Elaboration and Validation of HPLC/DAD Method for Quality Control of Products Containing Cannabidiol

2020 ◽  
Vol 16 ◽  
Author(s):  
Lily Andonova ◽  
Ervin Ivanov ◽  
Ivanka Pencheva ◽  
Spiro Konstantinov
Keyword(s):  
High Performance ◽  
Cannabis Sativa ◽  
Practical Importance ◽  
Biological Properties ◽  
Hplc Method ◽  
Food Supplements ◽  
Purification Method ◽  
Technical Requirements ◽  
Extraction And Purification ◽  
Hypnotic Agent

Background: Cannabidiol (CBD) is the main, physiologically active, but psycho-inactive constituent of the glandular hairs of Cannabis sativa. CBD exhibits diverse pharmacological activities and it is used as anticonvulsant, sedative and hypnotic agent. Other biological properties shown by CBD are antipsychotic, anti-inflammatory and neuroprotective. Objective: The aim of this study is to develop, validate and apply high performance liquid chromatography (HPLC/DAD) method with diode array detection for identification and assay of CBD in food supplements obtained by different types of extraction and purification. Method: HPLC method with isocratic elution using column C18 ODS, 250 x 4.6, 100 A, 5 μm, mobile phase - mixture of acetonitrile and water in ratio 80:20v/v, flow rate of 1.0 ml/min and DAD detection at 220 nm. Results: The method was developed and validated according to European Pharmacopoeia and International Council for Harmonisation of Technical Requirements for Pharmaceuticals for Human Use (ICH). For the purposes analytical parameters repeatability, linearity, accuracy, LOD, LOQ, specificity and system suitability test were studied. The developed method was successfully applied on a series of food supplements containing CBD. Conclusion: The developed method is of practical importance for determination of purity, identification and assay tests of food supplements containing CBD extract in accordance with EU regulation concerning food authorizations because it is useful for analytical tests for identification, purity determination and assay of products containing CBD extract and could serve as part of the testing process in the pharmaceutical industry.

Development and Validation of a Novel Reversed Phase High Performance Liquid Chromatography with Refractive Index Detector Method for Assay of Polyvinyl Alcohol in an Ophthalmic Solution

2020 ◽  
Vol 16 (7) ◽  
pp. 867-871
Author(s):  
Harun Ergen ◽  
Muge Guleli ◽  
Cigdem Sener ◽  
Cem Caliskan ◽  
Sercan Semiz ◽  
...  
Keyword(s):  
Refractive Index ◽  
Liquid Chromatography ◽  
Polyvinyl Alcohol ◽  
High Performance ◽  
Ophthalmic Solution ◽  
Reversed Phase ◽  
Hplc Method ◽  
Solution Stability ◽  
Technical Requirements ◽  
Refractive Index Detector

Introduction: Polyvinyl alcohol (PVA), a polymer, is in demand due to its usage in different applications such as pharmaceutical, biomedical and textile, paper, food industries. Methods: A new sensitive reversed phased high-pressure liquid chromatography (RP-HPLC) method with refractive index detector (RID) was developed for determination of PVA in an ophthalmic solution containing dexpanthenol and PVA as active substances and it was validated according to The International Council for Harmonisation of Technical Requirements for Pharmaceuticals for Human Use (ICH) guideline. Results: Chromatographic separation was achieved on a Chiral-AGP (150 mm × 4.0 mm, 5 μm) column kept at 30°C with an isocratic flow at a flow rate of 1.0 ml/min. The detector temperature was 30°C, the retention time of PVA was around 1.0 min and the total run time was 5 minutes. Conclusion: The proposed method showed linearity, accuracy, precision, specificity, robustness, solution stability, and system suitability results within the acceptance criteria.

scholarly journals Systematic and Model-Assisted Process Design for the Extraction and Purification of Artemisinin from Artemisia annua L.—Part III: Chromatographic Purification

