Determination of Phenicols Using a Fast and Reliable HPLC Method Developed on Hypercarb Stationary Phase

2017 ◽  
Vol 68 (3) ◽  
pp. 545-548
Author(s):  
Georgeta Simona Stan ◽  
Florentina Moldovanu ◽  
Irinel Adriana Badea
Keyword(s):  
Stationary Phase ◽  
Mobile Phase ◽  
Reliable Method ◽  
Limit Of Detection ◽  
Hplc Method ◽  
Detection Capability ◽  
Milk Samples ◽  
Precision And Accuracy ◽  
Detection And Quantification

Hypercarb porous graphitic stationary phase was used to develop a fast and reliable method for simultaneous determination of chloramphenicol, thiamphenicol and florfenicol. The separation was achieved in 7 min elution being made isocratic using water modified with acetonitrile as mobile phase. The method was fully validated and showed good linearity, precision and accuracy. Limit of detection and quantification together with decision limit and detection capability were established. This method was applied for analysis of milk samples.

QUANTITATIVE DETERMINATION OF CURCUMIN IN TURMERIC POWDER AND TURMERIC–HONEY BALL PILLS BY HPLC

2018 ◽  
Vol 8 (4) ◽  
pp. 42-47
Author(s):  
Tien Nguyen Huu ◽  
Tram Le Thi Bao ◽  
Ngoc Nguyen Thi Nhu ◽  
Thang Phan Phuoc ◽  
Khan Nguyen Viet
Keyword(s):  
Acetic Acid ◽  
Gastric Mucosa ◽  
Quantitative Determination ◽  
Mobile Phase ◽  
Curcuma Longa ◽  
Biological Marker ◽  
Hplc Method ◽  
Chromatography Analysis ◽  
Precision And Accuracy

Background: Curcumin is a major ingredient in turmeric (Curcuma longa L., Zingiberaceae), which has important activities such as anti-tumor, anti-inflammatory, antioxidant, anti-ischemia, protection of gastric mucosa etc,. Curcumin can be considered as a biological marker of turmeric and turmeric products. Objectives: Developing an HPLC method for quantification of curcumin in turmeric powder and turmeric - honey ball pills; applying this method for products on the market. Materials and methods: turmeric powder and turmeric - honey ball pills collected in Thua Thien Hue province. After optimization process, the method was validated and applied to evaluate the content of curcumin. Results: The chromatography analysis was performed with: Zorbaz Eclipse XDB-C18 (150 × 4.6 nm; 5 µm); Mobile phase: acetonitril: 2% acetic acid (45:55), Flow rate was kept constant at 1.0 ml/min; Detector PDA (420 nm). The method was validated for the HPLC system compatibility, specificity, linearity range, precision and accuracy; the recovery greater than 98%. Conclusion: The developed HPLC method can determine curcumin in turmeric powder and turmeric - honey ball pills. Key words: Curcumin, turmeric powder, turmeric-honey ball pills, quantitative determination, HPLC

scholarly journals Box-Behnken Assisted Validation and Optimization of an RP-HPLC Method for Simultaneous Determination of Domperidone and Lansoprazole

Separations ◽  
2021 ◽  
Vol 8 (1) ◽  
pp. 5
Author(s):  
Mohd Afzal ◽  
Mohd. Muddassir ◽  
Abdullah Alarifi ◽  
Mohammed Tahir Ansari
Keyword(s):  
Flow Rate ◽  
Mobile Phase ◽  
Limit Of Detection ◽  
Hplc Method ◽  
Box Behnken Design ◽  
Rp Hplc ◽  
System Suitability ◽  
Method Optimization ◽  
Key Variables

A highly specific, accurate, and simple RP-HPLC technique was developed for the real-time quantification of domperidone (DOMP) and lansoprazole (LANS) in commercial formulations. Chromatographic studies were performed using a Luna C8(2), 5 μm, 100Å, column (250 × 4.6 mm, Phenomenex) with a mobile phase composed of acetonitrile/2 mM ammonium acetate (51:49 v/v), pH 6.7. The flow rate was 1 mL·min−1 with UV detection at 289 nm. Linearity was observed within the range of 4–36 µg·mL−1 for domperidone and 2–18 µg·mL−1 for lansoprazole. Method optimization was achieved using Box-Behnken design software, in which three key variables were examined, namely, the flow rate (A), the composition of the mobile phase (B), and the pH (C). The retention time (Y1 and Y3) and the peak area (Y2 and Y4) were taken as the response parameters. We observed that slight alterations in the mobile phase and the flow rate influenced the outcome, whereas the pH exerted no effect. Method validation featured various ICH parameters including linearity, limit of detection (LOD), accuracy, precision, ruggedness, robustness, stability, and system suitability. This method is potentially useful for the analysis of commercial formulations and laboratory preparations.

