UHPLC-UV/PDA Method Validation for Simultaneous Quantification of Luteolin and Apigenin Derivatives from Elaeis guineensis Leaf Extracts: An Application for Antioxidant Herbal Preparation

Luteolin and apigenin derivatives present in oil palm (Elaeis guineensis) leaves (OPL) are reported to possess excellent antioxidant properties relating to numerous health benefits. To meet the global demand for flavonoids, OPL, which is plentifully generated as an agricultural by-product from oil palm plantations, can be further exploited as a new source of natural antioxidant compounds. However, to produce a standardized herbal preparation, validation of the quantification method for these compounds is required. Therefore, in this investigation, we developed and validated an improved and rapid analytical method, ultra-high-performance liquid chromatography equipped with ultraviolet/photodiode array (UHPLC-UV/PDA) for the quantification of 12 luteolin and apigenin derivatives, particularly focusing on flavonoid isomeric pairs: orientin/isoorientin and vitexin/isovitexin, present in various OPL extracts. Several validation parameters were assessed, resulting in the UHPLC-UV/PDA technique offering good specificity, linearity, accuracy, precision, and robustness, where the values were within acceptable limits. Subsequently, the validated method was employed to quantify luteolin and apigenin derivatives from OPL subjected to different drying treatments and extraction with various solvent systems, giving total luteolin (TLC) and apigenin content (TAC) in the range of 2.04–56.30 and 1.84–160.38 µg/mg extract, respectively. Additionally, partial least square (PLS) analysis disclosed the combination of freeze dry-aqueous methanol yielded OPL extracts with high TLC and TAC, which are strongly correlated with antioxidant activity. Therefore, we provide the first validation report of the UHPLC-UV/PDA method for quantification of luteolin and apigenin derivatives present in various OPL extracts, suggesting that this approach could be employed in standardized herbal preparations by adopting orientin, isoorientin, vitexin, and isovitexin as chemical markers.

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Authentication of Greek PDO Kalamata Table Olives: A Novel Non-Target High Resolution Mass Spectrometric Approach

Molecules ◽

10.3390/molecules25122919 ◽

2020 ◽

Vol 25 (12) ◽

pp. 2919

Author(s):

Natasa P. Kalogiouri ◽

Reza Aalizadeh ◽

Marilena E. Dasenaki ◽

Nikolaos S. Thomaidis

Keyword(s):

High Performance ◽

Model Development ◽

Principal Component ◽

Partial Least Square ◽

Least Square ◽

Table Olives ◽

Method Performance ◽

Validation Parameters ◽

Targeted Screening ◽

Mass Spectrometric Approach

Food science continually requires the development of novel analytical methods to prevent fraudulent actions and guarantee food authenticity. Greek table olives, one of the most emblematic and valuable Greek national products, are often subjected to economically motivated fraud. In this work, a novel ultra-high-performance liquid chromatography–quadrupole time of flight tandem mass spectrometry (UHPLC-QTOF-MS) analytical method was developed to detect the mislabeling of Greek PDO Kalamata table olives, and thereby establish their authenticity. A non-targeted screening workflow was applied, coupled to advanced chemometric techniques such as Principal Component Analysis (PCA) and Partial Least Square Discriminant Analysis (PLS-DA) in order to fingerprint and accurately discriminate PDO Greek Kalamata olives from Kalamata (or Kalamon) type olives from Egypt and Chile. The method performance was evaluated using a target set of phenolic compounds and several validation parameters were calculated. Overall, 65 table olive samples from Greece, Egypt, and Chile were analyzed and processed for the model development and its accuracy was validated. The robustness of the chemometric model was tested using 11 Greek Kalamon olive samples that were produced during the following crop year, 2018, and they were successfully classified as Greek Kalamon olives from Kalamata. Twenty-six characteristic authenticity markers were indicated to be responsible for the discrimination of Kalamon olives of different geographical origins.

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Metabolomic Characterization of Commercial, Old, and Red-Fleshed Apple Varieties

Metabolites ◽

10.3390/metabo11060378 ◽

2021 ◽

Vol 11 (6) ◽

pp. 378

Author(s):

Adriana Teresa Ceci ◽

Michele Bassi ◽

Walter Guerra ◽

Michael Oberhuber ◽

Peter Robatscher ◽

...

