Development and Validation of an HPLC Method for the Analysis of Flowers of Wild-Growing Primula veris from Epirus, Greece

Planta Medica ◽  
2021 ◽  
Author(s):  
Panagiota-Iro Chintiroglou ◽  
Nikos Krigas ◽  
Paschalina Chatzopoulou ◽  
Anastasia Karioti
Keyword(s):  
Standard Deviation ◽  
Relative Standard Deviation ◽  
2D Nmr ◽  
Hplc Method ◽  
Phytochemical Investigation ◽  
Relative Standard ◽  
Primula Veris ◽  
Chemical Content ◽  
Response Correction ◽  
Development And Validation

AbstractAn HPLC-PDA method was developed for the determination of the flavonoids in the flowers of Primula veris from Epirus, Greece. The aim was to investigate the chemical content of the over-harvested P. veris populations of Epirus and to develop and optimize an extraction protocol to allow fast, exhaustive, and repeatable extraction. Qualitative analysis revealed that the P. veris flowers from Epirus were particularly rich in flavonoids, especially flavonol triglycosides including derivatives of quercetin, isorhamnetin, and kaempferol. A phytochemical investigation of a 70% hydromethanolic extract from the flowers afforded a new flavonoid, namely, isorhamnetin-3-Ο-β-glucopyranosyl-(1 → 2)-β-glucopyranosyl-(1 → 6)-β-glucopyranoside, which is also the main constituent of the flower extracts. Its structure elucidation was carried out by means of 1D and 2D NMR and mass spectrometry analyses. The HPLC-PDA method was developed and validated according to the International Council for Harmonisation guidelines. Since the main flavonol glycoside of the plant is not commercially available, rutin was used as a secondary standard and the response correction factor was determined. Finally, the overall method was validated for precision (% relative standard deviation ranging between 1.58 and 4.85) and accuracy at three concentration levels. The recovery ranged between 93.5 and 102.1% with relative standard deviation values < 5%, within the acceptable limits. The developed assay is fast and simple and will allow for the quality control of the herbal drug.

scholarly journals Development and validation of spectrophotometric method for phenylephrine hydrochloride estimation in nasal drops formulations

2008 ◽  
Vol 27 (2) ◽  
pp. 149 ◽  
Author(s):  
Ivana Savić ◽  
Goran Nikolić ◽  
Vladimir Banković
Keyword(s):  
Standard Deviation ◽  
Sodium Hydroxide ◽  
Relative Standard Deviation ◽  
Spectrophotometric Method ◽  
Molar Absorptivity ◽  
Dosage Forms ◽  
Phenylephrine Hydrochloride ◽  
Relative Standard ◽  
Development And Validation

Simple, accurate and reproducible UV-spectrophotometric method was developed and validated for the estimation of phenylephrine hydrochloride in pharmaceutical nasal drops formulations. Phenylephrine hydrochloride was estimated at 291 nm in 1 mol⋅dm-3 sodium hydroxide (pH 13.5). Beer’s law was obeyed in the concentration range of 10–100 μg⋅cm−3 (r2 = 0.9990) in the sodium hydroxide medium. The apparent molar absorptivity was found to be 1.63×103 dm3⋅mol−1⋅cm−1. The method was tested and validated for various parameters according to the ICH (International Conference on Harmonization) guidelines. The detection and quantitation limits were found to be 0.892 and 2.969 μg⋅cm−3, respectively. The proposed method was successfully applied for the determination of phenylephrine hydrochloride in pharmaceutical nasal drops formulations. The results demonstrated that the procedure is accurate, precise and reproducible (relative standard deviation < 1 %), while being simple, cheap and less time consuming, and hence can be suitably applied for the estimation of phenylephrine hydrochloride in different dosage forms.

Determination of Flavanol and Procyanidin (by Degree of Polymerization 1–10) Content of Chocolate, Cocoa Liquors, Powder(s), and Cocoa Flavanol Extracts by Normal Phase High-Performance Liquid Chromatography: Collaborative Study

2012 ◽  
Vol 95 (4) ◽  
pp. 1153-1160 ◽  
Author(s):  
Rebecca J Robbins ◽  
Jadwiga Leonczak ◽  
Julia Li ◽  
J Christopher Johnson ◽  
Tom Collins ◽  
...  
Keyword(s):  
Standard Deviation ◽  
Relative Standard Deviation ◽  
High Performance ◽  
Collaborative Study ◽  
Hplc Method ◽  
Degree Of Polymerization ◽  
Fluorescent Detection ◽  
Relative Standard ◽  
International Collaborative Study

