Development and Validation of a UHPLC-DAD Method for the Quantitative Analysis of Major Dihydrochalcone Glucosides from Thonningia sanguinea VAHL

Planta Medica ◽  
2019 ◽  
Vol 85 (11/12) ◽  
pp. 911-916 ◽  
Author(s):  
Luca Pompermaier ◽  
Stefan Schwaiger ◽  
Monizi Mawunu ◽  
Thea Lautenschlaeger ◽  
Hermann Stuppner
Keyword(s):  
Gradient Elution ◽  
Array Detector ◽  
Bioactive Constituents ◽  
Ultrasound Assisted Extraction ◽  
Complex Samples ◽  
Photodiode Array Detector ◽  
In The Wild ◽  
Elution Method ◽  
Thonningia Sanguinea ◽  
Liquid Chromatographic

Abstract Thonnigia sanguinea is a plant widely used in traditional African medicine against a variety of diseases. The obligate parasite is growing throughout tropical African forests and utilizes a large variety of hosts. Dihydrochalcone glucoside derivatives isolated from the subaerial parts of this plant were identified as potential antidiabetic lead compounds. In this study, an ultrahigh-performance liquid chromatographic method coupled with a photodiode array detector was developed for the quantitation of six major dihydrochalcone derivatives. The analytes were baseline separated in complex samples within 14 minutes on a Phenomenex Luna Omega 1.6 µm C18 column using a mobile phase consisting of water and acetonitrile (each + 0.01% trifluoroacetic acid) in gradient elution. Method validation confirmed the selectivity, linearity (R2 ≥ 0.9992), precision (inter-day ≤ 1.98%, intraday ≤ 2.00%), and accuracy (recovery rates of 97.4 – 106.3% for all analytes). At 280 nm, the LODs and LOQs were found to be lower than 1.42 and 4.30 µg/mL, respectively. Eight plant batches from the northern Angolan province of Uíge (collected in the wild or bought on markets) were extracted with methanol using an ultrasound-assisted extraction protocol and subsequently analyzed with the validated method. Results indicated high contents of dihydrochalcone glucosides in all eight samples. Most notably, the two bioactive constituents thonningianin A and B were present in fairly large amounts (2.42 – 5.35 w%).

Toxicological screening of drugs by microbore high-performance liquid chromatography with photodiode-array detection and ultraviolet spectral library searches

1991 ◽  
Vol 37 (7) ◽  
pp. 1210-1215 ◽  
Author(s):  
A Turcant ◽  
A Premel-Cabic ◽  
A Cailleux ◽  
P Allain
Keyword(s):  
High Performance ◽  
Gradient Elution ◽  
Reversed Phase ◽  
Array Detector ◽  
Photodiode Array Detection ◽  
Photodiode Array Detector ◽  
Degree Of Confidence ◽  
Photodiode Array ◽  
High Degree ◽  
Liquid Chromatographic

Abstract We use ultraviolet data, acquired with a photodiode-array detector coupled to a reversed-phase liquid-chromatographic system, to identify unknown drugs in plasma samples of acutely poisoned patients. Both retention time and spectra of the peaks obtained with a microbore Hypersil ODS column under gradient elution are compared with a library of approximately 350 compounds. We present our three-year experience with this system, which identifies drugs in less than 1 h, with a high degree of confidence.

A Novel HPLC Method for Simultaneous Determination of Methyl, Ethyl, n-propyl, Isopropyl, n-butyl, Isobutyl and Benzyl Paraben in Pharmaceuticals and Cosmetics

2020 ◽  
Vol 23 ◽  
Author(s):  
Saniye Özcan ◽  
Serkan Levent ◽  
Nafiz Öncü Can
Keyword(s):  
High Performance ◽  
Gradient Elution ◽  
High Performance Liquid Chromatographic ◽  
Hplc Method ◽  
Array Detector ◽  
Methyl Ethyl ◽  
Photodiode Array Detector ◽  
Photodiode Array ◽  
Liquid Chromatographic

