelength 341nm in which CEL has zero absorbance and shows no interference. For estimation of CEL, corrected absorbance was calculated at 253nm due to the interference of DIA at this wavelength. Linearity was observed in the range of 6–22μgmL−1 for CEL and 3–11μgmL−1 for DIA. The method was validated as per ICH guidelines. Chemometric methods including classical least square (CLS), inverse least square (ILS), principal component regression (PCR) and partial least square (PLS) were studied for simultaneous determination of CEL and DIA in capsule using spectrophotometry. A set of 25 standard mixtures containing both drugs were prepared in range of 5–25μgmL−1 for CEL and 3–15μgmL−1 for DIA. Analytical figure of merit (FOM), such as sensitivity, selectivity, analytical sensitivity, limit of detection and limit of quantitation were determined for chemometric methods. The proposed methods were applied for determination of two components from combined dosage form.

CHROMATOGRAPHIC AND CHEMOMETRICS-ASSISTED SPECTROPHOTOMETRIC METHODS FOR THE SIMULTANEOUS DETERMINATION OF ALLOBARBITAL, ADIPHENINE HYDROCHLORIDE, AND PARACETAMOL IN SUPPOSITORY

High-performance liquid chromatography (HPLC) and multivariate spectrophotometric methods were developed for the simultaneous determination of allobarbital (ALO), adiphenine hydrochloride (ADI), and paracetamol (PAR) in suppository medication. The HPLC method was performed on a C18 column with a mobile phase consisting of a mixture of acetonitrile and buffer solution (pH 4.0) of sodium acetate and acetic acid (60:40, v/v) and UV detection at 195 nm. This method was validated for its linearity, precision, accuracy, and robustness. Also, the resolution of three components has been accomplished by using the multivariate calibration methods PCR and PLS-2. Experimental calibration matrix was constructed using 27 samples, according to the 33 full factorial design. These chemometric methods were tested by analyzing the synthetic mixtures of three drugs. The proposed methods were succesfully applied for the analysis of pharmaceutical formulations containing ALO, ADI, and PAR combinations and the obtained results were statistically compared with each other.

Univariate versus Multivariate Spectrophotometric Methods for Simultaneous Determination of Complex Binary Mixtures with Overlapped Spectra: A Comparative Study

Two novel simple and accurate univariate spectrophotometric methods were described for the determination of a binary mixture of Sodium cromoglicate (SCG) and Fluorometholone (FLU) namely; ratio subtraction coupled with extended ratio subtraction (RS-EXRSM) and constant center (CCSM) spectrophotometric methods. The methods were able to recover the zero order absorption spectra of both drugs from their binary mixture through simple mathematical calculations. The linearity ranges were found to be (2.5–25 µg/mL) and (4- 25 µg/mL) for SCG and FLU, respectively. A comparative study was conducted between the proposed univariate methods versus multivariate ones, based on using principle component regression (PCR) and partial least squares (PLS-2). Upon applying the methods for the determination of SCG and FLU in laboratory prepared mixtures, the (CCSM and PLS-2) proved to be of higher predictive ability rather than (RS-EXRSM and PCR) in prediction of mixtures containing low concentration of one of the components. The proposed methods were validated in compliance with the ICH guidelines. These methods could be alternative to different HPLC techniques in quality control laboratories lacking the required facilities for those expensive techniques

SIMULTANEOUS DETERMINATION OF TWO MULTICOMPONENT MIXTURES CONTAINING PHENOBARBITONE AND EPHEDRINE HYDROCHLORIDE USING HPLC AND CHEMOMETRIC ASSISTED SPECTROPHOTOMETRIC METHODS

Three methods for the simultaneous determination of two multicomponent mixtures containing phenobarbitone and ephedrine hydrochloride with theophylline, and postafene hydrochloride [mix 1]; or dihydroxypropyltheophylline and chlorpheniramine maleate [mix 2] were proposed. The HPLC method depended on the use of gradient mobile phase system consisting of (A) acetonitrile and (B)12 mM ammonium acetate; pH 4.5 with cyanopropyl column at a flow rate of 1.5 mL min−1. Quantitation was achieved with UV detection at 215 nm, based on peak area. The two other methods were multivariate spectrophotometric calibration methods: partial least squares (PLS-1) and principal component regression (PCR). These approaches were successfully applied to quantify each component in the mixture. Analytical figures of merit (FOM) were calculated for both PLS-1 and PCR. The proposed methods were successfully applied for the analysis of pharmaceutical formulations containing the two multicomponent combinations and the results were compared.