Keyword(s):

Antioxidant Activity ◽

High Performance ◽

Polyphenolic Compounds ◽

Partial Least Square ◽

Least Square ◽

Antioxidant Compounds ◽

Apple Varieties ◽

Apple Cultivars ◽

Health Features

In this study, a metabolomic investigation was presented to correlate single polyphenolic compounds in apple pulp with quality characteristics such as antioxidant activity and content of phenolic compounds and anthocyanins in apple skin. Since the concentration of these compounds is influenced by environmental factors, the twenty-two apple cultivars originate from the same site. The polyphenolic compounds were analyzed by ultra-high-performance liquid chromatography coupled with triple quadrupole mass spectrometry (UHPLC-QqQ-MS/MS). The antioxidant activity, phenolic content, and anthocyanins were evaluated on the sunny and the shady sides of apple skin by spectrometric assays. In old apple varieties, the measured parameters were higher than in the commercial and red-fleshed varieties. By contrast, the profile of flavan-3-ols and anthocyanins was variable amongst commercial and red-fleshed varieties. The partial least square (PLS) method was applied to investigate the association between the skin proprieties and the metabolic profile of the pulp. The highest coefficients of determination in prediction (Q2) were obtained for compounds quantified in old cultivars. These results provided information to define the old apple varieties as a reliable group based on the pathway of the antioxidant compounds and anthocyanins content. Our results show the possibility to find cultivars with promising health features based on their content of polyphenols suitable for commercialization or breeding.

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A Novel Validated Injectable Colistimethate Sodium Analysis Combining Advanced Chemometrics and Design of Experiments

Molecules ◽

10.3390/molecules26061546 ◽

2021 ◽

Vol 26 (6) ◽

pp. 1546

Author(s):

Ioanna Dagla ◽

Anthony Tsarbopoulos ◽

Evagelos Gikas

Keyword(s):

Design Of Experiments ◽

High Performance ◽

Similarity Index ◽

Principal Component ◽

Partial Least Square ◽

Least Square ◽

Partial Least Square Regression ◽

Distance Measures ◽

Linear Regression Models ◽

Colistimethate Sodium

Colistimethate sodium (CMS) is widely administrated for the treatment of life-threatening infections caused by multidrug-resistant Gram-negative bacteria. Until now, the quality control of CMS formulations has been based on microbiological assays. Herein, an ultra-high-performance liquid chromatography coupled to ultraviolet detector methodology was developed for the quantitation of CMS in injectable formulations. The design of experiments was performed for the optimization of the chromatographic parameters. The chromatographic separation was achieved using a Waters Acquity BEH C8 column employing gradient elution with a mobile phase consisting of (A) 0.001 M aq. ammonium formate and (B) methanol/acetonitrile 79/21 (v/v). CMS compounds were detected at 214 nm. In all, 23 univariate linear-regression models were constructed to measure CMS compounds separately, and one partial least-square regression (PLSr) model constructed to assess the total CMS amount in formulations. The method was validated over the range 100–220 μg mL−1. The developed methodology was employed to analyze several batches of CMS injectable formulations that were also compared against a reference batch employing a Principal Component Analysis, similarity and distance measures, heatmaps and the structural similarity index. The methodology was based on freely available software in order to be readily available for the pharmaceutical industry.

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Metabolomics profiling of Polygoni Multiflori Radix and Polygoni Multiflori Radix Preparata extracts using UPLC-Q/TOF-MS

Chinese Medicine ◽

10.1186/s13020-019-0268-3 ◽

2019 ◽

Vol 14 (1) ◽

Cited By ~ 1

Author(s):

Zhaoyan Zhang ◽

Liang Yang ◽

Xiaoyan Huang ◽

Yue Gao

Keyword(s):

