scholarly journals Very Fast RP–UHPLC–PDA Method for Identification and Quantification of the Cannabinoids from Hemp Oil

2021 ◽  
Vol 11 (20) ◽  
pp. 9414
Author(s):  
Nicoleta Mirela Blebea ◽  
Dan Rambu ◽  
Teodor Costache ◽  
Simona Negreș
Keyword(s):  
High Performance ◽  
Reference Standard ◽  
Reverse Phase ◽  
European Area ◽  
Therapeutic Benefits ◽  
Mobile Phases ◽  
Cannabidiolic Acid ◽  
Wide Range ◽  
Health Products ◽  
Hemp Oil

In recent years, hemp oils have become ubiquitous in health products on the European market. As the trend continues to grow and more cannabinoids are researched for their therapeutic benefits, more academic and industrial interests are drawn to this direction. Cannabidiol, Δ9-tetrahydrocannabinol, and their acidic forms remain the most examined cannabinoids in hemp and cannabis oils, in the case of cannabidiol due to its proven health implications in numerous articles, and in the case of Δ9-tetrahydrocannabinol, due to the legislation in the European area. These oils sold on the internet contain a wide range of cannabinoids that could demonstrate their effects and benefits. As a result of these claims, we developed a robust and rapid method that can identify and quantify 10 of the most common cannabinoids found in hemp oils: cannabivarin, cannabidiolic acid, cannabigerolic acid, cannabigerol, cannabidiol, cannabinol, Δ9-tetrahydrocannabinol, Δ8-tetrahydrocannabinol, cannabichromene, and tetrahydrocannabinolic acid in less than 11 min, with reverse-phase–high-performance liquid chromatography–photodiode matrix system (RP–UHPLC–PDA) equipped with C18 column, eluting in a gradient using water and acetonitrile with formic acid as mobile phases. The quantification of 9 sample products presented in different matrixes was performed using a calibration curve obtained by analyzing standard solutions from a 10-cannabinoid-mix-certified reference standard. The developed method demonstrated the ability to identify and quantify the main cannabinoids in hemp oil and is a useful tool for pharmaceutical professionals.

scholarly journals Development and Validation of Simple, Rapid and Sensitive High- Performance Liquid Chromatographic Method for the Determination of Butenafine Hydrochloride

2020 ◽  
pp. 116-125
Author(s):  
Mohammad Javed Ansari ◽  
Mohammed Muqtader Ahmed ◽  
Md. Khalid Anwer ◽  
Mohammed F. Aldawsari ◽  
Saad M. Al Shahrani ◽  
...  
Keyword(s):  
Mobile Phase ◽  
High Performance ◽  
Linear Regression Analysis ◽  
Pharmaceutical Formulations ◽  
Hplc Method ◽  
Least Square ◽  
Reverse Phase ◽  
Rp Hplc ◽  
Relative Standard ◽  
Wide Range