New validated liquid chromatographic and chemometrics-assisted UV spectroscopic methods for the determination of two multicomponent cough mixtures in syrup.

Multivariate spectrophotometric calibration and liquid chromatographic (LC) methods were applied to the determination of 2 multicomponent mixtures containing diprophylline, guaiphenesin, methylparaben, and propylparaben (Mixture 1), or clobutinol, orciprenaline, saccharin sodium, and sodium benzoate (Mixture 2). For the multivariate spectrophotometric calibration methods, principal component regression (PCR) and partial least-squares regression (PLS-1), a calibration set of the mixtures consisting of the components of each mixture was prepared in 0.1 M HCl. Analytical figures of merit such as sensitivity, selectivity, limit of quantitation, and limit of detection were determined for both PLS-1 and PCR. The LC separation was achieved on a reversed-phase C18 analytical column by using isocratic elution with 20 mM potassium dihydrogen phosphate, pH 3.3-acetonitrile (55 + 45, v/v) as the mobile phase and UV detection at 260 and 220 nm for Mixture 1 and Mixture 2, respectively. The proposed methods were validated and successfully applied to the analysis of pharmaceutical formulations and laboratory-prepared mixtures containing the 2 multicomponent combinations.

HPLC and chemometrics-assisted UV-spectroscopy methods for the simultaneous determination of ambroxol and doxycycline in capsule

High-performance liquid chromatography (HPLC) and multivariate spectrophotometric methods are described for the simultaneous determination of ambroxol hydrochloride (AM) and doxycycline (DX) in combined pharmaceutical capsules. The chromatographic separation was achieved on reversed-phase C 18 analytical column with a mobile phase consisting of a mixture of 20 mM potassium dihydrogen phosphate, pH 6–acetonitrile in ratio of (1:1, v/v) and UV detection at 245 nm. Also, the resolution has been accomplished by using numerical spectrophotometric methods as classical least squares (CLS), principal component regression (PCR) and partial least squares (PLS-1) applied to the UV spectra of the mixture and graphical spectrophotometric method as first derivative of the ratio spectra ( 1DD) method. Analytical figures of merit (FOM), such as sensitivity, selectivity, analytical sensitivity, limit of quantitation and limit of detection were determined for CLS, PLS-1 and PCR methods. The proposed methods were validated and successfully applied for the analysis of pharmaceutical formulation and laboratory-prepared mixtures containing the two component combination.

Development and Validation of Chemometrics-Assisted Spectrophotometry and Liquid Chromatography Methods for the Simultaneous Determination of the Active Ingredients in Two Multicomponent Mixtures Containing Chlorpheniramine Maleate and Phenylpropanolamine Hydrochloride

Multivariate spectrophotometric calibration and liquid chromatography (LC) methods were used for the simultaneous determination of the active ingredients in 2 multicomponent mixtures containing chlorpheniramine maleate and phenylpropanolamine hydrochloride with ibuprofen and caffeine (mixture 1) or with propyphenazone (mixture 2). For the multivariate spectrophotometric calibration methods, principal component regression (PCR) and partial least squares (PLS-1), a calibration set of the mixtures consisting of the components of each mixture was prepared in distilled water. A leave-1-out cross-validation procedure was used to find the optimum numbers of latent variables. Analytical parameters such as sensitivity, selectivity, analytical sensitivity, limit of quantitation, and limit of detection were determined for both PLS-1 and PCR. The LC method depends on the use of a cyanopropyl column with the mobile phase acetonitrile-12 mM ammonium acetate, pH 5.0 (25 + 75, v/v), for mixture 1 or acetonitrile-10 mM potassium dihydrogen phosphate, pH 4.7 (45 + 55, v/v), for mixture 2; the UV detector was set at 212 nm. In spite of the presence of a high degree of spectral overlap of these components, they were rapidly and simultaneously determined with high accuracy and precision, with no interference from the matrix excipients. The proposed methods were successfully applied to the analysis of pharmaceutical formulations and laboratory-prepared mixtures containing the 2 multicomponent combinations.