A NEW INVESTIGATIONAL METHOD FOR QUANTIFICATION AND VALIDATION OF ANALYTICAL METHOD FOR CEFIXIME AND ERDOSTEINE BY UPLC WITH PHOTO DIODE ARRAY DETECTOR IN BULK AND FORMULATION. APPLICATION TO THE ESTIMATION OF PRODUCT TRACES

INDIAN DRUGS ◽  
2021 ◽  
Vol 57 (11) ◽  
pp. 52-62
Author(s):  
Mohanrao Tammisetty ◽  
Challa balasekhara Reddy ◽  
Puttagunta Srinivasa Babu

Specific and innovative method was developed and validated for the identification and quantification of cefixime and erdosteine in the bulk and formulation samples by UPLC with PDA detector.The analytical technique was with buffer (pH: 7.0): methanol, (65:35%, v/v) using the Sunfire C18, 5μ, 46mmX150mm analytical column with analysis time of six minutes. Flow of mobile phase through the column was 1.0 mL/min. Sample volume was 10 μL. Detection was carried at 254 nm in photo diode array detector. The retention times of cefixime and erdosteine were 2.012 min and 3.122 min., respectively. The curve indicates that correlation coefficient (r2) was superior by having the value 1.000 with linear range of 20.0 ng/mL-200.0 ng/mL for Cefixime and 30 ng/mL-300.0 ng/mL for erdosteine. The correlation coefficient (r2) for erdosteine found 1.000. The LoQ for cefixime and erdosteine was 20ng/mL and 30ng/mL respectively. The LOD for cefixime and erdosteine was 1.0 ng/mL and 1.5 ng/mL respectively. The developed method was applied for the bulk and formulation and equipement cleaning sample.

2006 ◽  
Vol 89 (1) ◽  
pp. 139-143 ◽  
Author(s):  
Maria Helena Iha ◽  
Myrna Sabino

Abstract A method was developed and validated in-house for the determination of patulin (PAT), a toxic mold metabolite, in apple juice. The sample was extracted with ethyl acetatehexane and analyzed by liquid chromatography equipped with a C18 column and diode array detector. The mobile phase used for the quantification was waterethanol, at a flow rate of 0.5 mL/min. The method showed a mean recovery of 84.8%, the relative standard deviation obtained in the precision study was <7.7%, the quantification and detection limits were 7 and 3 μg/L, respectively, and the linear range for PAT in apple juice was 2.6650 μg/L. The ruggedness was evaluated by an intralaboratory experiment, in which 5 factors were studied, and only one was found to influence the observed results. The developed method is fast, practical, and simple; the solvents (except hexane) and reagents used were nontoxic. The results of the validation confirmed the efficiency of the method, which is sensitive enough to be used in studies required to quantify PAT in apple juice.


1996 ◽  
Vol 42 (5) ◽  
pp. 761-765
Author(s):  
J B Pappas ◽  
E M Allen ◽  
M Ross ◽  
W Banner

Abstract Amrinone (AMR), a bipyridine derivative, is receiving increasing use in postoperative cardiac patients as an inotrope and vasodilator. The hemodynamic response to amrinone in adults is linearly related to AMR concentrations, warranting therapeutic drug monitoring. We report a rapid microsample HPLC method for monitoring AMR and its principal metabolites, N-acetyl (N-ac) and N-glycolyl (N-gly) AMR. Serum was precipitated with acetonitrile, and the supernatant fluid was then injected into a C18 narrow-bore column. The mobile phase consisted of a 0.1 mol/L sodium phosphate buffer (pH 6) with a gradient of acetonitrile going from 50 to 100 mL/L of eluent. Detection with a diode-array detector (DAD) concurrently monitored the absorbances at 320 and 345 nm. Monitoring 320 nm allows optimal quantification of AMR, N-gly, and N-ac. Patients often receive concurrent cephalosporin therapy, which is detectable at 320 nm but not 345 nm. Because cephalosporins coelute with AMR or metabolites, monitoring at 345 nm allows separation of these antibiotics from AMR and metabolites while retaining a detection limit of 0.5 mg/L.


