scholarly journals Development and Validation of an Analytical Method for Deacetylasperulosidic Acid, Asperulosidic Acid, Scopolin, Asperuloside and Scopoletin in Fermented Morinda citrifolia L. (Noni)

Separations ◽  
2021 ◽  
Vol 8 (6) ◽  
pp. 80
Author(s):  
Sun-Il Choi ◽  
Hee-Yeon Kwon ◽  
Im-Joung La ◽  
Yeon-Hui Jo ◽  
Xionggao Han ◽  
...  
Keyword(s):  
Bioactive Compounds ◽  
High Performance ◽  
Limit Of Detection ◽  
Hplc Method ◽  
Biologically Active ◽  
Morinda Citrifolia ◽  
Coefficient Of Determination ◽  
Analysis Method ◽  
Food Ingredients

Fermentation is a technology that enhances biologically active ingredients, improves the absorption rate and induces the generation of new functional ingredients by the catalytic action of enzyme systems possessed by microorganisms. In this study, changes in the content of five kinds of bioactive compounds (deacetylasperulosidic acid, asperulosidic acid, scopolin, asperuloside and scopoletin) of Morinda citrifolia L. were confirmed by fermentation, and a high-performance liquid chromatography-photodiode array (HPLC-PDA) analysis method for measuring analytes was developed and validated. HPLC method for the determination of five bioactive compounds in Morinda citrifolia L. extracts (MCE) was validated in terms of sensitivity, linearity, selectivity, limit of detection (LOD) and quantification (LOQ), precision and accuracy. The coefficient of determination of the calibration curve for bioactive compounds (1.56–100 μg/mL) showed linearity (R2 ≥ 0.9999). LOD and LOQ were in the range 0.04–0.97 and 0.13–2.95 μg/mL, respectively. The range of intra- and intraday accuracies values (recovery) were 97.5–121.9% and 98.8–118.1%, respectively, and precision value (RSDs) of the bioactive compounds were <4%. In addition, changes in the content of five bioactive compounds in MCE by fermentation were confirmed. These results indicate that the developed fermentation and analysis method could be applied in the development of potential functional food ingredients.

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 HPLC method validation and application for organic acid analysis in wine after solid-phase extraction

2016 ◽  
Vol 35 (2) ◽  
pp. 225 ◽  
Author(s):  
Violeta Ivanova-Petropulos ◽  
Krste Tašev ◽  
Marina Stefova
Keyword(s):  
Solid Phase Extraction ◽  
Organic Acids ◽  
High Performance ◽  
Limit Of Detection ◽  
Solid Phase ◽  
Hplc Method ◽  
Phase Extraction ◽  
Hplc Separation ◽  
Limit Of Quantification

<p>A solid-phase extraction method followed by reverse phase high-performance liquid chromatography (RP-HPLC) was optimized and validated for the quantitative determination of tartaric, malic, shikimic, lactic, citric and succinic acids in wine. Solid-phase extraction was carried out with C18 cartridges and extraction recoveries for all acids ranging from 98.3 to 103% were obtained. HPLC separation was performed with isocratic elution on a LiChrosorb RP-18 column (250 × 4.6 mm I.D., 5 µm) protected with the appropriate guard column. The mobile phase was a 5 mM solution of H<sub>3</sub>PO<sub>4</sub> with pH 2.1 at a flow rate of 1 ml/min. Detection of the organic acids was performed at 210 nm. The developed method was validated by checking its linearity, limit of detection (LOD), limit of quantification (LOQ), precision and recovery. The method was applied to the analysis of organic acids in Macedonian red and white wines.</p>

scholarly journals STABILITY INDICATING RP-HPLC METHOD DEVELOPMENT AND VALIDATION FOR THE SIMULTANEOUS DETERMINATION OF VILDAGLIPTIN AND METFORMIN IN PHARMACEUTICAL DOSAGE FORM

2017 ◽  
Vol 9 (3) ◽  
pp. 150
Author(s):  
Ramesh Jayaprakash ◽  
Senthil Kumar Natesan
Keyword(s):  
High Performance ◽  
Method Development ◽  
Limit Of Detection ◽  
Potassium Dihydrogen Phosphate ◽  
Hplc Method ◽  
Dihydrogen Phosphate ◽  
Pharmaceutical Dosage Form ◽  
Stability Indicating ◽  
Rp Hplc