Processes ◽  
2018 ◽  
Vol 6 (10) ◽  
pp. 180 ◽  
Author(s):  
Fabian Mestmäcker ◽  
Axel Schmidt ◽  
Maximilian Huter ◽  
Maximilian Sixt ◽  
Jochen Strube
Keyword(s):  
High Performance ◽  
Artemisia Annua ◽  
Batch Process ◽  
Pilot Scale ◽  
Hplc Method ◽  
Artemisia Annua L ◽  
Reproducibility Study ◽  
Extraction And Purification ◽  
Layer Chromatography ◽  
Characteristic Process

In this study, the purification of an extract from Artemisia annua L. using chromatographic methods is studied. In a first step, a screening of different phases and solvents using thin-layer chromatography (TLC) was performed. Then, a laboratory-scale high performance liquid chromatography (HPLC) method was developed and transferred to a pilot scale. A reproducibility study based on 120 injections was carried out. The batch process that was developed and the results from a designed continuous simulated moving bed (SMB) chromatography were compared based on characteristic process numbers and economy.

scholarly journals Development of a Direct Competitive ELISA Kit for Detecting Deoxynivalenol Contamination in Wheat

Molecules ◽  
2019 ◽  
Vol 25 (1) ◽  
pp. 50
Author(s):  
Li Han ◽  
Yue-Tao Li ◽  
Jin-Qing Jiang ◽  
Ren-Feng Li ◽  
Guo-Ying Fan ◽  
...  
Keyword(s):  
High Throughput Screening ◽  
High Performance ◽  
Limit Of Detection ◽  
High Specificity ◽  
Hplc Method ◽  
Rapid Screening ◽  
Enzyme Linked Immunosorbent Assay ◽  
Detection Range ◽  
Technical Requirements ◽  
Relative Standard

This study was conducted to develop a self-assembled direct competitive enzyme-linked immunosorbent assay (dcELISA) kit for the detection of deoxynivalenol (DON) in food and feed grains. Based on the preparation of anti-DON monoclonal antibodies, we established a standard curve with dcELISA and optimized the detection conditions. The performance of the kit was evaluated by comparison with high-performance liquid chromatography (HPLC). The minimum detection limit of DON with the kit was 0.62 ng/mL, the linear range was from 1.0 to 113.24 ng/mL and the half-maximal inhibition concentration (IC50) was 6.61 ng/mL in the working buffer; there was a limit of detection (LOD) of 62 ng/g, and the detection range was from 100 to 11324 ng/g in authentic agricultural samples. We examined four samples of wheat bran, wheat flour, corn flour and corn for DON recovery. The average recovery was in the range of 77.1% to 107.0%, and the relative standard deviation (RSD) ranged from 4.2% to 11.9%. In addition, the kit has the advantages of high specificity, good stability, a long effective life and negligible sample matrix interference. Finally, wheat samples from farms in the six provinces of Henan, Anhui, Hebei, Shandong, Jiangsu and Gansu in China were analyzed by the kit. A total of 30 samples were randomly checked (five samples in each province), and the results were in good agreement with the standardized HPLC method. These tests showed that the dcELISA kit had good performance and met relevant technical requirements, and it had the characteristics of accuracy, reliability, convenience and high-throughput screening for DON detection. Therefore, the developed kit is suitable for rapid screening of DON in marketed products.

scholarly journals A New, Rapid and Efficient HPLC Method to Assay Resveratrol in Food Supplements

2019 ◽  
Vol 70 (9) ◽  
pp. 3202-3205 ◽  
Author(s):  
Veronica Isabela Craciun ◽  
Felicia Gabriela Gligor ◽  
Anca Maria Juncan ◽  
Adriana Aurelia Chis ◽  
Luca Liviu Rus
Keyword(s):  
High Performance Liquid Chromatography ◽  
Liquid Chromatography ◽  
High Performance ◽  
Dosage Form ◽  
Hplc Method ◽  
Food Supplements

The aim of this study consisted in the development of a rapid and reliable high performance liquid chromatography (HPLC) method for resveratrol identification and assay in food supplements, trying to offer a robust, direct and convenient solution. By this method, several supplements with varying resveratrol content, between 103 and 119% of the stated amount per dosage form, were analyzed.

