Özgür Üstündağ

An Approach to Quantitative Two‐Component Analysis of a Mixture Containing Hydrochlorothiazide and Spironolactone in Tablets by One‐Dimensional Continuous Daubechies and Biorthogonal Wavelet Analysis of UV‐Spectra

In this study a new method of quantitative two‐component analysis of a mixture of hydrochlorothiazide (HCT) and spironolactone (SP) in the presence of strongly overlapping signals was achieved by using one‐dimensional continuous wavelet analysis. This new method was built on the simultaneous use of both continuous wavelet transform and the zero crossing technique for the quantitative resolution of this binary mixture. A series of solutions, in the concentration range of 2–22 mg/ml for both compounds, in methanol and 0.2 M sodium acetate buffer, pH = 5 (20:80), were considered. The absorption spectra of the standard solutions were recorded in the wavelength range of 215–330 nm. To apply our methods we selected 400 points from the absorption spectra and we subjected the corresponding signal to Daubechies2 (DAUB2) and Biorthogonal1.5 (BIOR1.5) one‐dimensional wavelet transform. In the transformed signals, the amplitude of HCT was measured at the position of a zero crossing point of SP and vice versa. Thus simple linear regression analysis can be applied to establish calibrations for both components. These calibrations were validated with synthetic mixtures of HCT and SP. MATLAB 6.5 software was used for one‐dimensional wavelet analysis, and the basic concepts about wavelet method are briefly explained. The method developed in this paper is rapid, easy to apply, inexpensive and it is suitable for analysis of the overlapping signals of compounds in their mixtures without any chemical pre‐treatment.

Simultaneous spectrophotometric determination of chlorphenoxamine hydrochloride and caffeine in a pharmaceutical preparation using first derivative of the ratio spectra and chemometric methods

Three new methods are described for the simultaneous determination of chlorphenoxamine hydrochloride (CP) and caffeine (CAF) in their combination. In the first method, ratio spectra derivative spectrophotometry, analytical signals were measured at the wavelengths corresponding to either maxima and minima for both drugs in the first derivative spectra of the ratio spectra obtained by using each other spectra as divisor in their solution in 0.1 M HCl. In the other two methods, chemometric techniques, classical least-squares (CLS) and inverse least-squares (ILS), the concentration data matrix were prepared by using the synthetic mixtures containing these drugs in 0.1 M HCl. The absorbance data matrix corresponding to the concentration data matrix was obtained by the measurements of absorbances in the range 225-285 nm in the intervals with Deltalambda = 5 nm at 13 wavelengths in their zero-order spectra, then, calibration or regression was obtained by using the absorbance data matrix and concentration data matrix for the prediction of the unknown concentrations of CP and CAF in their mixture. The numerical values were calculated by using MAPLE V software in chemometric methods. The procedures do not require any separation step. The accuracy and the precision of the methods have been determined and they have been validated by analyzing synthetic mixtures containing title drugs. These three methods were successfully applied to a pharmaceutical formulation, sugar-coated tablet, and the results were compared with each other.

Chemometric resolution of a mixture containing hydrochlorothiazide and amiloride by absorption and derivative spectrophotometry

Four chemometric techniques, classical least squares (CLS) and inverse least squares (ILS) and principal component regression (PCR) and partial least squares regression (PLSR) were applied to the absorption and derivative spectrophotometric determinations of amiloride and hydrochlorothiazide in a pharmaceutical preparation. Four chemometric calibrations for both zero-order and first derivative spectra were constructed by measuring the absorbance and their dA/dlambda values at 34 points in the wavelength range 205-395 nm for a training set containing 2-10 microg/ml amiloride and 4-28 microg/ml hydrochlorothiazide corresponding to 25 point mixture design. The building chemometric calibrations were confirmed by using the synthetic mixtures containing two drugs. The results obtained by the proposed techniques based on the use of the measurements at the absorption spectra and at the first derivative spectra were statistically compared with each other.

A New Application of Chemometric Techniques to HPLC Data for the Simultaneous Analysis of a Two‐Component Mixture

Abstract A new chemometric approach using high performance liquid chromatography (HPLC) with photodiode array (PDA) detection was developed and applied to the simultaneous determination of enalapril maleate (EA) and hydrochlorothiazide (HCT) in tablets. Chemometric calibration techniques, classical least squares (CLS), principle component regression (PCR), and partial least squares (PLS) were subjected to the peak area at multiwavelength PDA detector responses. The combination of HPLC and chemometric calibration techniques was called HPLC‐CLS, HPLC‐PCR, and HPLC‐PLS. For comparison purposes, the HPLC method called classical HPLC method was used for the confirmation of the results obtained from combined HPLC‐chemometric calibration techniques. A good chromatographic separation between two drugs and internal standard (IS) was achieved using a Waters Symmetry® C18 Column 5 µm 4.6×250 mm and a mobile phase consisting of 0.2 M acetate buffer and acetonitrile (v/v, 60∶40). The multiwavelength PDA detection was done at 230 (A), 240 (B), 250 (C), 250 (D), 240 (E) nm wavelengths, and peak area was recorded for the concentration set in the mobile phase. Three HPLC‐chemometric calibrations and a classical‐HPLC method were tested by analyzing the synthetic mixture of EA and HCT in the presence of losartan potassium (IS). The proposed methods were applied to real samples containing the present two drugs. The obtained results were statistically compared with each other.

Simultaneous chemometric determination of pyridoxine hydrochloride and isoniazid in tablets by multivariate regression methods

The sole use of pyridoxine hydrochloride during treatment of tuberculosis gives rise to pyridoxine deficiency. Therefore, a combination of pyridoxine hydrochloride and isoniazid is used in pharmaceutical dosage form in tuberculosis treatment to reduce this side effect. In this study, two chemometric methods, partial least squares (PLS) and principal component regression (PCR), were applied to the simultaneous determination of pyridoxine (PYR) and isoniazid (ISO) in their tablets. A concentration training set comprising binary mixtures of PYR and ISO consisting of 20 different combinations were randomly prepared in 0.1 M HCl. Both multivariate calibration models were constructed using the relationships between the concentration data set (concentration data matrix) and absorbance data matrix in the spectral region 200-330 nm. The accuracy and the precision of the proposed chemometric methods were validated by analyzing synthetic mixtures containing the investigated drugs. The recovery results obtained by applying PCR and PLS calibrations to the artificial mixtures were found between 100.0 and 100.7%. Satisfactory results obtained by applying the PLS and PCR methods to both artificial and commercial samples were obtained. The results obtained in this manuscript strongly encourage us to use them for the quality control and the routine analysis of the marketing tablets containing PYR and ISO drugs.

Wavelet transform for the simultaneous prediction of the colorants in food product

Wavelet transform method was successfully applied to the multicomponent analysis of the binary mixtures containing different colorants in commercial food product. In this application, wavelet transform method is suitable for the quantitative resolution of the mixtures of these colorants and this hybrid approach doesn’t require any separation and extraction steps. The method was tested by using various synthetic ternary mixtures and applied to the sample and successfully results were obtained.