Abstract An international collaborative study was conducted on an HPLC method with fluorescent detection (FLD) for the determination of flavanols and procyanidins in materials containing chocolate and cocoa. The sum of the oligomeric fractions with degree of polymerization 1–10 was the determined content value. Sample materials included dark and milk chocolates, cocoa powder, cocoa liquors, and cocoa extracts. The content ranged from approximately 2 to 500 mg/g (defatted basis). Thirteen laboratories representing commercial, industrial, and academic institutions in six countries participated in the study. Fourteen samples were sent as blind duplicates to the collaborators. Results from 12 laboratories yielded repeatability relative standard deviation (RSDr) values that were below 10% for all materials analyzed, ranging from 4.17 to 9.61%. The reproducibility relative standard deviation (RSDR) values ranged from 5.03 to 12.9% for samples containing 8.07 to 484.7 mg/g. In one sample containing a low content of flavanols and procyanidins (approximately 2 mg/g), the RSDR was 17.68%. Based on these results, the method is recommended for Official First Action for the determination of flavanols and procyanidins in chocolate, cocoa liquors, powder(s), and cocoa extracts.

scholarly journals HPLC method for analysis of substrate and products in beverage alcohol production

1969 ◽  
Vol 74 (4) ◽  
pp. 357-364
Author(s):  
Eduardo Rosado ◽  
Heriberto Batiz ◽  
Mercedes Vilella
Keyword(s):  
High Performance Liquid Chromatography ◽  
Liquid Chromatography ◽  
Standard Deviation ◽  
Relative Standard Deviation ◽  
High Performance ◽  
Hplc Method ◽  
Alcohol Production ◽  
Relative Standard

A procedure was developed and validated for the determination of sugars by high performance liquid chromatography (HPLC). The system studied consisted of a Sugar-pak column operated continuously and with a methanol flow when not in use, as opposed to manufacturer's instructions, which recommend refrigeration of the column during the weekends when idle. This column is recommended for analysis of sugar products and process streams such as those of beet and sugarcane. Evaluations of this technique included a range of samples and procedure variables necessary to validate the effectiveness of the column. An excellent resolution and reproducibility was obtained among the sucrose, glucose, fructose and ethanol signals. The precision was within the accepted limits of less than 2% relative standard deviation.

Rapid determination of fosetyl-aluminium in commercial pesticide formulations by high-performance liquid chromatography

2014 ◽  
Vol 68 (6) ◽  
Author(s):  
Helen Karasali ◽  
Konstantinos Kasiotis ◽  
Kyriaki Machera
Keyword(s):  
Standard Deviation ◽  
Relative Standard Deviation ◽  
High Performance ◽  
Limit Of Detection ◽  
Rapid Determination ◽  
Hplc Method ◽  
Negative Ion ◽  
Rp Hplc ◽  
Relative Standard

AbstractAn isocratic reversed-phase high-performance liquid chromatographic (RP-HPLC) method with diode array detection (DAD) was developed for the determination of aluminium tris(ethyl phosphonate) (fosetyl-aluminium, fosetyl-Al) in plant-protection products. The method involves extraction of the active ingredient by sonication of the sample with water and direct measurement by RPHPLC. The isocratic RP-HPLC method for the analysis of fosetyl-Al thus developed was then validated for specificity, linearity, precision, and accuracy. The chromatographic peak confirmation was performed by LC-MS using electron spray ionisation in the negative-ion mode. The repeatability of the method, expressed as relative standard deviation (RSD, %), was found to be 0.5 % and the limit of detection was 0.035 mg mL−1. The average recoveries of the three fortification levels varied from 96.7 % to 100.6 % and the RSDs ranged between 2.6 % and 6.3 %. The precision of the method was also considered to be acceptable as the experimental repeatability relative standard deviation (RSDr) was lower than the RSDr, calculated using the Horwitz equation. The method is rapid, simple, accurate, cost-effective, and provides a new and reliable means for the analysis of fosetyl-Al in formulated products.

scholarly journals ULTRAVIOLET SPECTROPHOTOMETRIC METHOD DEVELOPMENT FOR ESTIMATION OF NEW ANTIVIRAL REPURPOSING DRUG FAVIPIRAVIR

2021 ◽  
pp. 67-69
Author(s):  
JEEVANA JYOTHI B ◽  
VENKATA KAVYA R
Keyword(s):  
Standard Deviation ◽  
Relative Standard Deviation ◽  
Spectrophotometric Method ◽  
Method Development ◽  
Quantitation Limit ◽  
Ich Guidelines ◽  
Relative Standard ◽  
Recovery Study ◽  
Development And Validation ◽  
Interday Precision