scholarly journals Bioaccessibility and Cellular Uptake of Carotenoids Extracted from Bactris gasipaes Fruit: Differences between Conventional and Ionic Liquid-Mediated Extraction

Molecules ◽  
2021 ◽  
Vol 26 (13) ◽  
pp. 3989
Author(s):  
Leonardo M. de Souza Mesquita ◽  
Daniella Carisa Murador ◽  
Bruna Vitória Neves ◽  
Anna Rafaela Cavalcante Braga ◽  
Luciana Pellegrini Pisani ◽  
...  
Keyword(s):  
Cellular Uptake ◽  
High Performance ◽  
In Vitro Digestion ◽  
Bactris Gasipaes ◽  
Purification Method ◽  
Extraction Solvent ◽  
Extraction And Purification ◽  
Feasible Alternative ◽  
Synthetic Colorants

Currently, on an industrial scale, synthetic colorants are used in many fields, as well as those extracted with conventional organic solvents (COSs), leading to several environmental issues. Therefore, we developed a sustainable extraction and purification method mediated by ionic liquids (IL), which is considered an alternative high-performance replacement for COSs. Carotenoids are natural pigments with low bioaccessibility (BCT) and bioavailability (BV) but with huge importance to health. To investigate if the BCT and cellular uptake of the carotenoids are modified by the extraction method, we conducted a comparison assay between both extraction procedures (IL vs. COS). For this, we used the Amazonian fruit Bactris gasipaes, a rich source of pro-vitamin A carotenoids, to obtain the extract, which was emulsified and subjected to an in vitro digestion model followed by the Caco-2 cell absorption assay. The bioaccessibility of carotenoids using IL was better than those using COS (33.25%, and 26.84%, respectively). The cellular uptake of the carotenoids extracted with IL was 1.4-fold higher than those extracted using COS. Thus, IL may be a feasible alternative as extraction solvent in the food industry, replacing COS, since, in this study, no IL was present in the final extract.

Evaluation of Gloriosa superba for Yield Attributing Characters and Quantification of Colchicine Originated from Different Agro Climatic Zones of Tamil Nadu and Andhra Pradesh

2017 ◽  
Vol 9 (3) ◽  
Author(s):  
Arun Kumar P. ◽  
Elangaimannan R.
Keyword(s):  
Seed Yield ◽  
Tamil Nadu ◽  
High Performance ◽  
Andhra Pradesh ◽  
Crop Improvement ◽  
Mean Value ◽  
Hplc Method ◽  
Gloriosa Superba ◽  
Climatic Zones ◽  
Colchicine Alkaloid

The study was conducted to evolve Gloriosa superba for yield characters and alkalodi content for selecting elite genotypes for comercial exploitatio n. The genotypes were sowm in Variyankaval village, Udayarpalayam taluk of Ariyalur district, Tamil Nadu. The highest mean value for fresh and dry seed yield was observed in Chittor local. The genotype Mulanur local has recorded the highest mean value for number of pods per plant and number of seeds per pod and Arupukotai local excelled the general mean for the traits seeds per pod, fresh and dry seed yield and also for tuber characters. An investigation was carried out to quantify the colchicine (alkaloid) present in tubers by High Performance Liquid Chromatography (HPLC) method. The genotypes collected from Arupukotai recorded the highest colchicine content (0.760 mg/g) followed by Chittoor (0.578 mg/g) and Mulanur (0.496 mg/g) and there by these three genotypes were utilized for further crop improvement.

Developing a High-performance Liquid Chromatography Method for Simultaneous Determination of Loratadine and its Metabolite Desloratadine in Human Plasma

2020 ◽  
Vol 20 (13) ◽  
pp. 1053-1059
Author(s):  
Mahmoud M. Sebaiy ◽  
Noha I. Ziedan
Keyword(s):  
High Performance Liquid Chromatography ◽  
Liquid Chromatography ◽  
Human Plasma ◽  
High Performance ◽  
Allergic Diseases ◽  
Reversed Phase ◽  
Hplc Method ◽  
H1 Receptor ◽  
Chromatography Method

