scholarly journals The Effect of Enantiomer Elution Order on the Determination of Minor Enantiomeric Impurity in Ketoprofen and Enantiomeric Purity Evaluation of Commercially Available Dexketoprofen Formulations

Molecules ◽  
2020 ◽  
Vol 25 (24) ◽  
pp. 5865
Author(s):  
Kenan Can Tok ◽  
Mehmet Gumustas ◽  
Giorgi Jibuti ◽  
Halit Sinan Suzen ◽  
Sibel A. Ozkan ◽  
...  

In a recent study, opposite enantiomer elution order was observed for ketoprofen enantiomers on two amylose-phenylcarbamate-based chiral columns with the same chemical composition of the chiral selector but in one case with coated while in the other with an immobilized chiral selector. In the present study, the influence of this uncommon effect on method validation parameters for the determination of minor enantiomeric impurity in dexketoprofen was studied. The validated methods with two alternative elution orders for enantiomers were applied for the evaluation of enantiomeric impurity in six marketed dexketoprofen formulations from various vendors. In most of these formulations except one the content of enantiomeric impurity exceeded 0.1% (w/w).

2011 ◽  
Vol 49 (No. 11) ◽  
pp. 500-510 ◽  
Author(s):  
M. Prevolnik ◽  
M. Čandek-Potokar ◽  
D. Škorjanc

In contrast to conventional methods for the determination of meat chemical composition and quality, near infrared spectroscopy (NIRS) enables rapid, simple and simultaneous assessment of numerous meat properties. The present article is a review of published studies that examined the ability of NIRS to predict different meat properties. According to the published results, NIRS shows a great potential to replace the expensive and time-consuming chemical analysis of meat composition. On the other hand, NIRS is less accurate for predicting different attributes of meat quality. In view of meat quality evaluation, the use of NIRS appears more promising when categorizing meat into quality classes on the basis of meat quality traits for example discriminating between feeding regimes, discriminating fresh from frozen-thawed meat, discriminating strains, etc. The performance of NIRS to predict meat properties seems limited by the reliability of the method to which it is calibrated. Moreover, the use of NIRS may also be limited by the fact that it needs a laborious calibration for every purpose. In spite of that, NIRS is considered to be a very promising method for rapid meat evaluation.    


2001 ◽  
Vol 56 (7-8) ◽  
pp. 666-668 ◽  
Author(s):  
Kadriye Sorkun ◽  
Banu Süer ◽  
Bekir Salih

The aim of the present work is to study the chemical composition of Turkish propolis. Propolis samples were collected from different regions of Turkey (Bursa, Erzurum-Askale, Gumushane-Sogutagil and Trabzon-Caglayan) in 1999. Ethanol extracts of propolis (EEP) were prepared for chemical analysis, using gas chromatograph coupled with mass spectrometry (GC-MS). Our findings show that propolis samples from Trabzon and Gumushane region have a similar chemical composition. In both samples aromatic acids, aliphatic acids and their esters, and also ketone derivatives are the main compound groups. The chemical composition of the single sample that was collected from Erzurum region shows a very different pattern than the other two samples. In this propolis, the main compounds are aromatic acid esters and alcohols. However, it contains a high amount of amino acids compared to the other samples. The other samples collected from three different region of Bursa City are rich with flavavones, aromatic acids and their esters, terpenoids, flavones and ketones


2022 ◽  
Vol 24 (1) ◽  
pp. 201-215
Author(s):  
Radhika. V ◽  
◽  
T. Ramesh ◽  

A new RP-HPLC method was developed for selective and simultaneous determination of betamethasone dipropionate and tolnaftate in combined semisolid formulation containing other components. Further, the proposed method was validated for linearity, precision (system precision, method precision, intermediate or inter-day precision), accuracy, stability in analytical solution, robustness or system suitability and ruggedness. The developed method exhibited the best results in terms of the aforesaid validation parameters. The other components and additives did not interfere in their determinations. The method was found to be selective, simple, economical, accurate, reproducible, rapid and reliable for routine estimation purpose of these drugs in combined semisolid formulations.


2011 ◽  
Vol 94 (3) ◽  
pp. 723-734 ◽  
Author(s):  
Marija Mašković ◽  
Yannis Dotsikas ◽  
Anđelija Malenović ◽  
Biljana Jančić-Stojanović ◽  
Darko Ivanović ◽  
...  