Molecules ◽  
2019 ◽  
Vol 25 (1) ◽  
pp. 40 ◽  
Author(s):  
Kang Ma ◽  
Xiaojia Li ◽  
Yiwen Zhang ◽  
Fei Liu

In China, white spirit is not only an alcoholic drink but also a cultural symbol. A novel and accurate method for simultaneously determining nine sweeteners (most authorized for use in China) in white spirits by ultrahigh performance liquid chromatography (UHPLC) with a photo-diode array detector (PDA) and charged aerosol detector (CAD) was developed. The sweeteners were acesulfame, alitame, aspartame, dulcin, neotame, neohesperidine dihydrochalcone, saccharin, sodium cyclamate, and sucralose. The sweeteners were separated within 16 min using a BEH C18 column and linear gradient-elution program. The optimized method allowed low concentrations (micrograms per gram) of sweeteners to be simultaneously detected. The CAD gave good linearities (correlation coefficients > 0.9936) for all analytes at concentrations of 0.5 to 50.0 μg/g. The limits of detection were 0.16 to 0.77 μg/g. Acesulfame, dulcin, neohesperidine dihydrochalcone, and saccharin were determined using the PDA detector, which gave correlation coefficients > 0.9994 and limits of detection of 0.16 to 0.22 μg/g. The recoveries were 95.1% to 104.9% and the relative standard deviations were 1.6% to 3.8%. The UHPLC-PDA-CAD method is more convenient and cheaper than LC-MS/MS methods. The method was successfully used in a major project called “Special Action against Counterfeit and Shoddy white spirits” and to monitor risks posed by white spirits in China.


2014 ◽  
Vol 989-994 ◽  
pp. 1060-1063
Author(s):  
Xiao Gong ◽  
Xiao Bing Huang ◽  
Yong Hua Wei ◽  
Ning Li Qi ◽  
Li Jing Lin ◽  
...  

A simple and sensitive ultra-performance convergence chromatography system coupled with a diode array detector for analysis of paclitaxel, 10-deacetyl-7-epipaclitaxel and cephalomannine in paclitaxel injection was developed. The analyses were carried out on a Waters Acquity UPC2 BEH 2-EP using the mobile phase of mixture of supercritical CO2 and methanol with a linear gradient elution from 92:8 to 82:18 at 50 °C. The method offers good linearity, higher resolution, and good repeatability. LOD and LOQ were 0.45 and 1.32 ng, respectively.


Foods ◽  
2021 ◽  
Vol 10 (1) ◽  
pp. 191
Author(s):  
Cristina Cebrián-Tarancón ◽  
José Oliva ◽  
Miguel Ángel Cámara ◽  
Gonzalo L. Alonso ◽  
M. Rosario Salinas

Nowadays, the techniques for the analysis of glycosidic precursors in grapes involve changes in the glycoside structure or it is necessary the use of very expensive analytical techniques. In this study, we describe for the first time an approach to analyse intact glycosidic aroma precursors in grapes by high-performance liquid chromatography with a diode array detector (HPLC-DAD), a simple and cheap analytical technique that could be used in wineries. Briefly, the skin of Muscat of Alexandria grapes was extracted using a microwave and purified using solid-phase extraction combining Oasis MCX and LiChrolut EN cartridges. In total, 20 compounds were selected by HPLC-DAD at 195 nm and taking as a reference the spectrum of phenyl β-D-glucopyranoside, whose DAD spectrum showed a first shoulder from 190 to 230 nm and a second around 200–360 nm. After that, these glycosidic compounds were identified by High-performance liquid chromatography–quadrupole time-of-flight mass spectrometry (HPLC-qTOF-MS). Disaccharides hexose pentose were the most abundant group observed with respect to the sugars and monoterpendiols the main aglycones found.


INDIAN DRUGS ◽  
2019 ◽  
Vol 56 (08) ◽  
pp. 79-80
Author(s):  
M. S Akhade ◽  
◽  
K. S Laddha

The main aim was to study the variation in vasicine and vasicinone concentration in different marketed cough syrups using HPLC with photo-diode array detector. Since the marketed formulations were containing Adhathoda vasica extract of varying amount, the amount of vasicine, which is the main constituent, deviated extensively. Also a complete and effective extraction method for quantitative estimation of vasicine and vasicinone from these formulations has been developed. Subsequently, based on the results, it was concluded that the need arises to standardize these marketed formulations.


2015 ◽  
Vol 70 (3) ◽  
pp. 369-373
Author(s):  
Jignasu P. Mehta ◽  
Chirag R. Fultariya ◽  
Pravin H. Parmar ◽  
Sohil H. Vadia ◽  
Balubhai A. Golakiya

2012 ◽  
Vol 28 (3) ◽  
pp. 305 ◽  
Author(s):  
Chandrashekara KARUNAKARA ◽  
Udupi APARNA ◽  
Venkateshappa CHANDREGOWDA ◽  
Chandrasekara G. REDDY

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