Background: Allergic diseases are considered as the major burden on public health with increased prevalence globally. Histamine H1-receptor antagonists are the foremost commonly used drugs in the treatment of allergic disorders. The target drug in this study, loratadine, belongs to this class of drugs and its biometabolite desloratadine which is also a non-sedating H1 receptor antagonist with anti-histaminic activity being 2.5 to 4 times greater than loratadine. This study aimed to develop and validate a novel isocratic Reversed-phase High-Performance Liquid Chromatography (RP-HPLC) method for rapid and simultaneous separation and determination of loratadine and its metabolite, desloratadine in human plasma. Methods: The drug extraction method from plasma was based on protein precipitation technique. The separation was carried out on a Thermo Scientific BDS Hypersil C18 column (5μm, 250 x 4.60 mm) in a mobile phase of MeOH: 0.025M KH2PO4 adjusted to pH 3.50 using orthophosphoric acid (85: 15, v/v) at an ambient temperature. The flow rate was maintained at 1 mL/min and maximum absorption was measured using the PDA detector at 248 nm. Results: The retention times of loratadine and desloratadine in plasma samples were recorded to be 4.10 and 5.08 minutes, respectively, indicating a short analysis time. Limits of detection were found to be 1.80 and 1.97 ng/mL for loratadine and desloratadine, respectively, showing a high degree of sensitivity of the method. The method was then validated according to FDA guidelines for the determination of the two analytes in human plasma. Conclusion: The results obtained indicate that the proposed method is rapid, sensitive in the nanogram range, accurate, selective, robust and reproducible compared to other reported methods.

Determination of Selected Phthalates in Some Commercial Cosmetic Products by HPLC-UV

2020 ◽  
Vol 23 (10) ◽  
pp. 1010-1022
Author(s):  
Emrah Dural
Keyword(s):  
High Performance ◽  
Phthalate Esters ◽  
High Sensitivity ◽  
Hplc Method ◽  
Cosmetic Products ◽  
Limit Of Quantification ◽  
Nail Polish ◽  
Accuracy And Precision ◽  
Butyl Phthalate

Aim and scope: Due to the serious toxicological risks and their widespread use, quantitative determination of phthalates in cosmetic products have importance for public health. The aim of this study was to develop a validated simple, rapid and reliable high-performance liquid chromatography (HPLC) method for the determination of phthalates which are; dimethyl phthalate (DMP), diethyl phthalate (DEP), benzyl butyl phthalate (BBP), di-n-butyl phthalate (DBP), di(2- ethylhexyl) phthalate (DEHP), in cosmetic products and to investigate these phthalate (PHT) levels in 48 cosmetic products marketing in Sivas, Turkey. Materials and Methods: Separation was achieved by a reverse-phase ACE-5 C18 column (4.6 x 250 mm, 5.0 μm). As the mobile phase, 5 mM KH2PO4 and acetonitrile were used gradiently at 1.5 ml min-1. All PHT esters were detected at 230 nm and the run time was taking 21 minutes. Results: This method showed the high sensitivity value the limit of quantification (LOQ) values for which are below 0.64 μg mL-1 of all phthalates. Method linearity was ≥0.999 (r2). Accuracy and precision values of all phthalates were calculated between (-6.5) and 6.6 (RE%) and ≤6.2 (RSD%), respectively. Average recovery was between 94.8% and 99.6%. Forty-eight samples used for both babies and adults were successfully analyzed by the developed method. Results have shown that, DMP (340.7 μg mL-1 ±323.7), DEP (1852.1 μg mL-1 ± 2192.0), and DBP (691.3 μg mL-1 ± 1378.5) were used highly in nail polish, fragrance and cream products, respectively. Conclusion: Phthalate esters, which are mostly detected in the content of fragrance, cream and nail polish products and our research in general, are DEP (1852.1 μg mL-1 ± 2192.0), DBP (691.3 μg mL-1 ± 1378.5) and DMP (340.7 μg mL-1 ±323.7), respectively. Phthalates were found in the content of all 48 cosmetic products examined, and the most detected phthalates in general average were DEP (581.7 μg mL-1 + 1405.2) with a rate of 79.2%. The unexpectedly high phthalate content in the examined cosmetic products revealed a great risk of these products on human health. The developed method is a simple, sensitive, reliable and economical alternative for the determination of phthalates in the content of cosmetic products, it can be used to identify phthalate esters in different products after some modifications.

