scholarly journals DEVELOPMENT AND VALIDATION OF HIGH-PERFORMANCE THIN LAYERCHROMATOGRAPHIC METHOD FOR CIPROFLOXACIN BY QUALITY BY DESIGN APPROACH

2021 ◽  
pp. 39-43
Author(s):  
SHRADDHA V TATHE ◽  
MORESHWAR P MAHAJAN ◽  
RASHMI G PINJARKAR ◽  
ARUN M KASHID
Keyword(s):  
Risk Assessment ◽  
High Performance ◽  
Quality By Design ◽  
Limit Of Detection ◽  
Uv Light ◽  
Linear Regression Analysis ◽  
Limit Of Quantification ◽  
Factor Screening ◽  
Validation Parameters ◽  
Time Band

Objective: The aim of this paper is to create a new, systematic high-performance thin-layer chromatography (HPTLC) method for ciprofloxacin that is based on quality by design (QbD). Methods: The mobile phase was chloroform: IPA: H2O: Formic Acid (2:7:0.5:0.5V/V), and the chromatographic separation was performed on aluminum-backed silica gel 60 F254 plates. Ciprofloxacin was detected using UV light at 278nm. In factor screening studies, a 3-factor 17-run standard 3-level factorial design was used, and a Box-Behnken design was used to optimize HPTLC experimental parameters for obtaining anticipated chromatographic conditions. The basic method parameters were tested to understand risk assessment. Three independent parameters, such as saturation time, band duration, and migration distance, were chosen and analyzed based on the risk assessment to see if these three parameters influenced the responses. For ciprofloxacin, the method produces a compact and well-resolved band at Rf = 0.40 0.02. In the linear regression analysis performed on ciprofloxacin, the regression coefficient was found to be r2 = 0.996. Results: According to the International Council on Harmonization (ICH) guidelines, it was validated for validation parameters such as accuracy, precision, robustness, the limit of detection, and the limit of quantification. The proposed method for ciprofloxacin determination was found to be straightforward, precise, reliable, stable, and sensitive. Conclusion: The QbD method produced a more robust method that can generate accurate, high-quality, and reliable data during the process, and it can be effectively used in the routine inspection of Ciprofloxacin in the tablets dosage form.

Nanoparticulate Mycophenolic Acid Eye Drops - Analytical Validation of a High Performance Liquid Chromatography Assay and Stability Studies

2021 ◽  
Vol 09 ◽  
Author(s):  
Ali Al-Kulabi ◽  
Louis Gooden ◽  
Ijeoma F. Uchegbu
Keyword(s):  
Mycophenolic Acid ◽  
High Performance ◽  
Limit Of Detection ◽  
Immunosuppressive Agent ◽  
Plate Count ◽  
Eye Drops ◽  
Limit Of Quantification ◽  
Drug Content ◽  
Relative Standard ◽  
Validation Parameters

Background: Mycophenolic acid (MPA), an immunosuppressive agent, is used orally to reduce corneal graft rejection. However its oral use is associated with gastrointestinal side effects. Objectives: To prepare MPA nanoparticle eye drops and a validated analytical method. Methods: Aqueous MPA eye drops were prepared by nanoencapsulation of MPA using Nanomerics MET (N-palamitoylN-monomethyl-N,N-dimethyl-N,N,N-trimethyl-6-O-glycolchitosan) at a MET, MPA ratio of 7.5: 1 g g-1 in the presence of glycerol (2.75% w/w). A validated MPA in-formulation drug substance assay was then developed. Results: MET-MPA formulations were prepared as well as a validated assay. Assay validation parameters for the analysis of MPA in the formulation were satisfactory [Plate count = 16458, Capacity Factor = 2.4, Tailing Factor = 1.02, linearity = 0.999 (0.016 – 0.5 mg mL-1 ), limit of detection = 0.056 mg mL-1 , limit of quantification = 0.17 mg mL-1 , accuracy = 98%, intraday and interday relative standard deviation = 0.45% and 4% respectively]. The candidate formulation (z - average mean = 66 ± 0.4 nm, polydispersity index = 0.12 ± 0.012, drug content = 1.14 ± 0.003 mg mL-1 , zeta potential = +8.5 ± 1.4 mV, pH = 7.4 ± 0.02, osmolarity = 309 ± 1.5 mOSm L-1 , viscosity = 1.04 ± 0.001 mPa.s) was then found to be stable for 14 days with respect to drug content at refrigeration, room and accelerated (40C )temperature and. All other formulation parameters were within the ocular comfort range. Conclusions: A validated assay (ICH and US FDA guidelines) for new MPA nanoparticle eye drops has been developed.