scholarly journals SENSITIVE DETERMINATION OF RELATED SUBSTANCES IN PIOGLITAZONE HYDROCHLORIDE BY HPLC

2017 ◽  
Vol 9 (2) ◽  
pp. 34
Author(s):  
N. Balaji ◽  
Sayeeda Sultana
Keyword(s):  
Mobile Phase ◽  
High Performance ◽  
Limit Of Detection ◽  
High Performance Liquid Chromatographic ◽  
Hplc Method ◽  
Internal Diameter ◽  
Related Substances ◽  
Relative Standard ◽  
Limit Of Quantitation

Objective: An efficient, high performance liquid chromatographic method has been developed and validated for the quantification of related substances in pioglitazone hydrochloride drug substance.Methods: This method includes the determination of three related substances in pioglitazone hydrochloride. The mobile phase A is 0.1% w/v triethylamine in water with pH 2.5 adjusted by dilute phosphoric acid. The mobile phase B is premixed and degassed mixtures of acetonitrile and methanol. The flow rate was 1 ml/min. The elution used was gradient mode. The HPLC column used for the analysis was symmetry C18 with a length of 250 mm, the internal diameter of 4.6 mm and particle size of 5.0 microns.Results: The developed method was found to be linear with the range of 0.006-250% with a coefficient of correlation 0.99. The precision study revealed that the percentage relative standard deviation was within the acceptable limit. The limit of detection and limit of quantitation of the impurities was less than 0.002%and 0.006% with respect to pioglitazone hydrochloride test concentration of 2000 µg/ml respectively. This method has been validated as per ICH guidelines Q2 (R1).Conclusion: A reliable, economical HPLC method was magnificently established for quantitative analysis of related substances of pioglitazone hydrochloride drug substance.

scholarly journals Photostability study of amlodipine besylate tablets packed in primary packaging

2021 ◽  
Vol 10 (1) ◽  
pp. 20-28
Author(s):  
Ivana Savić-Gajić ◽  
Ivan Savić ◽  
Predrag Sibinović ◽  
Valentina Marinković
Keyword(s):  
Mobile Phase ◽  
Limit Of Detection ◽  
Degradation Products ◽  
Hplc Method ◽  
Coefficient Of Determination ◽  
Amlodipine Besylate ◽  
Limit Of Quantification ◽  
First Order Kinetics ◽  
The Given

In this study, the modified stability-indicating RP-HPLC method was validated for quantitative analysis of amlodipine besylate in the presence of its impurity D (3-ethyl 5-methyl 2-[(2-aminoethoxy)methyl]-4-(2-chlorophenyl)-6-methylpyridine-3,5-dicarboxylate). The method was applied for the determination of an analyte in the tablets and irradiated samples packed in the primary packaging (Alu/PVC/PVDC blister packaging). The efficient chromatographic separation was achieved using a ZORBAX Eclipse XDB-C18 column (4.6×250 mm, 5 mm) with isocratic elution of mobile phase which consisted of acetonitrile:methanol:triethylamine solution (15:35:50, v/v/v) (pH 3.0). The flow rate of the mobile phase was 1 mL min-1, while the detection of amlodipine besylate was carried out at 273 nm. Amlodipine besylate and its impurity D were identified at the retention times of 16.529 min and 2.575 min, respectively. The linearity of the method with the coefficient of determination of 0.999 was confirmed in the concentration range of 10 - 75 µg mL-1 for amlodipine besylate. The limit of detection was 0.2 µg mL-1, while the limit of quantification was 0.66 µg mL-1. After UV and Vis radiation of the tablets packed in the primary packaging, the content of amlodipine besylate was reduced by 22.38% and 19.89%, respectively. The presence of new degradation products was not detected under the given chromatographic conditions. The photodegradation of amlodipine besylate followed pseudo-first-order kinetics. Based on the half-life of amlodipine besylate (38.4 days for UV radiation and 43.3 days for Vis radiation), it was concluded that amlodipine besylate in the tablets has satisfactory photostability after its packing in the Alu/PVC/PVDC blister packaging.

scholarly journals Determination of New Antidepressants in Pharmaceuticals by Thin-Layer Chromatography with Densitometry

2010 ◽  
Vol 93 (3) ◽  
pp. 778-782 ◽  
Author(s):  
Tatána Gondová ◽  
Iveta Petríková
Keyword(s):  
Thin Layer ◽  
Stationary Phase ◽  
Thin Layer Chromatography ◽  
Mobile Phase ◽  
Pharmaceutical Formulations ◽  
Simultaneous Separation ◽  
Tlc Plates ◽  
Precision And Accuracy ◽  
Layer Chromatography