scholarly journals Rapid Detection and Quantification of Patulin and Citrinin Contamination in Fruits

Molecules ◽  
2021 ◽  
Vol 26 (15) ◽  
pp. 4545
Author(s):  
Sudharsan Sadhasivam ◽  
Omer Barda ◽  
Varda Zakin ◽  
Ram Reifen ◽  
Edward Sionov
Keyword(s):  
High Performance ◽  
Cost Effective ◽  
Hplc Method ◽  
Pear Fruit ◽  
Cost Effective Method ◽  
Fruit Samples ◽  
Pome Fruits ◽  
Reliable Methods ◽  
By Products ◽  
Detection And Quantification

Patulin (PAT) and citrinin (CTN) are the most common mycotoxins produced by Penicillium and Aspergillus species and are often associated with fruits and fruit by-products. Hence, simple and reliable methods for monitoring these toxins in foodstuffs are required for regular quality assessment. In this study, we aimed to establish a cost-effective method for detection and quantification of PAT and CTN in pome fruits, such as apples and pears, using high-performance liquid chromatography (HPLC) coupled with spectroscopic detectors without the need for any clean-up steps. The method showed good performance in the analysis of these mycotoxins in apple and pear fruit samples with recovery ranges of 55–97% for PAT and 84–101% for CTN, respectively. The limits of detection (LOD) of PAT and CTN in fruits were 0.006 µg/g and 0.001 µg/g, while their limits of quantification (LOQ) were 0.018 µg/g and 0.003 µg/g, respectively. The present findings indicate that the newly developed HPLC method provides rapid and accurate detection of PAT and CTN in fruits.

scholarly journals Development and validation of RP-HPLC method for estimation of brexpiprazole in its bulk and tablet dosage form using Quality by Design approach

2021 ◽  
Vol 7 (1) ◽  
Author(s):  
Amol S. Jagdale ◽  
Nilesh S. Pendbhaje ◽  
Rupali V. Nirmal ◽  
Poonam M. Bachhav ◽  
Dayandeo B. Sumbre
Keyword(s):  
Flow Rate ◽  
High Performance ◽  
Reversed Phase ◽  
Hplc Method ◽  
Control Analysis ◽  
Uv Detector ◽  
Mobile Phase Flow Rate ◽  
Rp Hplc ◽  
Quality By Design Approach ◽  
Bulk Drug

Abstract Background A new, sensitive, suitable, clear, accurate, and robust reversed-phase high-performance liquid chromatography (RP-HPLC) method for the determination of brexpiprazole in bulk drug and tablet formulation was developed and validated in this research. Surface methodology was used to optimize the data, with a three-level Box-Behnken design. Methanol concentration in the mobile phase, flow rate, and pH were chosen as the three variables. The separation was performed using an HPLC method with a UV detector and Openlab EZchrom program, as well as a Water spherisorb C18 column (100 mm × 4.6; 5m). Acetonitrile was pumped at a flow rate of 1.0 mL/min with a 10 mM phosphate buffer balanced to a pH of 2.50.05 by diluted OPA (65:35% v/v) and detected at 216 nm. Result The developed RP-HPLC method yielded a suitable retention time for brexpiprazole of 4.22 min, which was optimized using the Design Expert-12 software. The linearity of the established method was verified with a correlation coefficient (r2) of 0.999 over the concentration range of 5.05–75.75 g/mL. For API and formulation, the percent assay was 99.46% and 100.91%, respectively. The percentage RSD for the method’s precision was found to be less than 2.0%. The percentage recoveries were discovered to be between 99.38 and 101.07%. 0.64 μg/mL and 1.95 μg/mL were found to be the LOD and LOQ, respectively. Conclusion The developed and validated RP-HPLC system takes less time and can be used in the industry for routine quality control/analysis of bulk drug and marketed brexpiprazole products. Graphical abstract

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