scholarly journals NOVEL RP-HPLC METHOD DEVELOPMENT AND VALIDATION FOR ESTIMATION OF TELMISARTAN AND NEBIVOLOL HCL IN PHARMACEUTICAL DOSAGE FORM

2018 ◽  
Vol 11 (9) ◽  
pp. 431 ◽  
Author(s):  
Heena Ar Shaikh ◽  
Vandana Jain
Keyword(s):  
High Performance ◽  
Dosage Form ◽  
Method Development ◽  
Limit Of Detection ◽  
Hplc Method ◽  
Limit Of Quantification ◽  
Pharmaceutical Dosage Form ◽  
Rp Hplc ◽  
Validation Parameters ◽  
Hplc Method Development

Objective: A simple, accurate, precise, robust reverse phase high performance liquid chromatography (RP-HPLC) method was developed for the estimation of telmisartan and nebivolol hydrochloride (HCl) simultaneously in its combined dosage form.Methods: The compounds were well resolved in an isocratic method using the mobile phase composition of acetonitrile: Buffer (potassium dihydrogen orthophosphate pH adjusted 3.1 with orthophosphoric acid) in a ratio of 40:60 v/v at a flow rate of 1.2 ml/min using C18 Shim-pack (150 mm × 4.6 mm, 5 μ) column. The detection was carried out at 280 nm.Results: The retention time of telmisartan and nebivolol HCl was 4.8 min and 6.5 min, respectively. The developed method was validated by evaluating various validation parameters such as linearity, precision, accuracy, robustness, specificity, limit of detection, and limit of quantification according to the international council for harmonization guidelines. The standard calibration curve was obtained in the concentration range of 24–56 μg/ml for telmisartan and 3–7 μg/ml for nebivolol HCl. The overall average % recovery was found out to be 100.35 for telmisartan and 98.84 for nebivolol HCl.Conclusion: Statistical analysis of the data showed that the method is reproducible and selective for the estimation of telmisartan and nebivolol HCl. The proposed method could be used for analysis of telmisartan and nebivolol HCl in their dosage form.

scholarly journals ESTIMATION OF GUGGULSTERONE-Z IN GOKSHURADI GUGGULU USING REVERSED-PHASE HIGH-PERFORMANCE LIQUID CHROMATOGRAPHY

2018 ◽  
Vol 11 (11) ◽  
pp. 204
Author(s):  
Kanan G Gamit ◽  
Niraj Y Vyas ◽  
Nishit D Patel ◽  
Manan A Raval
Keyword(s):  
High Performance Liquid Chromatography ◽  
Liquid Chromatography ◽  
High Performance ◽  
Limit Of Detection ◽  
Reversed Phase ◽  
Array Detector ◽  
Limit Of Quantification ◽  
Photodiode Array Detector ◽  
Validation Parameters ◽  
Photodiode Array

Objective: A study was aimed to estimate guggulsterone-Z (GZ) in Gokshuradi Guggulu (GG).Methods: An analytical method was developed and validated using Waters Alliance high-performance liquid chromatography system (Empower software), equipped with photodiode array detector. Separation was achieved using Phenomenex, C-18 (250 mm×4.6 mm, 5 μ) column. Mobile phase consisted of acetonitrile:water (70:30,v/v). Flow rate was set to 1 ml/min and detection was performed at 251 nm.Results and Discussion: Validation parameters such as linearity, precision, accuracy, limit of detection, limit of quantification, and robustness were performed. Amount of GZ was estimated using linearity equation.Conclusion: GG was found to contain 0.815±0.03 g% w/w GZ. Validated method may be used as one of the parameters to standardize the formulation.

scholarly journals Research Article on Development and Validation of RP-HPLC Method for Estimation of Canagliflozin