Abstract A new and simple TLC-densitometry method has been developed for the simultaneous separation of the two noradrenergic and specific serotonergic antidepressants mirtazapine and mianserine and validated for their determination in commercially available tablets. The method used TLC plates precoated with silica gel 60F254 as the stationary phase, and the mobile phase consisted of hexaneisopropanol25 ammonia (70 + 25 + 5, v/v/v). Densitometric analysis was carried out in the absorbance mode at 280 nm. The method was validated in accordance with International Conference on Harmonization guidelines in terms of linearity, LOD, LOQ, precision, and accuracy. Calibration curves were linear (R2 > 0.9970) with respect to peak area in the concentration range of 5002500 and 5005000 ng/spot for mirtazapine and mianserine, respectively. The LODs were 20 and 35 ng/spot for mirtazapine and mianserine, respectively. The described method was successfully applied to the determination of mirtazapine and mianserine in their pharmaceutical formulations with recovery ranging from 99.83 to 101.20 of the labeled amount of the compounds. The proposed method can be used in routine QC of these drugs in pharmaceutical formulations.

scholarly journals Development and application of a validated HPLC method for the analysis of dissolution samples of mexiletine hydrochloride capsules

2010 ◽  
Vol 75 (7) ◽  
pp. 975-985 ◽  
Author(s):  
Dragan Milenovic ◽  
Zoran Todorovic
Keyword(s):  
Flow Rate ◽  
Mobile Phase ◽  
Hplc Method ◽  
Uv Detection ◽  
In Vitro Dissolution ◽  
Selective Method ◽  
Dissolution Studies ◽  
Detection And Quantification

The aim of this work was to develop and validate a simple, efficient, sensitive and selective method for the analysis of dissolution samples of mexiletine hydrochloride capsules by HPLC without the necessity of any time-consuming extraction, dilution or evaporation steps prior to drug assay. Separation was performed isocratically on a 5 ?m LiChrospher 60, RP-Select B column (250 x 4 mm ID) using the mobile phase buffer-acetonitrile (60:42, v/v) at a flow rate of 1.2 mL min-1 and UV detection at 262 nm. The elution occurred in less than 10 minutes. The assay was linear in the concentration range 50-300 ?g mL-1 (r2 = 0.9998). The validation characteristics included accuracy, precision, linearity, specificity, limits of detection and quantification, stability, and robustness. Validation acceptance criteria were met in all cases (the percent recoveries ranged between 100.01 and 101.68 %, RSD < 0.44 %). The method could be used for the determination of mexiletine hydrochloride and for monitoring its concentration in in vitro dissolution studies.

Sensitive and Fast Determination of Ceftiofur in Honey and Veterinary Formulation by HPLC-UV Method with Pre-column Derivatization

2020 ◽  
Vol 59 (1) ◽  
pp. 15-22
Author(s):  
Noha Rashed ◽  
Sahar Zayed ◽  
Fatma Fouad ◽  
Amany Abdelazeem
Keyword(s):  
Present Method ◽  
Mobile Phase ◽  
High Performance ◽  
Limit Of Detection ◽  
Hplc Method ◽  
Fast Determination ◽  
Factors Affecting ◽  
Limit Of Quantitation ◽  
Derivatization Reaction

Abstract A novel, sensitive and rapid high performance liquid chromatography (HPLC) method for the determination of ceftiofur by pre-column derivatization with 1,2-naphthoquinone-4-sulfonate. Analysis was performed within 5 min on a Kinetex C18 column based on core-shell technology. The mobile phase composed of acetonitrile-water (50:50, v/v) pumped isocratically at a flow rate of 1.0 mL/min under UV detection at 254 nm. The factors affecting the derivatization reaction and separation conditions were carefully evaluated and optimized. The method was linear over the concentration range of 45–450 ng/mL with a limit of detection of 3.29 ng/mL and limit of quantitation of 10.97 ng/mL. The new method was successfully applied for the analysis of ceftiofur in the veterinary formulation and honey with average recoveries of 100.78% and 98. 83%, respectively. The present method is suitable and favorable for the analysis of ceftiofur on account of its sensitivity, rapidity and cost-effectiveness. In addition, it could have significant application for the determination of ceftiofur in other food products.

scholarly journals DEVELOPMENT AND VALIDATION OF RP-HPLC METHOD FOR THE ESTIMATION OF ESCITALOPRAM OXALATE AND FLUPENTIXOL DIHYDROCHLORIDE IN COMBINED DOSAGE FORM AND PLASMA

2021 ◽  
pp. 61-66
Author(s):  
MALATHI SELLAPPAN ◽  
DARTHI DEVAKUMAR
Keyword(s):  
Mobile Phase ◽  
Dosage Form ◽  
Limit Of Detection ◽  
Hplc Method ◽  
Accuracy And Precision ◽  
Relative Standard ◽  
Photodiode Array ◽  
Development And Validation ◽  
Potassium Dihydrogen Orthophosphate