: The alkyl esters of p-hydroxybenzoic acid at the C-4 position, “the parabens,” including methyl, ethyl, propyl, and butyl, are widely used as antimicrobial preservatives in foods, cosmetics, and pharmaceuticals. Official regulations on the use of these compounds make their analysis essential for the estimation of their exposure. On this basis, the presented study was realized to develop a simple, selective and cheap high-performance liquid chromatographic method for the quantitative determination of methyl paraben (MP), ethyl paraben (EP), n-propyl paraben (NPP), isopropyl paraben (IPP), n-butyl paraben (NBP), isobutyl paraben (IBP) and benzyl paraben (BP) in pharmaceuticals and cosmetic products. The chromatographic separation of the analytes was achieved under flow rate gradient elution conditions using a C18-bonded core-shell silica particle column (2.6 μm particle size, 150 × 3.0 mm from Phenomenex Co.). The samples were injected into the system as aliquots of 1.0 μL, and the compounds were detected by using a photodiode array detector set at 254 nm wavelength. With this technique, seven paraben derivatives can be determined in the concentration range of 250-2000 ng/mL. The recovery of the method is in the range of 99.95-13.84%, and the RSD is at a maximum value of 3.95%. The proposed method was fully validated and successfully applied to different pharmaceutical and cosmetic samples (n=16), including syrups, suspensions, oral sprays, gels, etc. At least one paraben derivative was detected in six of the samples, and was determined quantitatively. The maximum amount of a paraben derivative found in the analyzed samples is 321.7 ng/mL, which was MP. To the best of our knowledge, this is the first LC method, which is applicable both on pharmaceutical and cosmetic samples.

scholarly journals HPLC Characterization and Assessment of Antioxidant Status of Vetiveria Zizanioides Roots

2019 ◽  
Vol 8 (2S10) ◽  
pp. 482-485
Keyword(s):  
Phenolic Acids ◽  
Cell Damage ◽  
Gradient Elution ◽  
Array Detector ◽  
Root Extract ◽  
Enzymatic Antioxidants ◽  
Vetiveria Zizanioides ◽  
Photodiode Array Detector ◽  
Photodiode Array ◽  
Liquid Chromatographic

Vetiveria zizanioides has been assigned for the extraction of phenolic acids and flavonoids for soluble, glycoside and wall-bound fractions. There was the largest number of phenolic acids and flavonoids in the methanolic extract that constitutes the cell wall-bound portion. Free radicals can induce biomolecules to oxidize, resulting in cell damage and countless illnesses. The present study investigates the role of enzymatic antioxidants, i.e. catalase, superoxide dismutase, glutathione peroxidase,glutathione reductase.Vitamin Eand C enzyme activity was nonenzymaticantioxidant action by spectrophotometric method. The enzymatic glutothi-one peroxidase antioxidant was found to be exampling than the rest while Vitamin E, notified found to be best activity ratherthan Vitamin C.The reversed highperformance liquid chromatographic techniquewas created and validated for the concurrent identification of free phenolic acids and flavonoids using a photodiode array detector with gradient elution.(Caffeicacid, Hydroxy benzoic acid, Rutin, Quercetin, Para- cumaric acid and Kaempferol) in the methanolic root extract of Vetiveria zizanioides.

scholarly journals Development and Validation of a High-Performance Liquid Chromatographic Method for the Simultaneous Quantification of Marker Constituents in Cheonwangbosimdan

2014 ◽  
Vol 9 (12) ◽  
pp. 1934578X1400901
Author(s):  
Chang-Seob Seo ◽  
Hyeun-Kyoo Shin
Keyword(s):  
High Performance ◽  
Correlation Coefficients ◽  
Gradient Elution ◽  
High Performance Liquid Chromatographic ◽  
Array Detector ◽  
Mobile Phases ◽  
Photodiode Array Detector ◽  
Relative Standard ◽  
Development And Validation ◽  
Liquid Chromatographic

A high-performance liquid chromatography–photodiode array detector method was established for the simultaneous determination of 7 components in Cheonwangbosimdan extract. The components were 5-hydroxymethyl-2-furaldehyde (1), coptisine (2), berberine (3), nodakenin (4), harpagoside (5), cinnamic acid (6), and β-asarone (7). All analytes were separated by gradient elution using two mobile phases on a Gemini C18 column and maintained at 40°C. The flow rate was 1.0 mL/min and the injection volume was 10 μL. Calibration curves of the 7 compounds showed good linearity with correlation coefficients ( r2) ≥ 0.9996. The limits of detection and quantification of the 7 analytes were 0.01–0.04 and 0.03–0.12 μg/mL, respectively. The recoveries of the 7 marker constituents were 97.6–104.2% with relative standard deviations (RSD) of less than 2.2%. The RSD values of intra- and interday precision were 0.11–1.78 and 0.19–1.92%, respectively. Among the 7 biomarker compounds, the major compounds of Cheonwangbosimdan were berberine and coptisine, which originated from Coptis japonica. The results indicate that the developed analytical method is suitable for quality control use.