High Performance ◽

Principal Component ◽

Partial Least Square ◽

Least Square ◽

Alpha Linolenic Acid ◽

Multivariate Statistical ◽

Biochemical Indicators ◽

Flight Mass Spectrometry ◽

Underlying Mechanisms ◽

Tof Ms

Abstract Background The side effects caused by Polygoni Multiflori Radix (PMR) and Polygoni Multiflori Radix Praeparata (PMRP) have often appeared globally. There is no research on the changes of endogenous metabolites among PMR- and PMRP-treated rats. The aim of this study was to evaluate the varying metabolomic effects between PMR- and PMRP-treated rats. We tried to discover relevant differences in biomarkers and endogenous metabolic pathways. Methods Hematoxylin and eosin staining and immunohistochemistry staining were performed to find pathological changes. Biochemical indicators were also measured, one-way analysis of variance with Dunnett’s multiple comparison test was used for biochemical indicators comparison among various groups. Metabolomics analysis based on ultra-high performance liquid chromatography-quadrupole time of flight mass spectrometry (UPLC-Q/TOF-MS) was performed to find the changes in metabolic biomarkers. Multivariate statistical approaches such as principal component analysis (PCA) and orthogonal partial least square-discriminant analysis (OPLS-DA) were applied to reveal group clustering trend, evaluate and maximize the discrimination between the two groups. MetaboAnalyst 4.0 was performed to find and confirm the pathways. Results PMR extracts exhibited slight hepatotoxic effects on the liver by increasing aspartate and alanine aminotransferase levels. Twenty-nine metabolites were identified as biomarkers, belonging to five pathways, including alpha-linolenic acid metabolism, taurine and hypotaurine metabolism, glycerophospholipid metabolism, arginine and proline metabolism, and primary bile acid biosynthesis. Conclusion This study provided a comprehensive description of metabolomic changes between PMR- and PMRP-treated rats. The underlying mechanisms require further research.

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Products Derived from Buchenavia tetraphylla Leaves Have In Vitro Antioxidant Activity and Protect Tenebrio molitor Larvae against Escherichia coli-Induced Injury

Pharmaceuticals ◽

10.3390/ph13030046 ◽

2020 ◽

Vol 13 (3) ◽

pp. 46

Author(s):

Tiago Fonseca Silva ◽

José Robson Neves Cavalcanti Filho ◽

Mariana Mirelle Lima Barreto Fonsêca ◽

Natalia Medeiros dos Santos ◽

Ana Carolina Barbosa da Silva ◽

...

Keyword(s):

Escherichia Coli ◽

Lethal Dose ◽

Antioxidant Properties ◽

Tenebrio Molitor ◽

Antioxidant Compounds ◽

Antioxidant Action ◽

Leaf Extracts ◽

E Coli ◽

Tenebrio Molitor Larvae

The relevance of oxidative stress in the pathogenesis of several diseases (including inflammatory disorders) has traditionally led to the search for new sources of antioxidant compounds. In this work, we report the selection of fractions with high antioxidant action from B. tetraphylla (BT) leaf extracts. In vitro methods (DPPH and ABTS assays; determination of phenolic and flavonoid contents) were used to select products derived from B. tetraphylla with high antioxidant action. Then, the samples with the highest potentials were evaluated in a model of injury based on the inoculation of a lethal dose of heat-inactivated Escherichia coli in Tenebrio molitor larvae. Due to its higher antioxidant properties, the methanolic extract (BTME) was chosen to be fractionated using Sephadex LH-20 column-based chromatography. Two fractions from BTME (BTFC and BTFD) were the most active fractions. Pre-treatment with these fractions protected larvae of T. molitor from the stress induced by inoculation of heat-inactivated E. coli. Similarly, BTFC and BTFD increased the lifespan of larvae infected with a lethal dose of enteroaggregative E. coli 042. NMR data indicated the presence of aliphatic compounds (terpenes, fatty acids, carbohydrates) and aromatic compounds (phenolic compounds). These findings suggested that products derived from B. tetraphylla leaves are promising candidates for the development of antioxidant and anti-infective agents able to treat oxidative-related dysfunctions.

