scholarly journals Zero crossing and ratio spectra derivative spectrophotometry for the dissolution tests of amlodipine and perindopril in their fixed dose formulations

2014 ◽  
Vol 27 (2) ◽  
pp. 113-117 ◽  
Author(s):  
Paulina Maczka ◽  
Anna Gumieniczek ◽  
Justyna Galeza ◽  
Rafal Pietras

Abstract Dissolution tests of amlodipine and perindopril from their fixed dose formulations were performed in 900 mL of phosphate buffer of pH 5.5 at 37°C using the paddle apparatus. Then, two simple and rapid derivative spectrophotometric methods were used for the quantitative measurements of amlodipine and perindopril. The first method was zero crossing first derivative spectrophotometry in which measuring of amplitudes at 253 nm for amlodipine and 229 nm for perindopril were used. The second method was ratio derivative spectrophotometry in which spectra of amlodipine over the linearity range were divided by one selected standard spectrum of perindopril and then amplitudes at 242 nm were measured. Similarly, spectra of perindopril were divided by one selected standard spectrum of amlodipine and then amplitudes at 298 nm were measured. Both of the methods were validated to meet official requirements and were demonstrated to be selective, precise and accurate. Since there is no official monograph for these drugs in binary formulations, the dissolution tests and quantification procedure presented here can be used as a quality control test for amlodipine and perindopril in respective dosage forms.

2011 ◽  
Vol 94 (1) ◽  
pp. 128-135 ◽  
Author(s):  
Elif Karacan ◽  
Mehmet Gokhan Çaġlayan ◽  
İsmail Murat Palabiyik ◽  
Feyyaz Onur

Abstract A new RP-LC method and two new spectrophotometric methods, principal component regression (PCR) and first derivative spectrophotometry, are proposed for simultaneous determination of diflucortolone valerate (DIF) and isoconazole nitrate (ISO) in cream formulations. An isocratic system consisting of an ACE® C18 column and a mobile phase composed of methanol–water (95+5, v/v) was used for the optimal chromatographic separation. In PCR, the concentration data matrix was prepared by using synthetic mixtures containing these drugs in methanol–water (3+1, v/v). The absorbance data matrix corresponding to the concentration data matrix was obtained by measuring the absorbances at 29 wavelengths in the range of 242–298 nm for DIF and ISO in the zero-order spectra of their combinations. In first derivative spectrophotometry, dA/dλ values were measured at 247.8 nm for DIF and at 240.2 nm for ISO in first derivative spectra of the solution of DIF and ISO in methanol–water (3+1, v/v). The linear ranges were 4.00–48.0 μg/mL for DIF and 50.0–400 μg/mL for ISO in the LC method, and 2.40–40.0 μg/mL for DIF and 60.0–260 μg/mL for ISO in the PCR and first derivative spectrophotometric methods. These methods were validated by analyzing synthetic mixtures. These three methods were successfully applied to two pharmaceutical cream preparations.


INDIAN DRUGS ◽  
2020 ◽  
Vol 57 (09) ◽  
pp. 75-81
Author(s):  
Rakesh M Wani ◽  
Arun M Kashid ◽  
Amita Ghatge ◽  
Sumita Sahoo

The aim of the present work was to develop simple, precise and economic UV- spectrophotometric methods for the simultaneous estimation of aspirin and omeprazole in a laboratory sample. The absorbance maxima (λmax) for detection of aspirin and omeprazole were selected as 274 nm and 302 nm, respectively, for simultaneous equation method while wavelength range for detection of aspirin and omeprazole were selected as 270 nm - 276 nm and 300 nm - 305 nm, respectively for area under curve method. Absorbance ratio method uses the ratio of absorbances at two selected wavelengths, one which is an isoabsorptive point and other being the λ max of one of the two components. From the overlay spectra of two drugs, it is evident that aspirin and omeprazole show an isoabsorptive point at 238.6 nm. In zero crossing first derivative spectrophotometry, aspirin showed zero crossing point at 301nm and omeprazole showed zero crossing point at 274nm. Linearity for aspirin was between 25- 125 μg/mL and omeprazole it was 3-15 μg/mL. These methods were successfully applied for estimation of aspirin and omeprazole in the laboratory sample.


2013 ◽  
Vol 10 (3) ◽  
pp. 866-882
Author(s):  
Baghdad Science Journal

New derivative molecular absorption spectrophotometric methods have been developed for the determination of Al (III) , Mn (II) , individually and binary mixtures . The aim of this model of study is to obtain analytical results characterized by adequate standard of analytical figures of merits through application of derivative Spectrophotometry (dnA/d?n). The two metals acetyl acetonates are chemically stable and are widely used as catalysts . Where Interferences are probable due to very close or nearby peaks or Summits, the Zero – Crossing derivative measurement technique is used to avoid interfering effects between two metals pairs.


