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1.
Anal Methods ; 16(16): 2513-2521, 2024 04 25.
Article in English | MEDLINE | ID: mdl-38587209

ABSTRACT

Sweet tea is a functional herbal tea with anti-inflammatory, anti-diabetic, and other effects, in which phloridzin and trilobatin are two functional compounds. However, the current methods for their quantification are time-consuming, costly, and environmentally unfriendly. In this paper, we propose a rapid method that integrates online pressurized liquid extraction and high-performance liquid chromatography featuring a superficially porous column for fast separation. Moreover, we employ an equal absorption wavelength method to eliminate using multiple standard solutions and relative calibration factors. Our verification process corroborated the technique's selectivity, accuracy, precision, linearity, and detection limitations. Separately, our methodology demonstrated excellent analytical efficiency, cost-effectiveness, and environmental friendliness. Practical application using six distinct batches of sweet tea samples yielded results in congruence with the external standard method. The analytical rate of this technique is up to over 18 times faster than traditional methods, and organic solvent consumption has been reduced to less than 1.5 mL. Therefore, this method provides a valuable way to achieve quality control and green analysis of sweet tea and other herbal teas.


Subject(s)
Phlorhizin , Chromatography, High Pressure Liquid/methods , Phlorhizin/analysis , Phlorhizin/chemistry , Teas, Herbal/analysis , Hydrolyzable Tannins/analysis , Liquid-Liquid Extraction/methods , Reproducibility of Results
2.
Food Chem ; 447: 138960, 2024 Jul 30.
Article in English | MEDLINE | ID: mdl-38461727

ABSTRACT

Iron Chlorin e6 (ICE6), a star plant growth regulator (PGR) with independent intellectual property rights in China, has demonstrated its efficacy through numerous field experiments. We innovatively employed salting-out assisted liquid-liquid extraction (SALLE) with HPLC-UV/Vis to detect ICE6 residues in water, soil, garlic seeds, and sprouts. Using methanol and a C18 column with acetonitrile: 0.1% phosphoric acid mobile phase (55:45, v:v), we achieved a low LOQ of 0.43 to 0.77 µg kg-1. Calibration curves showed strong linearity (R2 > 0.992) within 0.01 to 5.00 mg kg-1. Inter-day and intra-day recoveries (0.05 to 0.50 mg kg-1) demonstrated high sensitivity and accuracy (recoveries: 75.36% to 107.86%; RSD: 1.03% to 8.78%). Additionally, density functional theory (DFT) analysis aligned UV/Vis spectra and indicated ICE6's first-order degradation (2.03 to 4.94 days) under various environmental conditions, mainly driven by abiotic degradation. This study enhances understanding of ICE6's environmental behavior, aids in risk assessment, and guides responsible use in agroecosystems.


Subject(s)
Garlic , Metalloporphyrins , Chromatography, High Pressure Liquid/methods , Hydrolysis , Soil , Liquid-Liquid Extraction/methods
3.
Drug Test Anal ; 16(7): 692-707, 2024 Jul.
Article in English | MEDLINE | ID: mdl-38482734

ABSTRACT

Vitamin D3, an essential micronutrient, often requires supplementation via medicines or food supplements, which necessitate quality control (QC). This study presents the development of a method for detecting and quantifying seven impurities of vitamin D3 in oily drug products using supercritical fluid chromatography-mass spectrometry (SFC-MS). Targeted impurities include two esters of vitamin D3 and five non-esters including four that are isobaric to vitamin D3. Firstly, a screening study highlighted the Torus 1-AA column and acetonitrile modifier as adequate for the separation, followed by optimization of the SFC conditions. Secondly, make-up solvent composition and MS settings were optimized to reach high sensitivity. For both the separation and MS response, the screening design of experiments proved useful. Lastly, a fast saponification and liquid-liquid extraction method was developed, enabling efficient sample cleanup and impurities recovery from the complex oily matrix. The SFC-MS method suitability was assessed in two validation studies. The first study employed the ICH Q2 guideline for impurity limit test to demonstrate method specificity and establish a limit of detection (LOD) and a limit of quantification (LOQ) at 0.2% and 0.5%, respectively, for ester impurities. The second study conducted a comprehensive quantitative assessment for three non-ester impurities using a total error approach, determining method validity through accuracy profiles. The validated method exhibited reliable performance across impurity concentrations from 0.1% to 2.0%, with estimated LODs ranging from 2 to 7 ng/mL. This study further promotes SFC-MS as a valuable, versatile, and green tool for routine pharmaceutical QC.