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Influence of Solvent on the Component Composition and Antioxidant Properties of Apricot Cake (Prunus armeniaca L.) Extracts

Journal of Chemistry ◽

10.1155/2020/2913454 ◽

2020 ◽

Vol 2020 ◽

pp. 1-10

Author(s):

A. S. Shakun ◽

V. I. Vorobyova ◽

O. E. Chygyrynets ◽

M. I. Skiba

Keyword(s):

High Performance ◽

Raw Materials ◽

Antioxidant Properties ◽

Component Composition ◽

Prunus Armeniaca ◽

Biologically Active ◽

Antioxidant Compounds ◽

Active Compounds ◽

Plant Raw Materials ◽

Prunus Armeniaca L

Antioxidants of natural origin which are based on agroprocessing waste appear as substance with high performance properties. They have complicated structure and contain a complex of biologically active compounds. This is why research of the above is particularly relevant in current competitive market. When working with plant raw materials and isolation of valuable compounds, the urgent issue is the choice of the method (extraction method) and extractant, which will ensure a maximum release of chemically active compounds. Known solvents such as methanol, ethanol, hexane, diethyl ether, and mixtures thereof are usually used for recovery. The purpose of this research was to study the effect of selected nonpolar solvents on the phytochemical composition and the antioxidant capacity of Prunus armeniaca L. Extracts were obtained using ethanol, silicone, propan-2-ol, and mixtures of ethanol silicone and propan-2-ol with silicone. In the obtained extracts, identification of the sequestered chemically active compounds was carried out by means of chromatography, mass spectrometry, and IR and UV spectrometry, and the extracts were evaluated on antioxidant properties. Various extracts showed varying degrees of antioxidant activity in various test systems, depending on the concentration. Since various antioxidant compounds have different mechanisms of action, several methods have been used to evaluate the effectiveness of antioxidant extracts. The results showed that the test solvents play an important role in the extraction of the plant material into the component composition, as well as the antioxidant ability of Prunus armeniaca L.

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Phenol Profiling and Nutraceutical Potential of Lycium spp. Leaf Extracts Obtained with Ultrasound and Microwave Assisted Techniques

Antioxidants ◽

10.3390/antiox8080260 ◽

2019 ◽

Vol 8 (8) ◽

pp. 260 ◽

Cited By ~ 9

Author(s):

Luna Pollini ◽

Rachele Rocchi ◽

Lina Cossignani ◽

Jordi Mañes ◽

Dario Compagnone ◽

...

Keyword(s):

Antioxidant Properties ◽

In Vitro Assays ◽

Array Detector ◽

Antioxidant Compounds ◽

Ultrasound Assisted Extraction ◽

Leaf Extracts ◽

Phenol Compounds ◽

Microwave Assisted ◽

Assisted Extraction

In recent years, agricultural and industrial residues have attracted a lot of interest in the recovery of phytochemicals used in the food, pharmaceutical, and cosmetic industries. In this paper, a study on the recovery of phenol compounds from Lycium spp. leaves is presented. Ultrasound-assisted extraction (UAE) and microwave-assisted extraction (MAE) have been used with alcoholic and hydroalcoholic solvents. Methanolic UAE was the most successful technique for extracting phenols from Lycium leaves, and we used on leaves from L. barbarum and L. chinense cultivated in Italy. The extracts were then characterized as regards to the antioxidant properties by in vitro assays and the phenol profiling by a high performance liquid chromatography-diode array detector (HPLC-DAD). Chlorogenic acid and rutin were the main phenol compounds, but considerable differences have been observed between the samples of the two Lycium species. For example, cryptochlorogenic acid was found only in L. barbarum samples, while quercetin-3-O-rutinoside-7-O-glucoside and quercetin-3-O-sophoroside-7-O-rhamnoside only in L. chinense leaves. Finally, multivariate statistical analysis techniques applied to the phenol content allowed us to differentiate samples from different Lycium spp. The results of this study confirm that the extraction is a crucial step in the analytical procedure and show that Lycium leaves represent an interesting source of antioxidant compounds, with potential use in the nutraceutical field.