Objective: The objective of the study was to develop a simple and rapid chromatographic method for quantification of escitalopram oxalate and flupentixol dihydrochloride in combined dosage form and plasma. Methods: The separation was achieved with a sun fire C8 [150×4.6 mm] 3.5 µm column with an isocratic mobile phase containing a mixture of potassium dihydrogen orthophosphate buffer: methanol: acetonitrile [30:60:10 v/v/v] pH adjusted to 11. The flow rate of the mobile phase was 1.5 ml/min with a Photodiode array [PDA] detection at 230 nm. Results: The HPLC method was developed and validated with respective linearity, accuracy, and precision, detection of limit, robustness, and specificity. The precision of the results stated as the relative standard deviation was below 2 %. The calibration curve was linear over a concentration range from 10-50 µg/ml for escitalopram oxalate and 1-5 µg/ml for flupentixol dihydrochloride with a correlation co-efficient 0.994 and 0.977 respectively. The accuracy of the method was demonstrated at levels in the range of 100 % and 120 % of the specification limit. The recovery of escitalopram oxalate and flupentixol dihydrochloride was found to be in the range of 90 % to 88 %, respectively. The lowest detection limits were found to be 2 µg/ml for escitalopram oxalate and 0.1 µg/ml for flupentixol dihydrochloride. The lowest quantification limits were found to be 5 µg/ml of escitalopram oxalate and 0.5 µg/ml of flupentixol dihydrochloride. Conclusion: The developed method was validated for linearity, accuracy, precision, the limit of detection and quantification, specificity. The method was applied successfully for the determination of escitalopram oxalate and flupentixol dihydrochloride in the combined dosage form and plasma.

scholarly journals Method validation for simultaneous quantification of whey proteins in dietary supplements by HPLC

2019 ◽  
Vol 2 (1) ◽  
pp. 32-38
Author(s):  
Hong Ngoc Nguyen Thi ◽  
Thanh Hoa Mac Thi ◽  
Thanh An Vu Thi ◽  
Thanh Ha Pham Thi ◽  
Khanh Cao Cong ◽  
...  
Keyword(s):  
Dietary Supplements ◽  
Simultaneous Determination ◽  
Method Validation ◽  
Mobile Phase ◽  
Whey Proteins ◽  
Hplc Method ◽  
Simultaneous Quantification ◽  
Precision And Accuracy ◽  
Beta Lactoglobulin

A HPLC method has been validated for simultaneous determination of Alpha-lactalbumin (&alpha;-&nbsp;LA) and Beta- lactoglobulin (&beta;-LG) contents in dietary supplements by HPLC-PDA. The method&nbsp;was carried out in C18 column with a gradient of 0.1% TFA/ water &ndash; 0.1% TFA/ acetonitrile as&nbsp;mobile phase. The proteins were detected at 215 nm wavelength within 50 minutes. The method&nbsp;was validated in specificity, linearity, precision and accuracy; and then was applied to analyze several random dietary supplements.

scholarly journals A simple isocratic RP-HPLC method for quality control of oseltamivir capsules

2012 ◽  
Vol 31 (2) ◽  
pp. 205
Author(s):  
Agim Ameti ◽  
Jasmina Slavkovska ◽  
Katerina Starkoska ◽  
Zorica Arsova-Sarafinovska
Keyword(s):  
Mobile Phase ◽  
Limit Of Detection ◽  
Degradation Products ◽  
Reversed Phase ◽  
Hplc Method ◽  
Sample Treatment ◽  
Limit Of Quantification ◽  
Elution Time ◽  
Rp Hplc

A simple isocratic reversed-phase high performance liquid chromatographic (RP-HPLC) method was developed for determination of oseltamivir active pharmaceutical ingredient (API) in bulk drug and pharmaceuticals. The separation was achieved on a Purospher STAR® RP – 18e column with a mobile phase consisting of methanol- 0.02 mol l-1 phosphate buffer, pH 5, 50:50 (v/v). Chromatographic results demonstrated the specificity of the method for determination of oseltamivir in presence of degradation products generated in studies of forced decomposition. The limit of detection (LOD) and limit of quantification (LOQ) for oseltamivir phosphate were 0,0162 μg ml-1 and 0,0491 μg ml-1, respectively. The advantages of this method include simple sample treatment and short elution time (less than 6 min). Furthermore, using methanol instead of acetonitrile in a mobile phase composition considerably reduces the laboratory expenses, still retaining adequate sensitivity for routine analysis as well as for evaluation of potentially counterfeit Tamiflu® products. 

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