scholarly journals Optimization of hydrophilic interaction liquid chromatographic method for simultaneous determination of cetylpyridinium chloride and benzocaine in lozenges

2012 ◽  
Vol 31 (1) ◽  
pp. 47 ◽  
Author(s):  
Natalija Nakov ◽  
Jelena Acevska ◽  
Katerina Brezovska ◽  
Rumenka Petkovska ◽  
Aneta Dimitrovska

A new Hydrophilic Interaction Liquid Chromatography (HILIC) method was developed for simultaneous determination of cetylpyridinium chloride and benzocaine as active substances in lozenges. Method development included investigation of the influence of the critical chromatographic conditions such as: type of organic modifier, mobile phase strength, ionic strength and pH value of the buffer used in the mobile phase, as well as experimental determination of dominant mechanism of retention. The optimal chromatographic conditions were obtained using bare silica column and a mobile phase consisting of acetonitrile and ammonium formate (50 mM, pH = 4.0) in ratio 80 : 20 V/V. The method was validated in terms of specificity, linearity, accuracy and precision. The validation results indicate that the proposed HILIC method is suitable for quantitative analysis of cetylpyridinium chloride and benzocaine in lozenges.

2019 ◽  
Vol 15 (6) ◽  
pp. 635-641
Author(s):  
Nadia M. Mostafa ◽  
Ghada M. Elsayed ◽  
Nagiba Y. Hassan ◽  
Dina A. El Mously

Background:The concept of green analytical chemistry prevails due to the growing environmental pollution.Objective:Our attempts are to develop simple and eco-friendly method which is non-harmful to the environment by producing minimal waste. In this context, a green liquid chromatographic method was applied for the simultaneous determination of chlorpheniramine maleate, pseudoephedrine hydrochloride and propyphenazone in their combined dosage form.Methods:Separation was carried out using X select HSS RP C18 analytical column (250 × 4.6 mm, 5μm) using methanol - 0.02 M phosphate buffer pH 3 - triethylamine (60:40: 0.1, by volume) as a mobile phase. The separated peaks were detected at 215 nm at a flow rate 1.0 mL/min.Results:Quantification was done over the concentration ranges of 1-25 µg/mL for chlorpheniramine maleate, 5-35 µg/mL for pseudoephedrine hydrochloride and 10-120 µg/mL for propyphenazone. The suggested method was validated with regard to linearity, accuracy and precision according to the International Conference on Harmonization guidelines with good results.Conclusion:It could be used as a safer alternative for routine analysis of the mentioned drugs in quality control laboratories.


2001 ◽  
Vol 84 (1) ◽  
pp. 24-28 ◽  
Author(s):  
Mythili Nagarajan ◽  
Ted W Waszkuc ◽  
Jidong Sun

Abstract Guggulipid, the standardized product from the extraction of the ole-gum-resin from the Commiphora mukul plant, has been marketed as a hypolipidemic agent. The ketosteroids, cis- and trans-4,17(20)-pregnadiene-3,16-dione, known as E- and Z-guggulsterones, respectively, are the main ingredients in guggulipid. A liquid chromatographic method was developed for simultaneous determination of E- and Z-guggulsterones in guggulipid preparations using synthetic E- and Z-guggulsterone standards. Realtively low amounts of guggulsterones (E and Z) were found in commercial guggulipid preparations in comparison with the manufacturer's claim of 2.5%. The mixture of E- and Z-guggulsterones was extracted and separated on a Symmetry C18 reversed-phase column, with a mobile phase of acetonitrile–water (46 + 54, v/v) and detected at 242 nm. The retention times of E- and Z-guggulsterones are approximately 8 and 11 min, respectively. Assay quantitation was based on the calibration curve obtained from a mixture of synthetic standard E- and Z-guggulsterones. Experimental data on selectivity, linearity, accuracy, and recoveries are presented.


2013 ◽  
Vol 49 (3) ◽  
pp. 521-528 ◽  
Author(s):  
Viviane Benevenuti Silva ◽  
Angel Arturo Gaona Galdos ◽  
Cintia Maria Alves Mothe ◽  
Michele Bacchi Pallastrelli ◽  
Maria Segunda Aurora Prado ◽  
...  

