scholarly journals Ruggedness testing of an HPLC method for the determination of ciprofloxacin

2005 ◽  
Vol 70 (7) ◽  
pp. 979-986 ◽  
Author(s):  
Predrag Sibinovic ◽  
Andreja Smelcerovic ◽  
Radosav Palic ◽  
Sinisa Djordjevic ◽  
Valentina Marinkovic
Keyword(s):  
Aqueous Phase ◽  
Mobile Phase ◽  
Limit Of Detection ◽  
Pharmaceutical Preparations ◽  
Hplc Method ◽  
Optimal Conditions ◽  
Column Temperature ◽  
Limit Of Quantitation ◽  
Peak Areas ◽  
Ruggedness Testing

The possibility of optimization of an HPLC method for the determinations of ciprofloxacin and ciprofloxacin impurity C was investigated according to the British Pharmacopoeia, using ruggedness testing. Four factors were selected to be tested in this ruggedness test (temperature of the column, volume of acetonitrile in the mobile phase, volume of the aqueous phase in the mobile phase and pH of the aqueous phase in the mobile phase). Seven responses were determined in each design experiment: retention times, peak heights, peak widths, number of theoretical plates, peak areas, peak areas RSD (%) and selectivity. A three-level design was used. The optimal conditions for the chromatographic procedure determined as the result of ruggedness testing were: pH of the aqueous phase in the mobile phase 3.0, column temperature 42 ?C and the acetonitrile to aqueous ratio in the mobile phase 14: 86 (v/v). The HPLC method using the optimal conditions was tested for selectivity linearity, precision, accuracy, limit of quantitation and limit of detection. The applicability of the suggested method was, as well, tested on the stability of ciprofloxacin in pharmaceutical preparations (tablets and infusion solution, products of Zdravlje-Pharmaco, Serbia) under stress stability data.

scholarly journals A Fast and Validated HPLC Method for Simultaneous Determination of Dopamine, Dobutamine, Phentolamine, Furosemide, and Aminophylline in Infusion Samples and Injection Formulations

2021 ◽  
Vol 2021 ◽  
pp. 1-9
Author(s):  
Fuchao Chen ◽  
Baoxia Fang ◽  
Sicen Wang
Keyword(s):  
Mobile Phase ◽  
Dosage Form ◽  
Limit Of Detection ◽  
Hplc Method ◽  
Stability Study ◽  
Precision Data ◽  
Column Temperature ◽  
Ich Guidelines ◽  
Limit Of Quantitation ◽  
The Stability

A simple, fast, and validated HPLC method was developed for the simultaneous quantization of five cardiovascular agents: dopamine (DPM), dobutamine (DBM), phentolamine (PTM), furosemide (FSM), and aminophylline (APL) either in infusion samples or in an injection dosage form. The proposed method was achieved with a 150 mm × 4.6 mm, 5.0 μm C18 column, by using a simple linear gradient. Mobile phase A was buffer (50 mM KH2PO4) and mobile Phase B was acetonitrile at a flow rate of 1.0 mL/min. The column temperature was kept at 30°C, and the injection volume was 20 μL. All analytes were separated simultaneously at a retention time (tr) of 3.93, 5.84, 7.06, 8.76, and 9.67 min for DPM, DBM, PTM, FSM, and APL, respectively, with a total run time of less than 15.0 min. The proposed method was validated according to ICH guidelines with respect to accuracy, precision, linearity, limit of detection, limit of quantitation, and robustness. Linearity was obtained over a concentration range of 12.0–240.0, 12.0–240.0, 20.0–200.0, 6.0–240.0, and 10.0–200.0 μg/mL DPM, DBM, PTM, FSM, and APL, respectively. Interday and intraday accuracy and precision data were recorded in the acceptable limits. The new method has successfully been applied for quantification of all five drugs in their injection dosage form, infusion samples, and for evaluation of the stability of investigated drugs in mixtures for endovenous use. The results of the stability study showed that mixtures of DPM, DBM, PTM, FSM, and APL in 5% glucose or 0.9% sodium chloride injection were stable for 48 hours when stored in polypropylene syringes at 25°C.

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.

