scholarly journals FORMING OF DIASTEREOISOMER WITH L-ISOLEUCIN TO SEPARATE OFLOXACIN ENANTIOMER USING PREPARATIVE LIQUID CHROMATOGRAPHY

2015 ◽  
Vol 3 (1) ◽  
Author(s):  
Diana Hendrati ◽  
Husein H. Bahti ◽  
Uji Pratomo ◽  
Zenith Putri Dewianti
Keyword(s):  
Liquid Chromatography ◽  
Mobile Phase ◽  
Bacterial Infections ◽  
Chiral Column ◽  
Preparative Liquid Chromatography ◽  
Separation Of Enantiomers ◽  
Pharmacology And Toxicology ◽  
The Right ◽  
Ofloxacin Enantiomers ◽  
Small Resolution

Ofloxacin is an antibiotic with a broad range of uses in human and veterinary medicine to prevent or treat bacterial infections which has an enantiomeric mixture structure of (-)-ofloxacin and (+)-ofloxacin. Enantiomers of drugs have different pharmacology and toxicology effects that need to be separated before it used to get the molecule target. Separation of enantiomers using chiral column is not quite economical separation, but the separation of enantiomers using a chiral column by converting the enantiomeric mixture into a diastereoisomeric form is the right solution. This study aims to separate mixture of ofloxacin enantiomers by forming diastereoisomeric with L-isoleusine and copper (II) into compound (-)-ofloxacin and (+)-ofloxacin and also to identify the optimum condition of separation using HPLC with preparative liquid chromatography column. Samples injected into the column and eluted by the mobile phase (consisting a mixture of water-methanol (88:12) and solution of L-isoleusine 4 mM and copper (II) sulfate 9 mM). Then the fractions were compared with the standard and the purity was tested by HPLC. This research resulted 47 fractions which four of early fractions have correspond with the standard of (-)-ofloxacin and 43 other factions do not. We obtained the resolution of this separtion about 0.98. The small resolution caused by complex formation is not perfect with the concentration of L-isoleucine and copper (II).

scholarly journals Simultaneous Determination of Levocetirizine and Pseudoephedrine in Dog Plasma by Liquid Chromatography-Mass Spectrometry in the Presence of Dextrocetirizine

2012 ◽  
Vol 15 (4) ◽  
pp. 519 ◽  
Author(s):  
Jae Kuk Ryu ◽  
Sun Dong Yoo
Keyword(s):  
Mass Spectrometry ◽  
Liquid Chromatography ◽  
Oral Administration ◽  
Mobile Phase ◽  
Internal Standard ◽  
Liquid Chromatography Mass Spectrometry ◽  
Chiral Column ◽  
Accuracy And Precision ◽  
Dog Plasma

Purpose. This study describes the development of a rapid and sensitive LC-ESI-MS assay for simultaneous enantioselective determination of levocetirizine and pseudoephedrine in dog plasma in the presence of dextrocetirizine. Methods. Separations were achieved on an Ultron ES-OVM chiral column using the mobile phase consisting of 10 mM aqueous NH4OAc (pH 6.6) and acetonitrile (9:1 v/v). Results. The retention times of pseudoephedrine, dextrocetirizine, levocetirizine and diazepam (internal standard) were 5.2, 8.3, 9.6 and 11.6 min, respectively, and the total run time was less than 15 min. The assay was validated to demonstrate the linearity, accuracy and precision, recovery and stability. The calibration curves were linear over the concentration range from 1 – 200 ng/mL for levocetirizine and from 5 – 1000 ng/mL for pseudoephedrine. Conclusions. The developed assay was successfully applied to a pharmacokinetic study after oral administration of the racemic cetirizine (0.5 mg/kg, or 0.25 mg/kg as levocetirizine) and pseudoephedrine (12 mg/kg) in the dog. This article is open to POST-PUBLICATION REVIEW. Registered readers (see “For Readers”) may comment by clicking on ABSTRACT on the issue’s contents page.