Aims: The current paper reports a simple, rapid, sensitive, accurate, and precise Reverse-phase high performance liquid chromatography (RP-HPLC) method with wide range of estimation to determine butenafine hydrochloride in nanosponges. This method has been validated as per ICH norms. Study Design:  Experimental design with influence of variables such as mobile phase composition, flow rate, temperature and wavelength on the chromatographic peaks. Place and Duration of Study: Department of Pharmaceutics, College of Pharmacy, Prince Sattam Bin Abdulaziz University, Al-Kharj, Saudi Arabia between Jan 2020 and March 2020. Methodology: Separation was achieved by utilizing the most commonly used reverse phase column (C-18, 5 μm, 150 mm x 4.6 mm) set at 30ºC and quantified by UV detection at 280 nm after isocratic elution from a mobile phase (70:30 v/v of methanol: phosphate buffer pH 3.0) flowing at 1 ml/min. Results: A sharp and symmetrical peak was observed at 4.08 ± 0.01 minutes. The low variation in peak area and retention time (1.12% and 0.29%, respectively) and a high number of theoretical plates (>2000) indicated this method’s efficiency and suitability. The least square linear regression analysis (Y = 9265.5 X + 1961.4) showed excellent correlation (r2 = 0.999 ± 0.0003) between concentration and peak area of butenafine hydrochloride through a wide concentration range of 1–50 µg/ml. The limits of detection and quantification (LOD and LOQ) were 0.18 µg/ml and 0.57 µg/ml, respectively. The assay or determinations were accurate, precise and reproducible with mean accuracy and mean relative standard deviation of precision of 101.53 ± 0.43% and 0.51 ± 0.11% respectively. Conclusion: The developed RP-HPLC method was simple, sensitive, reproducible with wide range of estimation of butenafine hydrochloride in the nanosponges. The proposed method could be used for the analysis of butenafine hydrochloride in the conventional pharmaceutical formulations such as tablets, syrup, creams including novel formulations such as nanoparticles, nanosponges, nanoemulsions. The proposed method overcomes the specificity, sensitivity and reproducibility related issues of ultraviolet-visible spectroscopy.

scholarly journals Efficient Separation of Phytochemicals from Muehlenbeckia volcanica (Benth.) Endl. by Polarity-Stepwise Elution Counter-Current Chromatography and Their Antioxidant, Antiglycation, and Aldose Reductase Inhibition Potentials

Molecules ◽  
2021 ◽  
Vol 26 (1) ◽  
pp. 224
Author(s):  
Guang-Lei Zuo ◽  
Hyun Yong Kim ◽  
Yanymee N. Guillen Quispe ◽  
Zhi-Qiang Wang ◽  
Seung Hwan Hwang ◽  
...  
Keyword(s):  
Aldose Reductase ◽  
High Speed ◽  
High Performance ◽  
Shikimic Acid ◽  
Aldose Reductase Inhibition ◽  
Mobile Phases ◽  
Wide Range ◽  
Therapeutic Properties ◽  
Counter Current ◽  
First Time

Muehlenbeckia volcanica (Benth.) Endl. (M. volcanica), native to South America, is a traditional Peruvian medicinal plant that has multi-therapeutic properties; however, no phytochemicals have been identified from it yet. In this study, a five-step polarity-stepwise elution counter-current chromatography (CCC) was developed using methanol/water (1:5, v/v) as the stationary phase and different ratios of n-hexane, ethyl acetate, and n-butanol as mobile phases to separate the compounds from the 70% methanol extract of M. volcanica, by which six compounds with a wide range of polarities were separated in a single run of CCC and were identified as gallic acid, protocatechuic acid, 4,4′-dihydroxy-3,3′-imino-di-benzoic acid, rutin, quercitrin, and quercetin. Then, two compounds from the fractions of stepwise elution CCC were separated using conventional high-speed CCC, pH-zone-refining CCC, and preparative high-performance liquid chromatography, and identified as shikimic acid and miquelianin. These compounds are reported from M. volcanica for the first time. Notably, except for shikimic acid, all other compounds showed anti-diabetic potentials via antioxidant, antiglycation, and aldose reductase inhibition. The results suggest that the polarity-stepwise elution CCC can be used to efficiently separate or fractionate compounds with a wide range of polarities from natural products. Moreover, M. volcanica and its bioactive compounds are potent anti-diabetic agents.