Development and Validation of Stability-Indicating HPLC Method for Roflumilast and Related Substances

2013 ◽  
Vol 781-784 ◽  
pp. 68-71 ◽  
Author(s):  
Fang Tan
Keyword(s):  
Limit Of Detection ◽  
Degradation Products ◽  
Reversed Phase ◽  
Hplc Method ◽  
Forced Degradation ◽  
Dihydrogen Phosphate ◽  
Column Temperature ◽  
Stability Indicating ◽  
Related Substances ◽  
Limit Of Quantitation

A reversed phase HPLC method was developed and validated for analysis of roflumilast, its related substances and degradation products, using Ecosil C18 column (250×4.6 mm, 5 μm) with a flow rate of 1.0 ml/min and detection wavelength of 215nm. The mobile phase was a mixture of acetonitrile and 0.005mol·L-1ammonium dihydrogen phosphate buffer pH 3.5 in the ratio of 48:52 (v/v). The samples were analyzed using 20 μl injection volume and the column temperature was maintained at 30°C. The limit of detection and limit of quantitation were found to be 2.6 ng/ml and 8ng/ml, respectively. The stability-indicating capability of method was established by forced degradation studies and method demonstrated successful separation of drug, its related substances and degradation products. The method is sensitive, specific, accurate, precise and stability indicating for the quantitation of drug, its related substances and other degradation compounds.

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 Enantioseparation of Citalopram by RP-HPLC, Using Sulfobutyl Ether-β-Cyclodextrin as a Chiral Mobile Phase Additive

2016 ◽  
Vol 2016 ◽  
pp. 1-7 ◽  
Author(s):  
Yangfeng Peng ◽  
Quan Sophia He ◽  
Jiang Cai
Keyword(s):  
Mobile Phase ◽  
Ph Value ◽  
Limit Of Detection ◽  
Dihydrogen Phosphate ◽  
Column Temperature ◽  
Aqueous Buffer ◽  
Rp Hplc ◽  
Chiral Mobile Phase Additive ◽  
Mobile Phase Additive ◽  
Limit Of Quantitation

Enantiomeric separation of citalopram (CIT) was developed using a reversed phase HPLC (RP-HPLC) with sulfobutylether-β-cyclodextrin (SBE-β-CD) as a chiral mobile phase additive. The effects of the pH value of aqueous buffer, concentration of chiral additive, composition of mobile phase, and column temperature on the enantioseparation of CIT were investigated on the Hedera ODS-2 C18column (250 mm × 4.6 mm × 5.0 um). A satisfactory resolution was achieved at 25°C using a mobile phase consisting of a mixture of aqueous buffer (pH of 2.5, 5 mM sodium dihydrogen phosphate, and 12 mM SBE-β-CD), methanol, and acetonitrile with a volumetric ratio of 21 : 3 : 1 and flow rate of 1.0 mL/min. This analytical method was evaluated by examining the precision (lower than 3.0%), linearity (regression coefficients close to 1), limit of detection (0.070 µg/mL for (R)-CIT and 0.076 µg/mL for (S)-CIT), and limit of quantitation (0.235 µg/mL for (R)-CIT and 0.254 µg/mL for (S)-CIT).

scholarly journals Development and Validation of New RP-HPLC Method for Simultaneous Determination of Methyl and Propyl Parabens with Levetiracetam in Pure Form and Pharmaceutical Formulation

2016 ◽  
Vol 2016 ◽  
pp. 1-5 ◽  
Author(s):  
Soad S. Abd El-Hay ◽  
Mostafa S. Mohram
Keyword(s):  
High Performance ◽  
Limit Of Detection ◽  
Degradation Products ◽  
Gradient Elution ◽  
Hplc Method ◽  
Pure Form ◽  
Mobile Phase Flow Rate ◽  
Column Temperature ◽  
Limit Of Quantitation

A simple and robust high-performance liquid chromatography (HPLC) method is described for the assay for levetiracetam (LTC), methyl paraben (MHB), and propyl paraben (PHB) either in their pure form or in commercial Levepsy® syrup. The method is selective and stability indicating and all chromatographic conditions were studied to obtain adequate separation of LTC, MHB, and PHB from their degradation products and from excipients. The HPLC separation was carried out on a RP C18 Hypersil BDS analytical column (150 mm × 4.6 mm ID) using gradient elution system. The mobile phase flow rate was 1.5 mLmin−1 and the column temperature was kept at 40°C. Complete separation of the studied components was obtained within a cycle time of 8 min. LTC, MHB, and PHB were eluted at 1.56, 5.86, and 7.85 min, respectively. Detection was carried out at 240 nm using a dual wavelength detector. The method has been validated for linearity, accuracy, precision, specificity, limit of detection, limit of quantitation, robustness, and ruggedness. The proposed method was successfully applied for the determination of LTC in the presence of parabens in Levepsy syrup.

scholarly journals Development and validation of stability-indicating RP-HPLC method for estimation of dalfampridine in bulk drug and tablet dosage form