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Pharmaceutical Applications of Chemometric Techniques

ISRN Analytical Chemistry ◽

10.1155/2013/795178 ◽

2013 ◽

Vol 2013 ◽

pp. 1-13 ◽

Cited By ~ 14

Author(s):

Inderbir Singh ◽

Prateek Juneja ◽

Birender Kaur ◽

Pradeep Kumar

Keyword(s):

High Performance ◽

Near Infrared ◽

Partial Least Square ◽

Least Square ◽

Solid Dosage Forms ◽

Solid Dosage ◽

Bilinear Models ◽

Process Testing ◽

Pulse Spectroscopy ◽

Parallel Factor

Chemometrics involves application of various statistical methods for drawing vital information from various manufacturing-related processes. Multiway chemometric models like parallel factor analysis (PARAFAC), Tucker-3, N-partial least square (N-PLS), and bilinear models like principle component regression (PCR) and partial least squares (PLS) have been discussed in the paper. Chemometric approaches can be used to analyze the data obtained from various instruments including near infrared (NIR), attenuated total reflectance Fourier transform infrared (ATR-FTIR), high-performance liquid chromatography (HPLC), and terahertz pulse spectroscopy. The technique has been used in the quality assurance and quality control of pharmaceutical solid dosage forms. Moreover, application of chemometric methods in the evaluation of properties of pharmaceutical powders and tablet parametric tests has also been discussed in the review. It has been suggested as a useful method for the real-time in-process testing and is a valuable process analytical tool.

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A Study on Gentiana dahurica Fisch Ethanol Extract Alleviating Alcoholic Liver Disease in Mice: A Metabolomic Analysis of the Liver

Evidence-based Complementary and Alternative Medicine ◽

10.1155/2021/5569538 ◽

2021 ◽

Vol 2021 ◽

pp. 1-7

Author(s):

Houkang Cao ◽

Yanxiu Guo ◽

Ling Jin

Keyword(s):

High Performance ◽

Principal Component ◽

Ethanol Extract ◽

Partial Least Square ◽

Least Square ◽

Control Group ◽

Metabolomic Analysis ◽

Pyrimidine Metabolism ◽

Alcohol Group ◽

Glucose And Lipid Metabolism

We clarified the hepatoprotective effect of Gentiana dahurica Fisch ethanol extract (GDEE) in our previous study, and we further revealed the mechanism with the help of metabolomics technology in this study. The livers from Control group, Alcohol group, and Alcohol + GDEE group were analyzed by metabolomics. The metabolites in the liver were separated by ultra-high-performance liquid chromatography (UHPLC) and were tentatively identified using mass spectrometry (MS)/MS analysis. Differential metabolites were defined with VIP > 1 and P < 0.05 . Principal component analysis (PCA) and orthogonal partial least square discriminant analysis (OPLS-DA) were applied to analyze differences among these groups. The results showed that the groups could be clearly distinguished by PCA and OPLS-DA analysis. Alcohol and GDEE could change the overall profile of liver metabolites. Alterations in liver tissues of ALD mice induced by alcohol were mainly involved in the dipeptides, purine and pyrimidine metabolism and glucose and lipid metabolism, which could be partly affected by GDEE. This study revealed that the mechanism of GDEE in alleviating ALD had the characteristics of multitarget and multipathway.

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Flavonoid Composition and Pharmacological Properties of Elaeis guineensis Jacq. Leaf Extracts: A Systematic Review

Pharmaceuticals ◽

10.3390/ph14100961 ◽

2021 ◽

Vol 14 (10) ◽

pp. 961

Author(s):

Wai-Kit Tow ◽

Asly Poh-Tze Goh ◽

Usha Sundralingam ◽

Uma Devi Palanisamy ◽

Yasodha Sivasothy

Keyword(s):

Systematic Review ◽

Oil Palm ◽

Elaeis Guineensis ◽

Total Phenolic ◽

Palm Tree ◽

Pharmacological Properties ◽

Leaf Extracts ◽

Flavonoid Composition ◽

Elaeis Guineensis Jacq ◽

Promising Source

The oil palm tree (Elaeis guineensis Jacq.) originates from West and Central Africa, and it is cultivated in Malaysia for its oil-producing fruits. Malaysia is the world’s second largest palm oil producer and the world’s largest exporter to date. Consequently, the Malaysian oil palm industry constantly generates a huge amount of biomass with the major contributor being the leaves. A large percentage of these leaves remain underutilized, making them a promising source of raw materials that can be converted into value-added products. The present review summarizes and discusses the flavonoid composition, total phenolic and flavonoid content, and the in vitro and in vivo pharmacological properties exhibited by the extracts of the leaves of E. guineensis. The purpose of this systematic review is to highlight the potential of valorizing the leaf extracts of the oil palm tree as pharmaceutical and cosmeceutical agents.

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