scholarly journals A Validated LC Method for Separation and Determination of Tetralone-4-O-β-D-Glucopyranoside and 4-Hydroxy-α-Tetralone in Ammannia multiflora

2012 ◽  
Vol 2012 ◽  
pp. 1-4 ◽  
Author(s):  
Harish C. Upadhyay ◽  
Ram K. Verma ◽  
Santosh K. Srivastava
Keyword(s):  
Quality Control ◽  
Flow Rate ◽  
Control Method ◽  
Hplc Method ◽  
Assay Method ◽  
Good Linearity ◽  
Rp Hplc ◽  
Quality Control Method ◽  
Calibration Curves

A rapid, sensitive, and reproducible RP-HPLC method was developed for the determination of two constituents in Ammannia multiflora, namely, tetralone-4-O-β-D-glucopyranoside (1) and 4-hydroxy-α-tetralone (2). The samples were separated on a Spherisorb ODS2 column (250×4.6 mm, i.d., 10 μm) and binary elution of water and methanol (2 : 3) with flow rate of 0.8 mL/min at λ 254 nm. The LOD and LOQ were found 0.05 and 0.18 μg/mL for compound 1 and 0.06 and 0.18 μg/mL for compound 2, respectively. All calibration curves showed good linearity (r2>0.999) within test ranges for both the analytes. The RSD values for intra-and inter-day precisions were less than 1.1%. The successful application of the developed method on five different samples revealed an average 0.0206% and 0.7636% (w/w) of compounds 1 and 2, respectively in A. multiflora indicating that the developed LC assay method may be readily utilized as a quality control method for the plant.

scholarly journals RP - HPLC Method for Determination of Piperine fromPiper longumLinn. andPiper nigrumLinn

2005 ◽  
Vol 2 (2) ◽  
pp. 131-135 ◽  
Author(s):  
M. K. Santosh ◽  
D. Shaila ◽  
I. Rajyalakshmi ◽  
I. Sanjeeva Rao
Keyword(s):  
Mobile Phase ◽  
Control Method ◽  
Hplc Method ◽  
Piper Nigrum ◽  
Detector Response ◽  
Piper Longum ◽  
Rp Hplc ◽  
Quality Control Method ◽  
Detection And Quantification

Piper longumLinn. andPiper nigrumLinn. are used as spices and medicines. Quantitative determination of piperine was undertaken to provide an easy and simple analytical method, which can be used as a routine quality control method. RP-HPLC was performed using methanol and water as mobile phase. The detection and quantification was performed at a wavelength of 345 nm. Linearity of detector response for piperine was between the concentrations 0.005% to 0.1%. The correlation coefficient obtained for the linearity was 0.998. The assay value of piperine for fruit and root ofP. longumwas found to be 0.879% and 0.31%. The assay value of piperine for fruit ofP. nigrumwas 4.5%. The recovery value of standard piperine was 99.4%. Low value of standard deviation and coefficient of variation are indicative of high precision of the method.

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 Development and Validation of a GMP-Compliant High-Pressure Liquid Chromatography Method for the Determination of the Chemical and Radiochemical Purity of [18F]PSMA-1007, a PET Tracer for the Imaging of Prostate Cancer

2021 ◽  
Vol 14 (3) ◽  
pp. 188
Author(s):  
Ines Katzschmann ◽  
Heike Marx ◽  
Klaus Kopka ◽  
Ute Hennrich
Keyword(s):  
Prostate Cancer ◽  
Quality Control ◽  
Radiochemical Purity ◽  
Control Method ◽  
Solid Phase ◽  
Hplc Method ◽  
Attractive Alternative ◽  
Chromatography Method ◽  
Pet Tracer