scholarly journals Penentuan Kadar Kalium Sorbat dan Persen Recovery Pada Selai dengan Metoda High Performance Liquid Chromatography

2020 ◽  
Vol 1 (1) ◽  
pp. 25
Author(s):  
Pevi Riani ◽  
Ulvie Ameinda Fannin
Keyword(s):  
High Performance Liquid Chromatography ◽  
Liquid Chromatography ◽  
Mobile Phase ◽  
High Performance ◽  
Food Additives ◽  
Quality Standard ◽  
Potassium Sorbate ◽  
Test Results ◽  
Standard Set ◽  
The Right

Fruit jam is one of the preserved products that have a soft texture that contains crushed fruit and is mixed with sugar with the addition or without the addition of water. Preservatives are added to prevent damage to jams. A preservative that is usually added to jam is potassium sorbate. Potassium sorbate is commonly used as a preservative because it dissolves more easily when added to food. This study aims to determine the levels of potassium sorbate in jam samples. Potassium sorbate was determined using High Performance Liquid Chromatography (HPLC). From the test results, it was found that potassium sorbate levels ranged from719, 65 mg/kg to 757,24 mg/kg. The results of this test will be compared with the standards set by the Food and Drug Supervisory Agency (BPOM) No. 36 of 2013 concerning the maximum limit for the use of preservative food additives, namely 500 mg/kg. From the test results, it can be seen that the potassium sorbate in all samples exceeds the quality standard set by the BPOM. Therefore, people must be more careful in choosing jam to consume daily. The test results have used the right method, namely by adjusting the stationary phase, mobile phase and the right wavelength so that the% recovery results are 103%.

Analysis of organic impurities of besifloxacin hydrochloride by high performance liquid chromatography with isocratic and gradient elution.

2019 ◽  
Vol 16 ◽  
Author(s):  
Joanna Wittckind Manoel ◽  
Camila Ferrazza Alves Giordani ◽  
Livia Maronesi Bueno ◽  
Sarah Chagas Campanharo ◽  
Elfrides Eva Sherman Schapoval ◽  
...  
Keyword(s):  
High Performance Liquid Chromatography ◽  
Liquid Chromatography ◽  
Mobile Phase ◽  
High Performance ◽  
Gradient Elution ◽  
Pharmaceutical Product ◽  
Raw Material ◽  
Isocratic Elution ◽  
Organic Impurities ◽  
Elution Method

Introduction: Impurity analysis is an important step in the quality control of pharmaceutical ingredients and final product. Impurities can arise from drug synthesis or excipients and even at small concentrations may affect product efficacy and safety. In this work two methods using high performance liquid chromatography (HPLC) were developed and validated for the evaluation of besifloxacin and its impurity synthesis, with isocratic elution and another with gradient elution. Method: The analysis by HPLC in isocratic elution mode was performed using a cyano column maintained at 25 °C. The mobile phase was composed by 0.5% triethylamine (pH 3.0): acetonitrile (88:12 v/v) eluted at a flow rate of 1.0 ml/min with detection at 330 nm. The gradient elution method was carried out with the same column and mobile phase components only modifying the rate between organic and aqueous phase during analysis. The procedures have been validated according to internationally accepted guidelines, observing results within acceptable limits. Results: The methods presented were found to be linear in the 140 to 260 µg/ml range for besifloxacin and 0.3 to 2.3 µg/ml for an impurity named A. The limits of detection and quantification were respectively 0.07 and 0.3 µg/ml for impurity A, with a 20 µL injection volume. The precision achieved for all analyses performed provided RSD inter-day equal to 6.47 and 6.36% for impurity A with isocratic elution and gradient, respectively. The accuracy was higher than 99% and robustness exhibited satisfactory results. In the isocratic method an analysis time of 25 min and 15 min was obtained for gradient. For impurity A, the number of theoretical plates in the isocratic mode was about 5000 while in the gradient mode it was about 45000, hence, it made the column more efficient by changing the mobile phase composition during elution. In besifloxacin raw material and in pharmaceutical product used in this study, other related impurities were present but but impurity A was searched for and not detected Conclusion: The proposed methods can be applied for quantitative determination of impurities in the analysis of the besifloxacin raw material, as well as in ophthalmic suspension of the drug, considering the quantitation limit.