Objective: A new, economical, precise, linear, sensitive, accurate, ultraviolet (UV) spectrophotometric method for the estimation of new antiviral repurposing drug favipiravir as there is no reported simple UV spectrophotometric method for estimation. The efforts were made for development and validation of favipiravir as per ICH guidelines, because drug has a wide scope for formulations to be developed for treating different viruses. Methods: This method was developed using ethanol and water as a solvent. Favipiravir showed the absorption maxima at 234 nm. A Shimadzu UV–visible spectrophotometer (UV JAPAN 1801) was used to carry out spectral analysis. Results: The developed method was linear for a range of 0–10 μg/ml and displayed a good correlation coefficient of 0.9995. Accuracy of the method was estimated using a recovery study. The amount of drug recovered was found to be in the range of 99.30–99.91%. The % relative standard deviation value of intraday precision was found to be 0.408% and interday precision was found to be in the range of 0.348–0.693%. The % relative standard deviation found to be <2 which are indicative of the precision and reproducibility of the method. Detection limit and quantitation limit were noticed as 0.095 and 0.290, respectively. Conclusion: The developed UV spectrophotometric method was validated statistically for linearity, accuracy, precision, and sensitivity and results proved that the method can be employed for routine analysis of favipiravir.

Chromatographic Quantification of Ivermectin and Pranziquantel in the Tablets Using Stability Indicating RP-HPLC Method

2019 ◽  
Vol 25 (3) ◽  
pp. 254-261
Author(s):  
Naga Venkata Suresh Kumar Devaka ◽  
Vallabhaneni Madhusudhan Rao
Keyword(s):  
Standard Deviation ◽  
Relative Standard Deviation ◽  
Limit Of Detection ◽  
Hplc Method ◽  
Assay Method ◽  
Array Detector ◽  
Limit Of Quantification ◽  
Stability Indicating ◽  
Rp Hplc ◽  
Relative Standard

Background: A new stability indicating RP-HPLC based assay method was developed to quantify ivermectin and praziquantel simultaneously and applied effectively to tablets. Methods: The simultaneous assay of ivermectin and praziquantel by RP-HPLC was done using an YMC C18 (250 mm × 4.6 mm, 5 µm) column with a mobile phase mixture of 0.1M disodium hydrogen phosphate (pH 4.5) and acetonitrile (55:45, v/v) using a isocratic flow rate of 1.0 ml/min and measured at 242 nm using photodiode array detector. All parameters were validated following the ICH guiding principles. The method was applied to quantify ivermectin and praziquantel simultaneously in tablets. Results: The retention values of ivermectin and praziquantel were 3.465 min and 4.468 min, respectively. The method’s linearity was found to be 1-3 µg/ml (ivermectin) and 25-75 µg/ml (praziquantel). The limit of detection was 0.010 µg/ml (ivermectin) and 0.046 µg/ml (praziquantel); limit of quantification was 0.033 µg/ml (ivermectin) and 0.155 µg/ml (praziquantel). The percent relative standard deviation of ivermectin and praziquantel was ˂1.0%. The percent assay was 99.51% and 99.20% for ivermectin and praziquantel, respectively. In tablets, the percent recovery of ivermectin and praziquantel was 99.60% and 99.38% with a percent relative standard deviation value of 0.353% and 0.106%, respectively. Stability indicating capability of the method was demonstrated through the stress degradation studies. Conclusion: The developed method was proved to be selective, precise and accurate for the quality control of ivermectin and praziquantel in tablets.

scholarly journals QUANTITATION OF METFORMIN IN URINE BY RP-HPLC METHOD AND ITS APPLICATION IN PHARMACOKINETICS

2021 ◽  
pp. 67-71
Author(s):  
MARY REBECCA Y. ◽  
SUDHA V. ◽  
VIJAYAKUMAR A. ◽  
HEMANTH KUMAR A. K.
Keyword(s):  
Particle Size ◽  
Standard Deviation ◽  
Sample Preparation ◽  
Relative Standard Deviation ◽  
Urine Sample ◽  
Hplc Method ◽  
Uv Detection ◽  
Pharmacokinetic Studies ◽  
Rp Hplc ◽  
Relative Standard

Objective: To develop and validate an easy and sensitive HPLC method for quantitation of metformin in urine. Methods: The technique involved deproteinisation of urine sample with methanol and analysis of the supernatant the usage of Zorbax 300–SCX, 4.6 X 150 mm ID, 5 µm particle size and UV detection at a wavelength of 233 nm. Results: The assay was specific for metformin and linear from 1.25 to 50.0μg/ml. The relative standard deviation of intra-and inter-day assays was lesser than 7%. The recovery of metformin from urine ranged from 97-103%. Conclusion: An easy and sensitive HPLC approach for quantitation of metformin in urine had been developed. Due to its simplicity in sample preparation and instrumentation, this technique can be used for pharmacokinetic studies of metformin in urine samples.