For the PET imaging of prostate cancer, radiotracers targeting the prostate-specific membrane antigen (PSMA) are nowadays used in clinical practice. [18F]PSMA-1007, a radiopharmaceutical labeled with fluorine-18, has excellent properties for the detection of prostate cancer. Essential for the human use of a radiotracer is its production and quality control under GMP-compliance. For this purpose, all analytical methods have to be validated. [18F]PSMA-1007 is easily radiosynthesized in a one-step procedure and isolated using solid phase extraction (SPE) cartridges followed by formulation of a buffered injection solution and for the determination of its chemical and radiochemical purity a robust, fast and reliable quality control method using radio-HPLC is necessary. After development and optimizations overcoming problems in reproducibility, the here described radio-HPLC method fulfills all acceptance criteria—for e.g., specificity, linearity, and accuracy—and is therefore well suited for the routine quality control of [18F]PSMA-1007 before release of the radiopharmaceutical. Recently a European Pharmacopeia monograph for [18F]PSMA-1007 was published suggesting a different radio-HPLC method for the determination of its chemical and radiochemical purity. Since the here described method has certain advantages, not least of all easier technical implementation, it can be an attractive alternative to the monograph method. The here described method was successfully validated on several radio-HPLC systems in our lab and used for the analysis of more than 60 batches of [18F]PSMA-1007. Using this method, the chemical and radiochemical purity of [18F]PSMA-1007 can routinely be evaluated assuring patient safety.

scholarly journals RP-HPLC Determination of Raloxifene in Pharmaceuticl Tablets

2006 ◽  
Vol 3 (1) ◽  
pp. 60-64 ◽  
Author(s):  
P. Venkata Reddy ◽  
B. Sudha Rani ◽  
G. Srinu Babu ◽  
J. V. L. N. Seshagiri Rao
Keyword(s):  
Flow Rate ◽  
Retention Time ◽  
Mobile Phase ◽  
Dosage Forms ◽  
Hplc Method ◽  
Reverse Phase Hplc ◽  
Reverse Phase ◽  
Pharmaceutical Dosage Forms ◽  
Rp Hplc

A reverse phase HPLC method is developed for the determination of Raloxifene in pharmaceutical dosage forms. Chromatography was carried out on an inertsil C18 column using a mixture of acetonitrile and phosphate buffer (30:70 v/v) as the mobile phase at a flow rate of 1 mL/min. Detection was carried out at 290 nm .The retention time of the drug was 10.609 min. The method produced linear responses in the concentration range of 0.5-200 µg/mL of Raloxifene. The method was found to be applicable for determination of the drug in tablets.

scholarly journals Quality-control method for the determination of biological activity of engineered calcineurin subunit B

2016 ◽  
Vol 59 (6) ◽  
pp. 584-588
Author(s):  
Xinchang Shi ◽  
Huan Yang ◽  
Li Xu ◽  
Xiang Li ◽  
Zongwen Huang ◽  
...  
Keyword(s):  
Quality Control ◽  
Biological Activity ◽  
Control Method ◽  
Quality Control Method ◽  
Subunit B

scholarly journals A Validated RP-HPLC Method for Simultaneous Estimation of Ciprofloxacin and Flucionolone in Pharmaceutical Formulation

2018 ◽  
Vol 6 (03) ◽  
pp. 48-51
Author(s):  
D. Mamatha ◽  
G. Naveen ◽  
Devi Singh
Keyword(s):  
Theoretical Plate ◽  
Hplc Method ◽  
Pharmaceutical Formulation ◽  
Assay Method ◽  
Plate Count ◽  
Simultaneous Estimation ◽  
Rp Hplc ◽  
Ich Guidelines ◽  
Validation Parameters

A simple, accurate, precise and sensitive RP-HPLC assay method have been validated for the simultaneous estimation of ciprofloxacin and flucionolone in pharmaceutical formulation by RP-HPLC .ciprofloxacin and flucionolone is separated using Develosil ODS HG-5 RP C18, 5μm, 15cmx4.6mm i.d. column at a flow rate of 0.8 ml/ min. Here resolution was good, theoretical plate count and symmetry was appropriate .The LOD and LOQ were calculated using statistical methods. The % RSD values were less than 1.The validation parameters, tested in accordance with the requirements of ICH guidelines, prove the suitability of this method. The method was successfully applied for determination of drug in tablets, wherein no interference from tablet excipients was observed, indicating the specificity of the developed method.The proposed method was found to be simple, precise, accurate, rapid, economic and reproducible for the estimation of ciprofloxacin and flucionolone in pharmaceutical formulation.