2019 ◽  
Vol 11 (02) ◽  
pp. 85-92
Author(s):  
Gudipally. Mounika ◽  
K. Bhavya Sri ◽  
R. Swethasri ◽  
M. Sumakanth
Keyword(s):  
Retention Time ◽  
High Performance ◽  
Limit Of Detection ◽  
Hplc Method ◽  
Limit Of Quantification ◽  
Chromatography Method ◽  
Pharmaceutical Dosage Form ◽  
Validation Parameters ◽  
Liquid Chromatography Method ◽  
Development And Validation

To develop an accurate, precise, specific high performance liquid chromatography method for quantification of Canagliflozin in bulk and dosage forms. A C18 column (250mm X 4.6mm; 5μm phenomenex) was used with mobile phase containing Acetonitrile-0.1% sodium acetate buffer (pH-4.6), (20:80) in isocratic mode. The flow rate maintained was 1.0ml/min and the U.V detector was operated at 291nm. The retention time of Canagliflozin was 3.307min and showed a good linearity in concentration range of 2-14μg/ml with correlation coefficient of 0.999. The average percent recovery was found to be 99.98%. The developed method follows validation parameters such as system suitability, linearity, precision, accuracy, limit of detection and limit of quantification and robustness as per ICH guidelinesQ2(R1). The proposed method was found to provide faster retention time with sharp resolution with linearity at a lowest concentration as compared to previous methods and this method is validated as per International conference on harmonization guidelines and successfully applied for bulk and pharmaceutical dosage form.

Chromatographic Separation of Fluoroquinolone Drugs and Drug Degradation Profile Monitoring through Quality-by-Design Concept

2020 ◽  
Vol 59 (1) ◽  
pp. 55-63
Author(s):  
Satya Prasad Asu ◽  
Naveen Kumar Sompalli ◽  
Akhila Maheswari Mohan ◽  
Prabhakaran Deivasigamani
Keyword(s):  
High Performance ◽  
Quality By Design ◽  
Limit Of Detection ◽  
Profile Monitoring ◽  
Limit Of Quantification ◽  
Antimicrobial Drugs ◽  
Statistical Tool ◽  
Drug Degradation ◽  
Tablet Formulations ◽  
Factorial Design Of Experiments

Abstract The article reports on the development of an efficient, robust and sensitive HPLC-DAD method for the simultaneous determination of five fluoroquinolone-based antimicrobial drugs, namely ciprofloxacin, moxifloxacin, norfloxacin, ofloxacin and pefloxacin in both aquatic and tablet formulations. The robustness of the high-performance liquid chromatography with diode-array detection (HPLC-DAD) method has been evaluated through the concepts of quality-by-design (QbD) and full factorial design of experiments (DoEs), using a Minitab 17 statistical tool. The proposed method offers sequential separation with well-defined peak shape and resolution, and has also been evaluated by following international council for harmonization (ICH) pharmaceutical guidelines. A linear signal response has been achieved for the target fluoroquinolones (FQ) drugs in the concentration range of 45–20,000 ng/mL, with an average correlation coefficient (r2) value of 0.9997, and a data precision and accuracy range of 99.3–100.9%, with an RSD value of ≤0.95%, for hexaplicate measurements. The methodology offers superior sensitivity for the target FQ drugs, with the limit of detection (LD) range of 10–25 ng/mL, and the limit of quantification (LQ) range of 51–86 ng/mL, respectively. Using the proposed method, the article carries the first of its kind report in studying the degradation profile monitoring and drug assay determination in tablet formulations and under various physiological buffer stress conditions, for pharmaceutical validation.

Quantification of Newly Discovered Anti-Cancer Drug Enzalutamide in Bulk and Synthetic Mixture by Stability Indicating TLC Method

2019 ◽  
Vol 16 (1) ◽  
pp. 104-112
Author(s):  
Dharmendra Jayantibhai Prajapati ◽  
Usmangani Khalilurraheman Chhalotiya ◽  
Minesh Dahyabhai Prajapati ◽  
Jalpa Upendrabhai Patel ◽  
Jaineel Vinodrai Desai
Keyword(s):  
High Performance ◽  
Limit Of Detection ◽  
Linear Regression Analysis ◽  
Analysis Data ◽  
Solvent System ◽  
Chemical Oxidation ◽  
Synthetic Mixture ◽  
Cancer Drug ◽  
Limit Of Quantification ◽  
Stability Indicating