Objective: The present study was aimed to develop a rapid, accurate, linear, sensitive and validate stability-indicating high performance liquid chromatographic [RP-HPLC] method for determination of vildagliptin and metformin in pharmaceutical dosage form.Methods: The chromatographic separation was performed on kromasil-C18 column [4.5 x 250 mm; 5 µm] using a mobile phase consisting of 0.05 mmol potassium dihydrogen phosphate buffer: acetonitrile [80:20 v/v], [pH adjusted to 3.5 using orthophosphoric acid]. The flow rate is 0.9 ml/min and the detection was carried out at 263 nm.Results: The chromatographic condition, the peak retention time of metformin and vildagliptin were found to be 2.215 min and 2.600 min respectively. Stress testing was performed in accordance with an international conference on harmonization [ICH] Q1A R2 guidelines. The method was validated as per ICH Q2 R1 guidelines. The calibration curve was found to be linear in the concentration range of 5-17.5 µg/ml and 50-175 µg/ml for vildagliptin and metformin. The limit of detection and quantification was found to be 0.0182 µg/ml and 0.0553 µg/ml for vildagliptin and 0.4451 µg/ml and 1.3490 µg/ml for metformin respectively.Conclusion: A new sensitive, simple and stability indicating reverse-phase high-performance liquid chromatography [RP-HPLC] method has been developed and validated for the determination of vildagliptin and metformin. The proposed method can be used for routine determination of vildagliptin and metformin.

RAPID HIGH PERFORMANCE LIQUID CHROMATOGRAPHY METHOD FOR THE DETERMINATION OF RALTEGRAVIR IN HUMAN SALIVA

INDIAN DRUGS ◽  
2019 ◽  
Vol 56 (09) ◽  
pp. 68-73
Author(s):  
K Vijaya Sri ◽  
M. Shiva Kumar ◽  
M. A. Madhuri ◽  
Suresha K. ◽  
Keyword(s):  
High Performance ◽  
Limit Of Detection ◽  
High Performance Liquid Chromatographic ◽  
Human Saliva ◽  
Hplc Method ◽  
Limit Of Quantification ◽  
Chromatography Method ◽  
Liquid Chromatography Method ◽  
Liquid Chromatographic

In this study, a high-performance liquid chromatographic method (HPLC) was developed, validated and applied for the determination of raltegravir in biological sample like saliva. Liquid- liquid extraction was performed for isolation of the drug and elimination of saliva interferences. Samples of saliva was extracted with 50µL of ortho phosphoric acid and 3ml of methanol was added and spiked with raltegravir. The chromatographic separation was performed on Agilent Eclipse C18 (100 mm × 4.6 mm, 3.5µm) column, by using 80:20 v/v acetonitrile: water as a mobile phase under isocratic conditions at a flow rate of 1.0 mL/min for UV detection at 240 nm. Retention time of raltegravir was found to be 1.030 min. Linearity was found to be in the range of 25-1000 ng/mL with regression equation y = 13864x + 40495 and correlation coefficient 0.999. The low % RSD value indicates the method is accurate and precise. The limit of detection (LOD) and limit of quantification (LOQ) were found to be 0.76 and 2.28 ng/mL, respectively. It can be concluded that this validated HPLC method is easy, precise, accurate, sensitive and selective for determination of raltegravir in saliva.

scholarly journals Stability-Indicating Assay for the Determination of Pentobarbital Sodium in Liquid Formulations

2015 ◽  
Vol 2015 ◽  
pp. 1-6 ◽  
Author(s):  
Myriam Ajemni ◽  
Issa-Bella Balde ◽  
Sofiane Kabiche ◽  
Sandra Carret ◽  
Jean-Eudes Fontan ◽  
...  
Keyword(s):  
High Performance ◽  
Limit Of Detection ◽  
Drug Stability ◽  
Reversed Phase ◽  
Hplc Method ◽  
Limit Of Quantification ◽  
Reliable Determination ◽  
Pentobarbital Sodium ◽  
Stability Indicating