Analysis of Rotenone in Cube and Derris Root Powders and Formulations by Liquid Chromatography

1988 ◽  
Vol 71 (2) ◽  
pp. 323-324
Author(s):  
Rodney J Bushway ◽  
Angela Yang ◽  
Ali AL-Yamany
Keyword(s):  
Liquid Chromatography ◽  
Mixed Solvent ◽  
Array Detector ◽  
Photodiode Array Detector ◽  
Coefficients Of Variation ◽  
Powder Samples ◽  
Photodiode Array ◽  
Aoac Official ◽  
Liquid Chromatographic ◽  
Good Agreement

Abstract A modified liquid chromatographic (LC) procedure, including an improved extraction, has been developed to analyze rotenone in root powders of derris and cube. The procedure is also applicable to formulations. Samples are sonicated for 5 min in chloroform or a mixed solvent of tetrahydrofuran-acetonitrile-water-glacial acetic acid, followed by liquid chromatography. Rotenone content of 4 lots of root powder samples showed good agreement between the new extraction and the AOAC official extraction; coefficients of variation ranged from 5 to 1.2%. Five formulations were also analyzed and showed good agreement with results for methanol extraction. Coefficients of variation were 4.5% or less. Purity of the rotenone peaks was tested by using a photodiode array detector in the spectrum and UV ratio modes. It is recommended that the new method be tested collaboratively.

scholarly journals SIMULTANEOUS QUANTIFICATION OF PENTAZOCINE AND NALOXONE BY STABILITY INDICATING REVERSE-PHASE-HIGH-PERFORMANCE LIQUID CHROMATOGRAPHIC METHOD

2019 ◽  
pp. 257-262
Author(s):  
RAMA KUMAR KANDULA ◽  
RAJA SUNDARARAJAN
Keyword(s):  
High Performance ◽  
High Performance Liquid Chromatographic ◽  
Hplc Method ◽  
Array Detector ◽  
Forced Degradation ◽  
Stability Indicating ◽  
Photodiode Array Detector ◽  
Photodiode Array ◽  
Alkali Hydrolysis ◽  
Liquid Chromatographic

Objective: The objective of the study was to develope a stability indicating high-performance liquid chromatographic (HPLC) method for simultaneous assay of pentazocine and naloxone in bulk and tablets. Methods: Pentazocine and naloxone were analyzed on Dionex C18 column using 0.1M K2HPO4 buffer (pH 4.0) and methanol (60:40, v/v) as the mobile phase. The concentration of pentazocine and naloxone was quantified by photodiode array detector set at 248 nm. The method was validated in compliance with ICH rules. Pentazocine and naloxone tablet formulation was subjected to forced degradation such as acid, neutral and alkali hydrolysis, oxidation, photo, and thermal degradation. Results: The method was linear, with R2=0.9999 in the concentration range 100–300 μg/ml for pentazocine and R2=0.9995 in the concentration range 1–3 μg/ml for naloxone. The level of detection and quantification was 0.097 μg/ml and 0.322 μg/ml for pentazocine and 0.0073 μg/ml and 0.0243 μg/ml for naloxone, respectively. The degraded products are resolved well from pentazocine and naloxone with significantly different retention time values. From validation results, it was proved that the method is selective, precise, robust, and accurate for the estimation of pentazocine and naloxone simultaneously. Conclusion: The developed stability-indicating HPLC method can be applied for quantitative determination of pentazocine and naloxone in tablets.

Simultaneous Determination of Diazinon and Chlorpyrifos Pesticide Formulations by Liquid Chromatography

1988 ◽  
Vol 71 (2) ◽  
pp. 321-322 ◽  
Author(s):  
Rodney J Bushway ◽  
L Brian Perkins ◽  
King M Joan
Keyword(s):  
Internal Standard ◽  
Butylated Hydroxytoluene ◽  
Array Detector ◽  
Photodiode Array Detector ◽  
Coefficients Of Variation ◽  
Pesticide Formulations ◽  
Photodiode Array ◽  
Total Analysis ◽  
Liquid Chromatographic