Objective: An impressionable, discriminatory and precise stability indicating high performance thin layer chromatographic method has been developed and validated for the estimation of Enzalutamide in bulk and synthetic mixture. Method: The method engaged HPTLC aluminium plates pre-coated with silica gel 60F-254 as the stationary phase while the solvent system was ethyl acetate: toluene (4.5:5.5, v/v). The Rf value of enzalutamide was detected to be 0. 39 &amp;#177; 0. 005 and the densitometric analysis was carried out in absorbance mode at 246 nm. The linear regression analysis data for the calibration plots presented a virtuous linear relationship for enzalutamide over a concentration range of 20 - 1000ng/band. Results: The limit of detection and limit of quantification for enzalutamide was found to be 9.05 and 27.43 ng/band. Enzalutamide was imperilled to acid and alkali hydrolysis, chemical oxidation, dry heat degradation and photolytic degradation. The degraded product peaks were well resolved from the pure drug peak with substantial difference in their Rf values. Conclusion: Stressed samples were assayed using developed TLC technique. Suggested method was validated with respect to linearity, accuracy, precision and robustness. The method was successfully applied to the estimation of enzalutamide in synthetic mixture.<P&gt;

scholarly journals Development of a Rapid and Eco-Friendly UHPLC Analytical Method for the Detection of Histamine in Fish Products

2020 ◽  
Vol 17 (20) ◽  
pp. 7453
Author(s):  
Antonello Cicero ◽  
Francesco Giuseppe Galluzzo ◽  
Gaetano Cammilleri ◽  
Andrea Pulvirenti ◽  
Giuseppe Giangrosso ◽  
...  
Keyword(s):  
High Performance ◽  
Limit Of Detection ◽  
Array Detector ◽  
Proficiency Tests ◽  
Limit Of Quantification ◽  
Relative Standard ◽  
Validation Parameters ◽  
Fish And Fishery Products ◽  
Short Time ◽  
Solid Liquid

We developed, validated, and confirmed with proficiency tests a fast ultra-high-performance liquid chromatography with diode array detector (UHPLC-DAD) method to determine histamine in fish and fishery products. The proposed method consists of two successive solid–liquid extractions: one with a dilute solution of perchloric acid (6%) and the second only with water. The instrumental analysis with UHPLC provides a very fast run time (only 6 min) with a retention time of approximately 4 min, a limit of quantification (LOQ) of 7.2 mg kg−1, a limit of detection (LOD) of 2.2 mg kg−1, a recovery around 100%, a relative standard deviation (RSD%) between 0.5 and 1.4, and an r2 of calibration curve equal to 0.9995. The method detected optimal values of the validation parameters and required a limited number of reagents in comparison to other methods reported in the literature. Furthermore, the method could detect histamine in a very short time compared with other methods. This method, in addition to being validated, precise, specific, and accurate, avoids wasting time, money, and resources, and limits the use of organic solvents.

scholarly journals Development and Validation of RP-HPLC-PDA Method for the Analysis of Diclofenac Sodium in the In Vitro Transdermal Permeation Samples

2019 ◽  
Vol 9 (2) ◽  
pp. 212-216 ◽  
Author(s):  
Saisrianusha Valluru ◽  
Buchi N Nalluri
Keyword(s):  
High Performance ◽  
Limit Of Detection ◽  
Skin Permeation ◽  
Diclofenac Sodium ◽  
Hplc Method ◽  
Limit Of Quantification ◽  
Validation Parameters ◽  
In Vitro Skin Permeation ◽  
Development And Validation

A new analytical method using high-performance liquid chromatography coupled with photo diode array detection was developed and validated for the quantification of Diclofenac (DIC) from in vitro skin permeation samples. Analysis was performed using a Phenomenex C18 column (150 x 4.6mm, 5µm) with 10mM ammonium acetate: Acetonitrile (62:38% v/v) as the mobile phase in isocratic mode and eluents were monitored at 276nm. DIC was eluted at 3.1min and showed a good linearity in the concentration range of 0.2-3µg/mL with a correlation coefficient >0.999. The validation parameters, such as specificity, linearity, accuracy and limit of detection, limit of quantification, precision, robustness fulfilled the regulatory requirements. The developed HPLC method was successfully used for the analysis of DIC in samples obtained from transdermal diffusate samples.