A stability-indicating assay by reversed-phase high performance liquid chromatography (RP-HPLC) method was developed for the determination of pentobarbital sodium in oral formulations: a drug used for infant sedation in computed tomography (CT) or magnetic resonance imaging (MRI) scan. The chromatographic separation was achieved on a reversed-phase C18 column, using isocratic elution and a detector set at 214 nm. The optimized mobile phase consisted of a 0.01 M potassium buffer pH 3 and methanol (40 : 60, v/v). The flow rate was 1.0 mL/min and the run time of analysis was 5 min. The linearity of the method was demonstrated in the range of 5 to 250 μg/mL pentobarbital sodium solution (r2= 0.999). The limit of detection and limit of quantification were 2.10 and 3.97 μg/mL, respectively. The intraday and interday precisions were less than 2.1%. Accuracy of the method ranged from 99.2 to 101.3%. Stability studies indicate that the drug is stable to sunlight and in aqueous solution. Accelerated pentobarbital sodium breakdown by strong alkaline, acidic, or oxidative stress produced noninterfering peaks. This method allows accurate and reliable determination of pentobarbital sodium for drug stability assay in pharmaceutical 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 Validation of an HPLC Method for Determination of Bisphenol-A Migration from Baby Feeding Bottles

2019 ◽  
Vol 2019 ◽  
pp. 1-6
Author(s):  
Ruth Rodriguez ◽  
Elianna Castillo ◽  
Diana Sinuco
Keyword(s):  
Bisphenol A ◽  
High Performance ◽  
Limit Of Detection ◽  
Hplc Method ◽  
Migration Test ◽  
Limit Of Quantification ◽  
Migration Assay ◽  
Filling Method ◽  
Migration Assays

A simple and economic high-performance liquid chromatography (HPLC-UV-Vis) analytical method was validated for the quantitation of specific Bisphenol-A migration from baby feeding bottles. Overall and specific migration assays were done with different food simulating matrices using the filling method. Good linearity was obtained over the concentration range of 0.01–0.6 mg/kg. The limit of detection (LOD) and limit of quantification (LOQ) were 0.004 and 0.010 mg/kg, respectively. The repeatability of the method (%RSD, n=10) was between 89.5 and 99.0%, while recovery ranged from 83.2 to 98.4%. The method was applied to specific migration assays from baby feeding bottles purchased from different plastic producers in Colombia. The results show that, in a first migration assay, Bisphenol-A was not detectable in all samples. In a second migration test, Bisphenol-A concentrations were higher than the most restricted limit (0.05 mg/kg) with ethanol 95% and isooctane as food simulants.

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 A Simple and Validated Reverse Phase HPLC Methodfor the Determination of Rabeprazole inPharmaceutical Dosage Forms

2010 ◽  
Vol 7 (2) ◽  
pp. 569-577 ◽  
Author(s):  
Uma Mahesh Karra ◽  
Sanjeeva Yarkala
Keyword(s):  
High Performance ◽  
Limit Of Detection ◽  
Hplc Method ◽  
Reverse Phase Hplc ◽  
Reverse Phase ◽  
Rp Hplc ◽  
Limit Of Quantitation ◽  
Tablet Formulations ◽  
Bulk Drug

A simple and rapid reverse phase high performance liquid chromatography (RP-HPLC) method was developed and validated for quantitative determination of rabeprazole in bulk drug samples and formulations. Rabeprazole was analyzed by using reverse phase LC-GC column (Inertsil ODS, 4.6 mm x 25 cm, 5 microns), with mobile phase consisting of methanol: water (78:22 v/v). The flow rate was set 1.0 mL/min and analysis was performed at wavelength 288 nm using Photo Diode Array (PDA) detector at ambient temperature. The method was validated and stability studies were conducted under different conditions. The retention time for rabeprazole was around 4.12 minutes. The calibration curves were linear (r≥0.9998) over a concentration range from 20.0 to 80.0 μg/mL. Limit of detection (LOD) and Limit of quantitation (LOQ) were 8 ng/mL and 24 ng/mL respectively. The developed method was successfully applied to estimate the amount of rabeprazole in tablet formulations.

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