A simple, rapid, economical and reliable high performance liquid chromatographic method has been developed and successfully applied in simultaneous determination of ethinyl estradiol and drospirenone in coated tablets. The HPLC method was performed on a LiChroCART® 100RP column (125x4 mm i.d., 5 µm) with acetonitrile:water 50:50 (v/v) as mobile phase, pumped at a flow rate of 1.0 mL.min-1. The fluorescence detection for ethinyl estradiol was made at λex= 280 nm and λem= 310 nm and a UV detection for drospirenone was made at 200 nm. The elution time for ethinyl estradiol and drospirenone were 4.0 and 5.7 min, respectively. The method was validated in accordance to USP 34 guidelines. The proposed HPLC method presented advantages over reported methods and is suitable for quality control assays of ethinyl estradiol and drospirenone in coated tablets.


1995 ◽  
Vol 78 (6) ◽  
pp. 1474-1480 ◽  
Author(s):  
Guo-Fang Pang ◽  
Yan-Zhong Chao ◽  
Xie-Shan Liu ◽  
Chun-Lin Fan

Abstract A simple and rapid liquid chromatographic (LC) method has been developed for simultaneous determination of 9 pyrethroid insecticides (biphenthrin, cypermethrin, fenpropathrin, fenvalerate, flucythrinate, methothrin, permethrin, py-115, and tetramethrin) in fruits and vegetables. Residues are extracted from crops with methanol and partitioned with toluene. Extracts are cleaned up by Florisil–charcoal column chromatography. LC separation is performed on a μBondapak C18 stainless steel column with acetonitrile–deionized water as mobile phase. The insecticides are detected at 206 nm with 0.03 absorbance unit full scale. Recoveries of 9 pyrethroid insecticides from 6 crops (cucumbers, tomatoes, cabbages, apples, pears, and peaches) fortified at 0.5–5.0 mg/kg were 62.7–129.2%. Detection limits were about 0.05 mg/kg, except for py-115, for which detection limit was 0.10 mg/kg.


2017 ◽  
Vol 2017 ◽  
pp. 1-9 ◽  
Author(s):  
Wafaa A. Zaghary ◽  
Shereen Mowaka ◽  
Moataz S. Hendy

New HPLC-UV method (method A), for simultaneous determination of metformin (MET) and canagliflozin (CANA), was developed and compared to another novel UPLC-UV method (method B) in their tablet combination. Concerning method A, isocratic separation was done by C18 column (100 mm × 2.1 mm, 3 μm) using methanol and 0.03 M phosphate buffer (75:25, v/v) at pH 3.2 as a mobile phase. Meanwhile, chromatographic separation in method B was achieved via Hypersil® gold (50 mm × 2.1 mm, 1.9 μm). Mobile phase was methanol and 0.03 M phosphate buffer at ratio of 80:20  v/v. In both, detection was done at wavelength of 240 nm. Method A showed satisfactory linearity results over 1–50 μg·mL−1 and 0.5–100 μg·mL−1, while method B linearity was at 0.1–50 μg·mL−1 and 0.25–100 μg·mL−1 for CANA and MET, respectively. In terms of accuracy and precision, method A accuracy was 99.81±0.73 and 99.37±0.54, while method B gave accuracy of 99.47±1.03 and 99.73±0.89 for CANA and MET, respectively. For precision, the % RSD was found to be less than 2% for three concentrations analyzed three times. The two methods are convenient for quality laboratories, yet the UPLC method offered the advantage of shorter run times and higher sensitivity.


2011 ◽  
Vol 94 (3) ◽  
pp. 823-832 ◽  
Author(s):  
Fathalla Belal ◽  
Amina M El-Brashy ◽  
Nahed El-Enany ◽  
Manar M Tolba

Abstract A new, specific, and sensitive RP-HPLC method was developed for the simultaneous determination of eprosartan (EPR) and hydrochlorothiazide (HCT). Good chromatographic separation was achieved using a 250 × 4.6 mm id, 5 μm particle size Symmetry® C18 column. The mobile phase acetonitrile–0.1 M phosphate buffer (35 + 65, v/v), pH 4.5, was pumped at a flow rate of 1 mL/min, with UV detection at 275 nm. The method showed good linearity in the ranges of 0.5–50 and 0.1–10 μg/mL, with LOD of 0.06 and 0.02 μg/mL and LOQ of 0.20 and 0.08 μg/mL for EPR and HCT, respectively. The proposed method was successfully applied for the analysis of the studied drugs in their synthetic mixture and co-formulated tablets. The method was further extended to the in vitro and in vivo determination of the two drugs in spiked and real human plasma. Interference likely to be encountered from the co-administered drugs was studied.


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