Validated Chromatographic Methods for Simultaneous Estimation of Cinnarizine in Binary Mixture with Domperidone and Paracetamol in Tablets

2019 ◽  
Vol 15 (5) ◽  
pp. 429-438
Author(s):  
Marianne Alphonse Mahrouse ◽  
Asmaa Ahmed El-Zaher ◽  
Ahmed Mohammed Al-Ghani
Keyword(s):  
Quality Control ◽  
Hplc Method ◽  
Simultaneous Estimation ◽  
Chromatographic Methods ◽  
Treatment And Prevention ◽  
Rp Hplc ◽  
Linear Relationships ◽  
Ich Guidelines ◽  
Analytical Tools

Background:Cinnarizine, an antihistaminic drug, is commonly formulated in combination with domperidone and with paracetamol for treatment and prevention of motion sickness and migraine.Objective:The aim of this work was to develop new, simple, precise and selective chromatographic methods (RP-HPLC and TLC-densitometric methods) for the determination of these drugs. These methods can be used as analytical tools in the routine examination in quality control laboratories.Methods:The first method was RP-HPLC method, the separation was carried out on an Inertsil® ODS- 3V C18 column (250 mm × 4.6 mm, 5 µm) using a mobile phase composed of methanol: acetonitrile (45: 55, v/v) at a flow rate of 1 ml/min. The detection was carried out at 220 nm. The second method was a TLC-densitometric method where the studied components were separated using a developing system composed of toluene: ethyl acetate: methanol: triethylamine (5: 4.3: 0.7: 0.5, v/v/v/v) on TLC silica gel 60 F254 plates, followed by densitometric scanning at 270 nm.Results:In RP-HPLC method, the peaks were sharp and well separated, the retention times were 5.25, 3.48 and 2.78 min, for cinnarizine, domperidone and paracetamol, respectively. Linearity was obtained over the concentration ranges 1-22, 0.75-16.5 and 25-550 µg/ml, for cinnarizine, domperidone and paracetamol, respectively. In TLC-densitometric method, good separation of spots and linear relationships were achieved over the concentration ranges of 0.2-2, 0.15-1.5 and 5-50 µg/spot, for cinnarizine, domperidone and paracetamol, respectively. Method validation was conducted according to ICH guidelines in terms of linearity, accuracy, selectivity, precision and robustness.Conclusion:The developed methods were applied for the determination of the cited drugs in tablets containing binary drug mixtures. The methods are simple and precise and can be used for routine analysis of the labelled drugs in combined dosage forms in quality control laboratories.

Degradation Profiling of Lisinopril and Hydrochlorothiazide by RP- HPLC method with QbD Approach

2021 ◽  
pp. 270-274
Author(s):  
Kalleshvar P. Jatte ◽  
R. D. Chakole ◽  
M. S. Charde
Keyword(s):  
Particle Size ◽  
Quality Control ◽  
Flow Rate ◽  
Mobile Phase ◽  
Dosage Form ◽  
Quality By Design ◽  
Hplc Method ◽  
Rp Hplc ◽  
Tablet Dosage ◽  
Gradient Mode

RP-HPLC method was developed for the estimation of Lisinopril and Hydrochlorothiazide in tablet dosage form with the help of Quality by Design (QbD) approaches. In this method concentration of each drug was obtained by using the absorptivity values calculated for drug wavelength 226.0 nm and solving the equation. The RP-HPLC method was performed C18-(100mm x 4.6 mm,)2.5 μm particle size in gradient mode, and the sample was analysed using methanol 45.0 ml and 55.0 ml (pH 3.3 0.05% OPA with TEA) as a mobile phase at a flow rate of 0.8 ml/min and detection at nm. By the retention time for Lisinopril and Hydrochlorothiazide found 3.39 and 4.59 min respectively. Validation related the method is specific, rapid, accurate, precise, reliable, and reproducible. Calibration plots by both HPLC were linear over the 5-25 and 12.5-62.5 μg/ml for Lisinopril and Hydrochlorothiazide respectively, and recoveries from tablet dosage form were between 99.02 and 100.00 %. The method can be used for routine of the quality control in pharmaceuticals. The degradation profiling of Lisinopril and Hydrochlorothiazide were also carried out.

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