Re-challenging antibiotic resistance with Daniel Berman

2020 ◽  
Author(s):  
Daniel Berman
Keyword(s):  
Bacterial Infections ◽  
Point Of Care ◽  
Healthcare Setting ◽  
Rapid Diagnostic Tests ◽  
Resistant Bacteria ◽  
Drug Resistant ◽  
Drug Resistant Bacteria ◽  
Global Threat ◽  
The Right ◽  
Point Of Care Tests

How can we prevent the rise of resistance to antibiotics? In this video, Daniel Berman,  Nesta Challenges, discusses the global threat of AMR and how prizes like the Longitude Prize can foster the development of rapid diagnostic tests for bacterial infections, helping to contribute towards reducing the global threat of drug resistant bacteria. Daniel outlines how accelerating the development of rapid point-of-care tests will ensure that bacterial infections are treated with the most appropriate antibiotic, at the right time and in the right healthcare setting.

Separation and Determination of Some Aromatic Sulfones by Reversed-Phase High-Performance Liquid Chromatography

1994 ◽  
Vol 59 (3) ◽  
pp. 569-574 ◽  
Author(s):  
Josef Královský ◽  
Marta Kalhousová ◽  
Petr Šlosar
Keyword(s):  
High Performance Liquid Chromatography ◽  
Liquid Chromatography ◽  
Mobile Phase ◽  
High Performance ◽  
Reversed Phase ◽  
Uv Spectra ◽  
Optimum Conditions ◽  
Linear Calibration ◽  
Technical Grade

The reversed-phase high-performance liquid chromatography of some selected, industrially important aromatic sulfones has been investigated. The chromatographic behaviour of three groups of aromatic sulfones has been studied. The optimum conditions of separation and UV spectra of the sulfones and some of their hydroxy and benzyloxy derivatives are presented. The dependences of capacity factors vs methanol content in mobile phase are mentioned. The results obtained have been applied to the quantitative analysis of different technical-grade samples and isomer mixtures. For all the separation methods mentioned the concentration ranges of linear calibration curves have been determined.

scholarly journals Analysis of some pharmaceuticals in the presence of their synthetic impurities by applying hybrid micelle liquid chromatography

2020 ◽  
Vol 18 (1) ◽  
pp. 377-390
Author(s):  
Dina El Sherbiny ◽  
Mary E. K. Wahba
Keyword(s):  
Liquid Chromatography ◽  
Sodium Dodecyl Sulfate ◽  
Phosphoric Acid ◽  
Mobile Phase ◽  
Sodium Dodecyl ◽  
Uv Detection ◽  
Stability Indicating ◽  
Photolytic Degradation ◽  
Amino Phenol ◽  
The Stability

AbstractA stability-indicating hybrid micelle liquid chromatography accompanied by UV detection was developed for the simultaneous analysis of either paracetamol (PCA) or pseudoephedrine hydrochloride (PSU) with their synthetic impurities. Mixture I contains PCA with p-amino phenol and p-nitro phenol, while mixture II involves the estimation of PSU with benzaldehyde and benzoic acid. Both mixtures were separated using a C18 column that was thermostatically maintained at 40°C and operating under a flow rate of 1.5 mL/min, applying UV detection at 240 nm for mixture I and 220 nm for mixture II. In both cases, the mobile phase consisted of 0.1 M sodium dodecyl sulfate, acetonitrile, and triethylamine (90:10:0.3, v/v/v) and adjusted to pH 4 (mixture I) or pH 3.7 (mixture II) using 2.0 M O-phosphoric acid. The proposed method was validated and successfully applied to assay different pharmaceuticals containing PCA or PSU. Moreover, the stability-indicating nature of the proposed method was proved through applying photolytic degradation procedures for PCA.

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