A high performance liquid chromatographic assay for the mycotoxin phomopsin A in lupin stubble

1987 ◽  
Vol 27 (1) ◽  
pp. 73 ◽  
Author(s):  
GR Hancock ◽  
P Vogel ◽  
DS Petterson
Keyword(s):  
High Performance ◽  
Limit Of Detection ◽  
High Performance Liquid Chromatographic ◽  
Exchange Chromatography ◽  
Reverse Phase ◽  
Extraction And Purification ◽  
Wide Range ◽  
Total Analysis ◽  
The Mean ◽  
Liquid Chromatographic

An assay using high performance liquid chromatography to measure phomopsin A, the principal mycotoxin responsible for lupinosis is described. Samples of lupin stubble are extracted with methanol: water and purified by partitioning between n-butanol and water, chromatography on Amberlite XAD-2 and by cation exchange chromatography. The analysis is performed on a reverse phase C18 column using a methanol:water gradient and UV detection. The limit of detection for this procedure is 0.5 mg phomopsin A per kg stubble. Improvements to the extraction and purification procedures were made and total analysis time was reduced to 2 days. The mean (� s.d.) recovery for the purification procedure was 64.3 � 4.5% over a wide range of concentrations.

scholarly journals Internal Validation of Rapid and Performant Method for Carotenoids Determination in Tomato Waste Powder by HPLC

2020 ◽  
Vol 71 (1) ◽  
pp. 342-349
Author(s):  
Luminita Catana ◽  
Monica Catana ◽  
Enuta Iorga ◽  
Adrian Constantin Asanica ◽  
Monica-Alexandra Lazar ◽  
...  
Keyword(s):  
High Performance ◽  
Nitrogen Atmosphere ◽  
Good Precision ◽  
Reverse Phase ◽  
Intermediate Precision ◽  
Internal Validation ◽  
Tomato Waste ◽  
Mobile Phases ◽  
Magnetic Stirring ◽  
Β Carotene

An analytical method was developed and validated for separation, detection and quantification of carotenoids (all-trans lutein, β-carotene and all-trans lycopene) in tomato waste powder by high-performance liquid chromatography (HPLC-DAD). Extraction of carotenoids was achieved in acetone under nitrogen atmosphere and magnetic stirring. Carotenoids were separated on a reverse-phase C30, 3 μm column (250 �4.6 mm) coupled to a 20 � 4.6 mm C30 guard column using mobile phases consisting of (A) methanol/ water (98:2, v/v), (B) methanol/water (95:5, v/v) and (C) methyl tert-butyl ether.The method has a good sensitivity (LOD = 0.161 �0.333 μg/mL and LOQ = 0.484 � 1.000 μg/mL) and a good precision (RDS (r) = 0.67 � 1.15% for injection repeatability; RSD (r) = 1.02 � 2.14% for analysis repeatability intra-day; RSD (r) = 1.23 � 2.43% for intermediate precision; RSD (R) = 1.57 � 3.07 % for intra-laboratory reproducibility. The method was applied byanalyzing 8 tomato waste powders, obtained through tomatoes processing as juice. Their carotenoids content varied in the following ranges: 1.474 � 2.452 mg/100g for all-trans lutein; 9.645 � 11.587 mg/100g for β-carotene; 60.150 - 64.855 mg/100g for all-trans lycopene.

scholarly journals A new RP-HPLC method as an auxiliary tool for optimization of sample preparation procedures for tracing of PPCPs of different hydrophilicities

2021 ◽  
Vol 71 (2) ◽  
pp. 305-315
Author(s):  
Omar J. Portillo-Castillo ◽  
Rocío Castro-Ríos ◽  
Abelardo Chávez-Montes ◽  
Azucena González-Horta ◽  
Norma Cavazos-Rocha ◽  
...  
Keyword(s):  
Sample Preparation ◽  
High Performance ◽  
Reversed Phase ◽  
Hplc Method ◽  
Suitable Alternative ◽  
Analytical Technique ◽  
Rp Hplc ◽  
Mobile Phases ◽  
Wide Range ◽  
Gradient Mode