Determination of patulin and hydroxymethylfurfural in beverages by UPLC-PDA

2020 ◽  
pp. 1-8
Author(s):  
M. Pernica ◽  
J. Martiník ◽  
R. Boško ◽  
V. Zušťáková ◽  
K. Benešová ◽  
...  
Keyword(s):  
High Performance ◽  
Limit Of Detection ◽  
Penicillium Expansum ◽  
Limit Of Quantification ◽  
Accuracy And Precision ◽  
Relative Standard ◽  
Validation Parameters ◽  
Photodiode Array ◽  
Quantification Accuracy

The present study describes using molecularly imprinted polymer (MIP) technology for determination of patulin (PAT) and 5-hydroxymethylfurfural (5-HMF) in beverages by ultra-high performance liquid chromatography coupled to photodiode array (UPLC-PDA). PAT (4-hydroxy-4H-furo[3,2-c]pyran-2(6H)-one) is a mycotoxin produced by Penicillium fungi and Penicillium expansum is probably the most commonly encountered species that infects apples during their growth, harvest, storage or processing. The occurrence of PAT as a natural contaminant of apples is a worldwide problem. 5-HMF (also known as 5-(hydroxymethyl) furan-2-carbaldehyde), is formed in the Maillard reaction as well as during caramelisation. It is a good storage time-temperature marker and flavour indicator, especially in beverages such as wine, beer, but also cider and apple juice which may contain PAT. PAT and 5-HMF were separated within 2 min using a Luna Omega C18 column and the PDA detector wavelength was set to 276 nm. The validation parameters of the analytical method such as linearity, limit of detection, limit of quantification, accuracy and precision were tested. The calibration curves were linear at least in the range 50-1000 ng/ml with a good linearity (R2>0.999) for both analytes, the limit of detection and the limit of quantification for PAT and 5-HMF were in the range 4.9-6.6 and 16.1-21.8 μg/l, respectively. The recoveries of the selected analyte were in the range 61.9-109.0% with a precision of <8.2% (relative standard deviation (RSD)) for PAT and in the range 50.8-98.0% with a precision of <10.0% (RSD) for 5-HMF. The validated procedure was successfully applied for the analysis of PAT and 5-HMF in beverages from retail shops.

scholarly journals Challenges of HPLC Method Development and Validation for the Assay of Bemotrizinol from Complex Matrix in Cosmeceutical Preparation

2020 ◽  
Vol 11 (03) ◽  
pp. 310-316
Author(s):  
Kallol S Jana ◽  
Beduin Mahanti
Keyword(s):  
Mobile Phase ◽  
High Performance ◽  
Method Development ◽  
Limit Of Detection ◽  
Linear Regression Analysis ◽  
Cost Effective ◽  
Analysis Data ◽  
Hplc Method ◽  
Limit Of Quantification ◽  
Relative Standard

A simple high performance liquid chromatography (HPLC) method was developed for the assay of bemotrizinol (Tinosorb-S) from the complex pharmaceutical cosmetics matrix. Unlike the existing methods, the proposed mobile phase used in this method is very simple and excluding buffer. The use of buffer reducing column longevity and also a time-consuming process which increases the cost of analysis. To overcome all the referred problems, the present article was developed and validated as per International Council for Harmonization (ICH) guidelines. The reverse-phase chromatography was performed on Shimadzu model no. SPD-M10A VP with LC solution software, μBondapack (3.9 × 300 mm, 10-micron particle size) column with methanol (100%) as mobile phase at a flow rate 2.5 mL per minutes and UV detection at 254 nm. The retention time of bemotrizinol was found in 17.599 minutes, and the linear regression analysis data for the calibration plots showed a good linear relationship in the concentration range 70 to 130 μg/mL. The value of the correlation coefficient, slope, and intercept were 0.996, 7,715, and 15,320, respectively. The limit of quantification (LoQ) and limit of detection (LoD) were found to be 1.32 and 0.44, respectively. The relative standard deviation (RSD) for intra-day sample A 1.0858, sample B 0.8859, and inter-day sample A 0.9921, sample B 0.967 which were found to be lesser than 2%. The developed method was validated with regard to linearity, accuracy, precision, selectivity, and robustness, and the method was found to be simple, cost-effective, precise, accurate, linear, and specific for the successful identification and determination of bemotrizinol in pharmaceutical cosmetic preparation.

Sign in / Sign up

Export Citation Format

Share Document