2021 ◽  
Vol 7 (1) ◽  
Author(s):  
Dipali Bagal ◽  
Akhil Nagar ◽  
Aditya Joshi ◽  
Aishwarya Chachare ◽  
Atul Shirkhedkar ◽  
...  
Keyword(s):  
Dosage Form ◽  
Limit Of Detection ◽  
Hplc Method ◽  
Stability Study ◽  
Main Peak ◽  
Forced Degradation ◽  
Column Temperature ◽  
Limit Of Quantitation ◽  
Bulk Drug ◽  
Tablet Dosage

Abstract Background In the current study, a simple, improved, precise, rapid, and accurate reverse phase liquid chromatographic method was produced for the estimation of dalfampridine in bulk and tablet dosage form which is a potassium channel blocker used for the treatment of multiple sclerosis (MS). The separation of dalfampridine was achieved isocratically on a C18 column (250 × 4.6 mm, 5 μm) using (0.1% v/v) buffer pH 3.0 ± 0.05 adjusted with diluted orthophosphoric acid (OPA) and acetonitrile (ACN) in the ratio of 60:40% (v/v) as a mobile phase, at a flow rate of 0.5 mL/min, and column temperature of 40 °C. HPLC grade methanol as diluents was used. Five microliters of the standard solution of the drug was injected, and the eluted analytes were detected at 262 nm. Results Dalfampridine was eluted at 4.5 min with a run time of 10 min. Linearity in the method was measured in the concentration range of 25–75 ppm with a correlation coefficient of 0.999. Limit of detection and limit of quantitation were found to be 0.711 μg/mL and 2.154 μg/mL, respectively. Dalfampridine was subjected for forced degradation stability study in conditions of thermal, acid, alkali, and oxidation and photo-degradation condition. The degradants were well resolved from the dalfampridine main peak. Validation of the developed method is carried as per USFDA and ICH guidelines. Conclusion The results of the analysis prove that the method is simple, improved, precise, accurate, and rapid for estimating the content of dalfampridine in bulk drug and tablet dosage form and can be applied for routine analysis.

scholarly journals A Validated RP-HPLC Method for the Determination of Citrinin in Xuezhikang Capsule and otherMonascus-Fermented Products

2012 ◽  
Vol 9 (1) ◽  
pp. 260-266 ◽  
Author(s):  
Li Xue-Mei ◽  
Shen Xing-Hai ◽  
Xue Lan ◽  
Duan Zhen-Wen ◽  
Guo Shu-Ren
Keyword(s):  
Mobile Phase ◽  
Limit Of Detection ◽  
Hplc Method ◽  
Quantitative Detection ◽  
Rp Hplc ◽  
Toxic Product ◽  
Limit Of Quantitation ◽  
Xuezhikang Capsule ◽  
Fermented Products

Citrinin is a toxic product usually produced during theMonascusfermentation. The presence of citrinin in xuezhikang capsule has been a concern due to its ingredient which is derived frommonascus-fermented rice. A rapid and sensitive RP-HPLC method with fluorescence detection at λex= 331 nm and λem= 500 nm for analysis of citrinin inMonascus-fermented products was developed to analyze citrinin inMonascus-fermented products. The chromatography was performed with mobile phase containing acidified water and acetonitrile. The calibration curve was linear (r = 0.9999) over a range of 0.0107- 0.537 μg/mL. The limit of detection (LOD) and the limit of quantitation (LOQ) were 0.187 ng/mL and 0.6 ng/mL respectively. The analysis of xuezhikang capsules using the developed method suggested that the product does not contain detectable citrinin and the result has been further confirmed using independent LC-MS/MS analysis. The proposed method has also been applied to analyze 11 samples of otherMonascus-fermented products. The results suggested that there were no detectable citrinin in 4 of the 11 samples, however citrinin with the levels between 0.10-594 ng/kg has been detected in the other 7 samples. It indicates that the proposed method can also be applied to carry out the quantitative detection of citrinin for otherMonascus-fermented products.

Perbandingan Akrilamidakopi Bubuk Tradisional Dan Luwak Dengan Metode HPLC

2019 ◽  
Vol 4 (2) ◽  
pp. 61
Author(s):  
Ridho Asra ◽  
Rusdi Rusdi ◽  
Sofia Nofianti ◽  
Nessa Nessa
Keyword(s):  
Mobile Phase ◽  
High Performance ◽  
Limit Of Detection ◽  
Hplc Method ◽  
Isocratic Elution ◽  
Roasted Coffee ◽  
Injection Volume ◽  
Limit Of Quantitation ◽  
Safe Limits ◽  
Ground Coffee