AbstractRecently, pharmaceutical and personal care products (PPCPs) have received considerable attention because of their increasing use. Analysis of PPCPs presents a significant analytical challenge, with high-performance liquid chromatography (HPLC) in reversed-phase mode, as the most widely used analytical technique. To facilitate the optimization of the procedures that are applied in the early stages of sample preparation, a simple and fast HPLC method is proposed in this work for the separation of some PPCPs with a wide range of hydrophilicity. Two columns were evaluated (Atlantis dC18 and Discovery HS F5); as for mobile phases: a formate buffer (40 mmol L−1, pH 4) and methanol were tested in a gradient mode. The fluorinated column allowed better separation in a shorter time and better resolution for all analytes (Rs > 1). The proposed method delivered good performance for the tracing of PPCPs and is a suitable alternative to traditional C18-based HPLC methods.

scholarly journals HPLC-DAD Analysis of Hemp Oil Supplements for Determination of Four Cannabinoids: Cannabidiol, Cannabidiolic Acid, Cannabinol and Delta 9-Tetrahydrocannabinol

Separations ◽  
2021 ◽  
Vol 8 (12) ◽  
pp. 227
Author(s):  
Katarzyna Madej ◽  
Aleksandra Chmiołek ◽  
Kamila Szlachta ◽  
Wojciech Piekoszewski
Keyword(s):  
High Performance ◽  
Liquid Extraction ◽  
The Other ◽  
Diode Array ◽  
Diode Array Detection ◽  
Measured Concentration ◽  
Cannabidiolic Acid ◽  
Array Detection ◽  
Hemp Oil

Growing consumer interest in hemp oilseed supplements requires quality control. Therefore, appropriate, effective and verified analytical methods are needed for the determination of some bioactive cannabinoids in them. The aim of the study is to present an extended (compared to our previous research) validated high performance liquid chromatography with diode array detection (HPLC-DAD) method for the determination of four cannabinoids (cannabidiol, cannabidiolic acid, cannabinol and delta-9-tetrahydrocannabinol) in an oil matrix, which was used to determine these cannabinoids in seven commercial hemp oil supplements. In our method, the isolation of the target compounds was based on liquid extraction with acetonitrile combined with the freezing (at −41 °C) of the oil phase. The results show that in some cases, the determined concentrations of cannabinoids in the tested supplements differ significantly from those declared by the manufacturers. As for the main medicinal cannabinoid (CBD) in hemp oil supplements, in two cases, the measured concentration was significantly lower (1.45 and 1.81%) than the declared (5 and 5%), and in the other supplements, the obtained results confirm the declared amount of CBD within the error range from 3.29 to 9.2%. Therefore, to ensure the safe and beneficial use of these supplements by consumers, it is necessary to monitor their cannabinoid composition.

Preparation and Characterization of NH2-Terminal Fibrinogen Bβ Fragments from N-DSK of Human Fibrinogen

1984 ◽  
Vol 51 (01) ◽  
pp. 016-021 ◽  
Author(s):  
S Birken ◽  
G Agosto ◽  
B Lahiri ◽  
R Canfield
Keyword(s):  
High Performance ◽  
Gel Filtration ◽  
Ion Exchange Chromatography ◽  
Exchange Chromatography ◽  
Reverse Phase ◽  
Human Fibrinogen ◽  
Human Volunteers ◽  
Cnbr Cleavage ◽  
Two Peaks

SummaryIn order to investigate the early release of NH2-terminal plasmic fragments from the Bβ chain of fibrinogen, substantial quantities of Bβ 1-42 and Bβ 1-21 are required as immunogens, as radioimmunoassay standards and for infusion into human volunteers to determine the half-lives of these peptides. Towards this end methods that employ selective proteolytic cleavage of these fragments from fibrinogen have been developed. Both the N-DSK fragment, produced by CNBr cleavage of fibrinogen, and Bβ 1-118 were employed as substrates for plasmin with the finding of higher yields from N-DSK. Bβ 1-42 and Bβ 1-21 were purified by gel filtration and ion-exchange chromatography on SP-Sephadex using volatile buffers. When the purified preparation of Bβ 1-42 was chromatographed on reverse-phase high performance liquid chromatography, two peaks of identical amino acid composition were separated, presumably due either to pyroglutamate or to amide differences.

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