scholarly journals Quality control and evaluation of Inonotus obliquus using HPLC method with novel marker compounds

2020 ◽  
Vol 11 (1) ◽  
Author(s):  
Jin Hyeok Kim ◽  
Seol Kyu Park ◽  
Chong Woon Cho ◽  
Ba Vinh Le ◽  
Young Ho Kim ◽  
...  
Keyword(s):  
Quality Control ◽  
Standard Deviation ◽  
Relative Standard Deviation ◽  
Hplc Method ◽  
Linear Regression Method ◽  
Inonotus Obliquus ◽  
Quantitative Monitoring ◽  
Relative Standard ◽  
Marker Compounds ◽  
Deviation Method

AbstractCurrent quality control of Inonotus obliquus requires chromogen complex content limit of 10% in accordance with the State Pharmacopoeia of the Union of Soviet Socialist Republics. However, this causes ambiguous results, impeding precise quality control. To improve ambiguous quality control criteria, this study developed a new HPLC method using two novel marker compounds (inotodiol and 3β-hydroxylanosta-8,24-dien-21-al) to control the quality control of I. obliquus. The HPLC analysis was carried out in a C18 column with an isocratic elution of 95% acetonitrile at 210 nm. The developed method validated in terms of linearity, precision, accuracy, and recovery. The content criteria were established by the linear regression method and relative standard deviation method. As the results of the quantitative monitoring, 1.165 mg/g of inotodiol and 1.717 mg/g of 3β-hydroxylanosta-8,24-dien-21-al, calculated by the relative standard deviation method, were suggested new quality criteria. A new HPLC method was developed to improve current quality control of I. obliquus and new lower content criteria were proposed as a result of quantitative monitoring. Graphical abstract

An Automated Procedure for the Determination of Ammonia in Tobacco

1972 ◽  
Vol 6 (4) ◽  
Author(s):  
P.F. Collins ◽  
W.W. Lawrence ◽  
J.F. Williams
Keyword(s):  
Standard Deviation ◽  
Relative Standard Deviation ◽  
Distillation Method ◽  
Relative Standard ◽  
Tobacco Sample ◽  
Automated Determination

AbstractA procedure for the automated determination of ammonia in tobacco has been developed. Ammonia is extracted from the ground tobacco sample with water and is determined with a Technicon Auto Analyser system which employs separation of the ammonia through volatilization followed by colourimetry using the phenate-hypochlorite reaction. The procedure has been applied to a variety of tobaccos containing from 0.02 to 0.5 % ammonia with an overall relative standard deviation of 2 %. The accuracy of the procedure as judged by recovery tests and by comparison to a manual distillation method is considered adequate

How Certain Are the Reported Ionic Conductivities of Thiophosphate-Based Solid Electrolytes? an Interlaboratory Study

2020 ◽  
Author(s):  
Saneyuki Ohno ◽  
Tim Bernges ◽  
Johannes Buchheim ◽  
Marc Duchardt ◽  
Anna-Katharina Hatz ◽  
...  
Keyword(s):  
Standard Deviation ◽  
Ionic Conductivity ◽  
Relative Standard Deviation ◽  
Solid Electrolytes ◽  
Ionic Conductivities ◽  
Ionic Conductors ◽  
Energy Storage Devices ◽  
Activation Barriers ◽  
Storage Devices ◽  
Relative Standard

<p>Owing to highly conductive solid ionic conductors, all-solid-state batteries attract significant attention as promising next-generation energy storage devices. A lot of research is invested in the search and optimization of solid electrolytes with higher ionic conductivity. However, a systematic study of an <i>interlaboratory reproducibility</i> of measured ionic conductivities and activation energies is missing, making the comparison of absolute values in literature challenging. In this study, we perform an uncertainty evaluation via a Round Robin approach using different Li-argyrodites exhibiting orders of magnitude different ionic conductivities as reference materials. Identical samples are distributed to different research laboratories and the conductivities and activation barriers are measured by impedance spectroscopy. The results show large ranges of up to 4.5 mScm<sup>-1</sup> in the measured total ionic conductivity (1.3 – 5.8 mScm<sup>-1</sup> for the highest conducting sample, relative standard deviation 35 – 50% across all samples) and up to 128 meV for the activation barriers (198 – 326 meV, relative standard deviation 5 – 15%, across all samples), presenting the necessity of a more rigorous methodology including further collaborations within the community and multiplicate measurements.</p>

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