Abstract This paper describes the development and validation of a microemulsion liquid chromatography (MELC) method for simultaneous determination of perindopril tert-butylamine and its impurities in bulk active substances and the pharmaceutical dosage form of tablets. An appropriate resolution with reasonable retention times was obtained for a microemulsion containing 0.24% (w/v) butyl acetate, 0.30% (w/v) ethyl acetate, 2% (w/v) sodium dodecyl sulfate, 7.75% (w/v) n-butanol, and 20.0 mM potassium dihydrogen phosphate, the pH of which was adjusted to 3.70 with 85% orthophosphoric acid. Separations were performed on a Nucleosil 120-5 butyl modified (C4), 250 × 4 mm, 5 μm particle size silica column at 40°C, with a mobile phase flow rate of 1.25 mL/min. UV detection was performed at 254 nm. The established method was subjected to method validation, and required validation parameters were defined. Robustness testing, an important part of method validation, was performed as well. Since robustness validation can be conducted using different experimental designs, the Plackett-Burman design was applied due to its possibility of testing many factors at the same time. The validated MELC method was found to be suitable for the simultaneous determination of perindopril tert-butylamine and its impurities in pharmaceuticals.


2013 ◽  
Vol 8 (9) ◽  
pp. 1934578X1300800
Author(s):  
Somendu K. Roy ◽  
Khemraj Bairwa ◽  
Jagdeep Grover ◽  
Amit Srivastava ◽  
Sanjay M. Jachak

The leaves of Vitex negundo have been reported to contain various bioactive constituents including iridoids and flavonoids. This is the first report on the simultaneous determination of iridoids and flavonoids by HPLC in three different samples of V. negundo leaves collected from three regions of India. Separation of iridoids and flavonoids was accomplished by HPLC and further elaborated for their quantification in V. negundo leaves using a C-18 column with detection at 254 and 330 nm, respectively. The developed HPLC method showed good linearity (r2≥0.999), high precision (RSD<5%) and a good recovery (99.3–103.0%) of the compounds. All the validation parameters of the developed HPLC were found to be within the permissible limits according to the ICH guidelines. The developed method was robust, accurate and reliable for the quality control of V. negundo leaves.


Author(s):  
F. Coles Phillips

The orientation of the ‘rhombic section’, the composition-plane of the pericline twin, in the plagioclase felspars as an index of the chemical composition of the felspar waJ first utilized by G. yore Rath, who measured the gngle a on the face (010) between the trace of the composition-plane and the edge [010,001]. Duparc and Reinhard, in their comprehensive work on the determination of the plagioclases, quote two series of values for this angle, one due to Wiilfmg and the other to Becke. They comment on the discordance between the two series, most marked at the acid end, and add that they did not then possess suitable material for critical determinations on their own account. Wülfing's values are given in the form of a curve based on data assembled by Schmidt, and those of Becke were first given in a paper on the felspars in crystalline schists.


2020 ◽  
Vol 23 (5) ◽  
pp. 177-182
Author(s):  
Supriyono Supriyono ◽  
Mudhiah Fitrillah ◽  
Arie Pratama Putra

Vitamin B1 plays an important role in the co-enzymatic reactions for energy-rich compounds called ATP (Adenosine Tri Phosphate). Therefore, it should be added to various food products, for example, milk powder. One method that can be used to determine vitamin B1 is SNI number 3751: 2009, but the method is intended for wheat flour. If the method is to be used for the analysis from other samples, such as milk powder, optimization, and validation, are needed. This experiment was carried out using HPLC, C18 column, and UV detector with a wavelength of 254 nm. The mobile phase used is methanol: acetic acid: bi-distilled water = 32:1:67 (v/v/v), flow rate = 1 mL/minute, isocratic, and reverse phased technique. Method validation parameters include tests of system suitability, linearity, the limit of detection, the limit of quantitation, precision (repeatability), and accuracy. The results showed that the system suitability test was obtained relative standard deviations (% RSD) for retention time and peak area, tailing factor, resolution, separation factor was 0.297%, 1.476%, 1.113, 6.693, and 4.406 respectively. The validation test gets a correlation coefficient (R) of 0.9996, the limit of detection and limit of quantitation were 0.0122 mg/100 mL and 0.0244 mg/100 mL, respectively. The precision test obtained Horwitz's ratio of 0.27%. Accuracy test using CRM obtained % recovery of 93.79-97.77%. All these results meet the requirements of method validation, so it can be concluded that the method of SNI number 3751: 2009 is valid for the determination of vitamin B1 in milk powder and can be used for routine analysis procedure.


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