Abstract A liquid chromatographic (LC) method has been developed to analyze simultaneously separate formulations of diazinon and chlorpyrifos. Samples of each formulation were mixed in a Polytron mixer with the internal standard butylated hydroxytoluene and were diluted with acetonitrile. An aliquot was injected into an Ultremex LC column. The mobile phase was acetonitrile-water-tetrahydrofuran-glacial acetic acid-monoethanolamine (480 + 230 + 55 + 2 + 0.75); all 3 compounds were monitored at 230 nm. Total analysis time was 11 min. Combinations of 11 different samples of each formulated pesticide were analyzed 9 times for coefficients of variation generally less than 3%. Purity of the diazinon, chlorpyrifos, and butylated hydroxytoluene was checked by using a photodiode array detector in the spectrum and absorbance ratio modes. No interferences were noted at 230 nm.

scholarly journals Method development and validation for Cabotegravir and Rilpivirine by using HPLC and its degradants are characterized by LCMS and FTIR

2021 ◽  
Vol 7 (1) ◽  
Author(s):  
Anuradha Vejendla ◽  
Subrahmanyam Talari ◽  
Raju Moturu ◽  
S. N. Murthy Boddapati ◽  
A. Emmanuel Kola
Keyword(s):  
High Performance ◽  
Method Development ◽  
High Performance Liquid Chromatographic ◽  
Array Detector ◽  
Forced Degradation ◽  
Current Application ◽  
Pharmaceutical Ingredients ◽  
Photodiode Array Detector ◽  
Development And Validation ◽  
Liquid Chromatographic

Abstract Background Using a Symmetry C18 (4.6 × 150 mm, 3.5) column, a high-performance liquid chromatographic method for quantification of Rilpivirine and Cabotegravir in active pharmaceutical ingredients was developed and validated. The mobile phase is made up of buffer, acetonitrile, and 0.1 percent formic acid in a 20:80v/v ratio. The flow rate was kept constant at 1.0 ml/min, and detection was accomplished through absorption at 231 nm with a photodiode array detector. Results The calibration curve was linear, with a regression coefficient (R2) value of 0.999 and concentrations ranging from 30 to 450 g/ml of Rilpivirine and 20–300 g/ml of Cabotegravir. The method's LOD and LOQ were 0.375 g/ml, 1.238 g/ml, and 0.25 g/ml, 0.825 g/ml for Rilpivirine and Cabotegravir, respectively. Conclusions In the forced degradation studies, the degradants were characterized by using LCMS and FTIR. The current application was found to be simple, economical, and suitable, and validated according to ICH guidelines.

scholarly journals MITRAGYNINE PERCENTAGES OF VARIOUS KRATOM VARIANTS SEIZED IN INDONESIA: A QUANTITATIVE ANALYSIS USING LIQUID CHROMATOGRAPHY-PHOTO DIODE ARRAY DETECTOR

2021 ◽  
pp. 252-256
Author(s):  
TANTI ◽  
CHRISTIEN ANDRIYANI LALANGI ◽  
ERI ARFIYANI ◽  
WIDIANTI NINGTIAS ◽  
ERLANA NINDYA MAULIDA
Keyword(s):  
Liquid Chromatography ◽  
Analytical Methods ◽  
Uv Light ◽  
Gradient Elution ◽  
Array Detector ◽  
Mobile Phases ◽  
Photodiode Array Detector ◽  
Photodiode Array ◽  
Layer Chromatography

Objective: This study details the determination of mitragynine in various kratom samples using the thin-layer chromatography (TLC) technique and validation of analytical methods for quantifying the concentration of mitragynine in various kratom samples using liquid chromatography with photodiode array detector (LC-PDA). Methods: TLC technique using n-hexane: ethyl acetate: ammonia 25% (30: 15: 1 v/v/v) was applied to isolate mitragynine from kratom samples. Several interesting spots obtained were visualized under UV light at 254 nm. Samples were also prepared with organic solvent extraction directly prior to LC analysis (non-isolation method of preparation) to quantify the concentration of mitragynine. Mobile phases used were acetonitrile (MP A) and 0.1% formic acid in water (MP B). Samples and standards were run by gradient elution with a flow rate of 0.3 ml/min, detection using PDA detector at 254 nm. Results: Mitragynine was successfully isolated from kratom samples in Rf 0.50 by TLC system applied. The validation of analytical methods for mitragynine passed the acceptance criteria as described by UNODC Guidance. The concentration of mitragynine in various kratom samples seized in Indonesia ranged from 0.37%-1.70% (%w/w). Conclusion: Both TLC and LC analytical methods could be applied to determine and quantify the concentration of mitragynine in each examined sample, respectively.

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