2010 ◽  
Vol 93 (4) ◽  
pp. 1180-1191 ◽  
Author(s):  
Laila S Abdel-Fattah ◽  
Zeinab A El-Sherif ◽  
Khadiga M Kilani ◽  
Dalia A El-Haddad

Abstract Three stability-indicating assay methods were developed for the determination of tropisetron in a pharmaceutical dosage form in the presence of its degradation products. The proposed techniques are HPLC, TLC, and first-derivative spectrophotometry (1D). Acid degradation was carried out, and the degradation products were separated by TLC and identified by IR, NMR, and MS techniques. The HPLC method was based on determination of tropisetron in the presence of its acid-induced degradation product on an RP Nucleosil C18 column using methanolwateracetonitriletrimethylamine (65 + 20 + 15 + 0.2, v/v/v/v) mobile phase and UV detection at 285 nm. The TLC method was based on the separation of tropisetron and its acid-induced degradation products, followed by densitometric measurement of the intact spot at 285 nm. The separation was carried out on silica gel 60 F254 aluminum sheets using methanolglacial acetic acid (22 + 3, v/v) mobile phase. The 1D method was based on the measurement of first-derivative amplitudes of tropisetron in H2O at the zero-crossing point of its acid-induced degradation product at 271.9 nm. Linearity, accuracy, and precision were found to be acceptable over concentration ranges of 40240 g/mL, 110 g/spot, and 636 g/mL for the HPLC, TLC, and 1D methods, respectively. The suggested methods were successfully applied for the determination of the drug in bulk powder, laboratory-prepared mixtures, and a commercial sample.


2013 ◽  
Vol 2013 ◽  
pp. 1-7 ◽  
Author(s):  
Mohammad H. AbdelHay ◽  
Azza A. Gazy ◽  
Rasha A. Shaalan ◽  
Heba K. Ashour

Two simple and selective methods were developed for the simultaneous determination of tenofovir fumarate (TEN) and emtricitabine (EMT) in combined tablets. The first method involves the application of first derivative spectrophotometry where the first derivative amplitudes were measured at 298.5 nm for determination of EMT in presence of TEN. The second method involves first derivative of ratio spectra spectrophotometry where the amplitudes at 251.5 nm have been used for quantitation of TEN in the presence of EMT. Different variables affecting each method were carefully investigated and optimized. Reliability and analytical performance of the proposed methods, including linearity, range, precision, accuracy, detection, and quantitation limits, were statistically validated. The methods were successfully applied for the determination of EMT and TEN in laboratory-prepared mixtures and in their combined tablets.


2021 ◽  
Vol 129 (7) ◽  
pp. 972
Author(s):  
S.S. Kurdaikar ◽  
A. Fernandes ◽  
S.V. Gandhi ◽  
P. Pattewar ◽  
A.A. Mahajan

The present research work was carried out in order to develop simple, accurate and precise UV sprctrophotometric methods having comparable sensitivity as that of sophisticated chromatographic techniques. Two methods were developed namely first derivative spectrophotometry and ratio spectra derivative spectrophotometry for accurate determination of specified impurity methimazole (imp A) in presence of drug carbimazole. First derivative spectrophotometric method involves recording of zero order spectra of both the drugs carbimazole and methimazole and its mixture in the range of 200-400 nm and subsequent conversion of these spectra into first derivative spectra. The drugs carbimazole and methimazole were determined by using zero crossing wavelengths of 227 and 260 nm respectively. In the second approach, ratio spectra were recorded for carbimazole and methimazole by selecting appropriate divisor concentration and converted into first derivative spectra. The determination of carbimazole and methimazole were carried out at wavelength 226.2 and 257 nm, respectively. Both the methods were validated as per ICH guideline. The drugs carbimazole and methimazole showed linear response with good correlation coefficient and exhibited specificity, accuracy and precision within acceptable range. The second method of ratio spectra derivative spectrophotometry was found more sensitive as compare to first derivative spectrophotometry in detecting level of impurity methimazole up to 0.5% as per official specification. Hence, these developed methods can be used as alternative to sophisticated chromatographic technique for determination of assay and related impurity in bulk drug and formulation. Keywords: carbimazole, methimazole, first derivative spectrophotometry, ratio spectra derivative spectrophotometry.


2012 ◽  
Vol 9 (3) ◽  
pp. 1357-1363 ◽  
Author(s):  
Rajni Rohilla ◽  
Usha Gupta

A first-derivative spectrophotometry method for the simultaneous determination of Co (II) and Ni (II) with Alizarin Red S in presence of Triton X-100 is described. Measurements were made at the zero-crossing wavelengths at 549.0 nm for Co (II) and 546.0 nm for Ni (II). The linearity is obtained in the range of 0.291- 4.676 μg/ml of Ni (II) and 0.293- 4.124 μg/ml of Co (II) in the presence of each other by using first derivative spectrophotometric method. The possible interfering effects of various ions were studied. The validity of the method was examined by using synthetic mixtures of Co (II) and Ni (II). The developed derivative procedure, using the zero crossing technique, has been successfully applied for the simultaneous analysis of Co (II) and Ni (II) in spiked water samples.


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