scholarly journals Analytical Method Development for Sodium Valproate through Chemical Derivatization

2020 ◽  
Vol 2020 ◽  
pp. 1-7
Author(s):  
Murad Abualhasan ◽  
Nihaya Wasif Odeh ◽  
Ghadeer Naser Younis ◽  
Oyoun Fadel Zeidan
Keyword(s):  
Valproic Acid ◽  
Sodium Valproate ◽  
Analytical Method ◽  
Method Development ◽  
Analytical Procedure ◽  
Phenyl Group ◽  
Chemical Derivatization ◽  
Reverse Phase Hplc ◽  
Reverse Phase ◽  
Low Concentrations

Background. Sodium valproate has anticonvulsant activity and is structurally different to conventional antiepileptic drugs. The problem with valproic acid is the lack of a chromophore, which means that gas chromatography is the sole assay methodology. The introduction of benzoyl and phenyl groups to the molecule is a useful derivatisation, which enables the creation of detectable chromophores for HPLC analysis for pharmaceutical dosages as well as biological systems. Methodology. Sodium valproate was derivatised by the addition of a chromophore to its structure by introducing a methyl benzoyl or a phenyl group. Trichlorophenol and 2-hydroxyacetophenone were used to introduce phenyl and benzoyl groups to valproic acid, respectively. The reaction used was estrification reaction using coupling agents. An analytical method was then developed and validated using reverse-phase HPLC. The method was validated for parameters like linearity, range, accuracy precision, and robustness. Results. The developed method was easy and feasible and can be applied to both routine analysis and bioanalysis. The method was very sensitive and could quantify valproic acid at a very low concentration of 0.75 × 10−5 mg/ml. The developed method was found to be linear (R2 = 0.997), accurate, precise, and robust. Conclusion. The proposed chemical derivatisation and the developed analytical method are novel. The developed analytical procedure is the first of its kind; it is easy and feasible and can be used to quantify and detect sodium valproate at very low concentrations compared to other available methods in the literature.

Method development of clarithromycin by chromophore addition through chemical derivatization

2020 ◽  
Vol 16 ◽  
Author(s):  
Murad Abualhasan ◽  
Amal Qato ◽  
Salam Qrareya ◽  
Tasneem Khassib
Keyword(s):  
Method Development ◽  
Bathochromic Shift ◽  
Hplc Method ◽  
Esterification Reaction ◽  
Chemical Derivatization ◽  
Reverse Phase Hplc ◽  
Reverse Phase ◽  
Limit Of Quantification ◽  
Pharmaceutical Dosage Forms ◽  
Low Concentration

Introduction: Clarithromycin is a macrolide antibiotic that is active against a variety of microorganisms. It is widely used in the local and international market in different pharmaceutical dosage forms. However, its chemical structure lacks a chromophore and hence it has a low absorption and this makes it more difficult to be detected at low concentrations. In this research project we proposed an easy and feasible chemical derivatization of clarithromycin to introduce a chromophore in order to increase its absorptivity at low concentration using a simple reverse phase HPLC analytical method. Methodology: Chemical derivatization of clarithromycin involved an introduction of benzoyl groups as a chromophore through esterification reaction. A reverse phase analytical HPLC method was developed to quantify clarithromycin at a very low concentration compared to the standard official pharmacopeia. Results: Clarithromycin was successfully derivatized and a hyperchromic and bathochromic shift to UV absorption lambda max (λmax) was achieved (λmax = 245nm.) A successful chromatographic separation was obtained using a reverse phase HPLC chromatography. The developed method was capable of detecting and quantifying clarithromycin at very low concentration. The limit of quantification (LOD) and limit of quantification (LOQ) was found to be 2*10-8 mg/ml and 2*10-6 mg/ml respectively. Conclusion: Clarithromycin was successfully derivatized to a chromophore containing molecule. The developed reverse phase HPLC method is capable to detect and quantify clarithromycin at a very low concentration. The method can successfully quantify clarithromycine when present in low concentration such as in biological and enviromental samples.

scholarly journals Method Development for 4-Hydroxy-2-Methyl-N- (5-Methyl-2-Thiazolyl)-2H-1,2-Benzothiazine-3-Carboxamide-1,1-Dioxide by Reverse Phase HPLC: New Analytical Technique

2019 ◽  
pp. 1-10
Author(s):  
Husnul Maab ◽  
Hammad Yousaf ◽  
Syed Saeed ul Hassan ◽  
Umar Farooq
Keyword(s):  
Mobile Phase ◽  
Method Development ◽  
Raw Material ◽  
New Method ◽  
Reverse Phase Hplc ◽  
Reverse Phase ◽  
Analytical Technique ◽  
Peak Areas ◽  
Standard Solution ◽  
Study Development

Purpose: In this study, development of a new analytical method for the evaluation of 4-Hydroxy-2-methyl-N-(5-methyl-2-thiazolyl)-2H-1,2-benzothiazine-3-carboxamide-1,1-dioxide (Meloxicam) by reverse phase HPLC was carried out. The basic aim of this research was to develop and validate a simple, precise, accurate and sensitive method for qualitative and quantitative analysis of Meloxicam in pharmaceutical raw material and its dosage forms. The existing reported method (BP) for the analysis of Meloxicam is potentiometric method which is an old, lengthy and tedious method. Methods: In the new method of reverse phase HPLC, C18 column was used while the mobile phase was acetonitrile and methanol (70:30). The flow rate of mobile phase was 0.6 ml/min and retention time was found to be 1.5min. Separately equal volume of standard solution and sample solutions in HPLC vials were injected in auto sampler compartment of HPLC in six replicates. Chromatogram and peak areas of Meloxicam in standard and sample solutions of different concentrations were recorded. Results: This method was later validated in different ways by which the calibration curve proved to be linear with linearity coefficient of 0.999 over the range of 100 to 600ppm. The precision was equivalent to 0.0003%. The LOD and LOQ were 0.0003ug/ml and 0.001ug/ml respectively. The system also showed accuracy over the range of 95 to 99%. Conclusion: Hence, this method proved to be an alternative to the existing reported method of potentiometric titration because the new method showed accuracy, reproducibility and sensitivity.

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