<p><em>Akrilamida merupakan senyawa kimia terdapat pada kopi yang disangrai pada suhu diatas 120 ˚C, berpotensi menyebabkan kanker pada manusia. Tujuan dari penelitian ini adalah untuk membandingkan kandungan akrilamida dalam kopi bubuk tradisional dan kopi  luwak dengan metode Kromatografi Cair Kinerja Tinggi.  Fase gerak yang digunakan asetonitril: aquabidest (15: 85, v/v), dengan detektor Photodioday-Array (PDA) pada ℷ   200 nm. Akrilamida dalam sampel kopi bubuk teridentifikasi pada waktu retensi (tR) ± 6,8 menit. Metode ini terbukti valid dengan linearitas y = 356468 + 293761 x, koefisien korelasi (r) = 0,9993, batas deteksi 1,9901 µg/mL dan batas kuantitasi 6,6337 µg/mL, presisi dengan % SBR = 0,207 %, akurasi dengan % perolehan kembali kopi bubuk tradisional dan kopi bubuk luwak 99 % dan 104 %. Kadar akrilamida dalam sampel kopi bubuk 1 sampai 6 berturut-turut adalah 1115 ± 12,17 µg/g sampel (1), 687 ± 7,58  µg/g sampel (2), 1461 ± 63,89 µg/g sampel (3), 221 ± 3,54 µg/g sampel (4), 128 ± 3,24 µg/g sampel (5), 195 ± 1 µg/g sampel (6). Dari keenam sampel kopi bubuk menunjukkan bahwa kadar akrilamida masing-masing sampel berkisar antara 128 sampai 1461 µg/g. Kadar yang diperoleh melebihi batas aman konsumsi akrilamida yang dikeluarkan oleh WHO</em></p><p><em><br /></em></p><p><em><em>Acrylamide is a chemical compound found in roasted coffee at temperatures above 120 ˚C which can potentially cause cancer in humans. The purpose of this research was to analyze acrylamide contents in traditional ground coffee and civet ground coffee by using High Performance Liquid Chromatography (HPLC) method. This analysis was carried out by isocratic elution system, the mobile phase of acetonitrile : aquabidest (15 : 85, v/v), using the stationary phase of the Shimadzu Shimpack ODS C18 column (250 × 4.6 mm), flow rate of 0.5 mL/minute, injection volume 20 µL, with a Photodioday-Array (PDA) detector at a wavelength of 200 nm. Acrylamide in ground coffee samples was identified at retention time (tR) ± 6.8 minutes. This method is proved valid with the linearity y = 356468 + 293761 x, correlation coefficient (r) = 0.9993, limit of detection 1.9901 µg / mL and limit of quantitation 6.6337 µg / mL, precision with % RSD = 0.207 %, acuracy with % recovery of traditional ground coffee and luwak ground coffee 99 % and 104 %. Acrylamide levels in 1 to 6 ground coffee samples in a row is 1115 ± 12.17 µg / g samples (1), 687 ± 7.58 µg / g samples (2), 1461 ± 63.89 µg / g samples (3), 221 ± 3.54 µg / g sample (4), 128 ± 3.24 µg / g sample (5), 195 ± 1 µg / g sample (6). Of the six ground coffee samples showed that the acrylamide levels of each sample ranged from 128 to 1461 µg / g. The levels obtained exceed the safe limits of acrylamide consumption released by WHO</em></em></p>

scholarly journals A Reversed-Phase HPLC Method for Determination of Osteopontin in Infant Formula

2019 ◽  
Vol 9 (18) ◽  
pp. 3711 ◽  
Author(s):  
Md Abdul Wazed ◽  
Mohammed Farid
Keyword(s):  
High Performance ◽  
Limit Of Detection ◽  
Reversed Phase ◽  
Hplc Method ◽  
Milk Formula ◽  
Reversed Phase Hplc ◽  
Column Temperature ◽  
System Suitability ◽  
Relative Standard ◽  
Limit Of Quantitation

Osteopontin (OPN) is a multifunctional whey protein which has recently received much attention for possibly applications in fortifying infant milk formula (IMF) with its bioactivity. However, to date, there is no established high-performance liquid chromatography (HPLC) method to quantify this protein in milk or IMF. In this study, a rapid, simple, isocratic and reliable reversed-phase HPLC method was developed and validated to quantify the OPN in IMF. A C18 column (4.6 × 150 mm × 5 micron) was employed with 20% of 0.1% trifluoroacetic acid (TFA) and 80% of 60% acetonitrile in 0.1% TFA for 10 min detected at 214 nm. The flow rate was 0.3 mL/min with an injection volume of 10 µL. The column temperature was 40 °C, and the peak appeared after 4 min. The validation was based on the system suitability, linearity (r2 = 0.999), limit of detection (LOD) (0.14 mg/L), limit of quantitation (LOQ) (0.41 mg/L), precision (% relative standard deviation (RSD) < 0.2), recovery (% RSD < 3) and robustness. The results confirm that the method developed is suitable for OPN determination in IMF.

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