Subject(s)
Cholecalciferol , Chromatography, Supercritical Fluid , Drug Contamination , Limit of Detection , Chromatography, Supercritical Fluid/methods , Cholecalciferol/analysis , Mass Spectrometry/methods , Quality Control , Liquid-Liquid Extraction/methods , Dietary Supplements/analysis , Dietary Supplements/standards
4.
Food Chem ; 439: 138099, 2024 May 01.
Article in English | MEDLINE | ID: mdl-38039613

ABSTRACT

Heating edible oils generates aldehydes, potentially leading to adverse health effects, making their analysis essential for quality control. This study presents a convenient miniaturized kapok fiber-supported liquid-phase extraction/in-situ derivatization method for the simultaneous extraction and derivatization of aldehydes in oils. The method involves placing 150 mg oil into a 1 mL pipette tip packed with 25 mg kapok fiber, adding 150 µL ACN with 1.5 mg mL-1 DNPH, and post 30-minute static extraction, retrieving the extractant with a pipettor for liquid chromatography-tandem mass spectrometry analysis. By optimizing critical parameters through a Box-Behnken design, the method exhibits good linearity (1-500 ng g-1, R2 ≥ 0.991), low detection limits (0.2-1.0 ng g-1), excellent accuracy (95.3-107.1%) and high precisions (relative standard deviation < 7.9%). This method simplifies sample preparation processes, cuts solvent use, and facilitates automation. It effectively identifies ten aldehyde variations in six heated oils, displaying distinct profiles consistent with prior research.


Subject(s)
Aldehydes , Tandem Mass Spectrometry , Tandem Mass Spectrometry/methods , Aldehydes/analysis , Chromatography, Liquid , Liquid-Liquid Extraction/methods , Plant Oils/chemistry , Chromatography, High Pressure Liquid/methods
5.
Chem Biodivers ; 21(2): e202301528, 2024 Feb.
Article in English | MEDLINE | ID: mdl-38116850

ABSTRACT

Immortelle, a revered Mediterranean medicinal plant, is celebrated for its potent essential oil renowned in the cosmetic industry for its skin-enhancing properties. Yet, immortelle hydrosol, an often-overlooked byproduct, holds promise in cosmetics due to its compatibility with polar active ingredients. This study investigates the chemical composition of immortelle hydrosol by employing liquid-liquid extraction (LLE) to transfer volatile organic components into nonpolar solvents. Four solvents - chloroform, dichloromethane, hexane, and benzene - were assessed through ten consecutive extractions from industrially produced immortelle hydrosol. Quantification was achieved using GC analysis with tetradecane as an internal standard. Chloroform emerged as the most efficient solvent, yielding 2447.0 mg/L of volatile compounds, surpassing dichloromethane, hexane, and benzene. Key compounds in immortelle hydrosol included 3-pentanone, 2-methyl-1-butanol, and γ-terpineol. Importantly, the study revealed that a portion of essential oil compounds persists in the hydrosol even after ten LLE cycles, with optimal results achievable in five extractions (~92 % in most cases).


Subject(s)
Hexanes , Oils, Volatile , Solvents , Benzene/analysis , Chloroform/analysis , Methylene Chloride/analysis , Liquid-Liquid Extraction , Oils, Volatile/chemistry
6.
J Chromatogr A ; 1710: 464413, 2023 Nov 08.
Article in English | MEDLINE | ID: mdl-37806044

ABSTRACT

Steroid hormones have been reported to be associated with endocrine system diseases. This paper proposes a novel procedure of deep eutectic solvent (DES)-assisted liquid-liquid extraction (LLE) to extract six steroid hormones (including cortisone, cortisol, androstenedione, testosterone, 17-hydroxyprogesterone, and progesterone) from serum coupled with liquid chromatography-tandem mass spectrometry (LC-MS/MS). A total of five types of L-proline, choline chloride, and citric acid-based DESs were tailored; the DES from L-proline and ethylene glycol at a molar ratio of 1:4 with 20 % acetonitrile was selected as the best-fit assisted solvent for the six steroid hormones compared with other DESs. The parameters for extraction by selected DES were optimized using Box-Behnken design (BBD), and the optimal extraction conditions are 200 µL of acetonitrile, 100 µL of the sample, and 80 µL of DES. Under optimum conditions, the method has good linear calibration ranges (between 0.07 ng mL-1 and 600 ng mL-1), correlation coefficients of determination (r2>0.99), and low limits of quantification (between 0.02 and 0.60 ng mL-1). The extraction recoveries were in the range of 81.84-114.43 %, and the intra-day and inter-day relative standard deviations (RSDs) were less than 10 %.In general, the DES-LC-MS/MS method is a simple and environmentally-friendly method, which can be complementary to the presently available methods for determining steroid hormones in serum.


Subject(s)
Deep Eutectic Solvents , Tandem Mass Spectrometry , Chromatography, Liquid/methods , Limit of Detection , Steroids/analysis , Liquid-Liquid Extraction , Hydrocortisone/analysis , Acetonitriles/analysis , Proline , Chromatography, High Pressure Liquid
7.
Molecules ; 28(14)2023 Jul 18.
Article in English | MEDLINE | ID: mdl-37513364

ABSTRACT

Rosmarinus officinalis leaves (ROLs) are widely used in the food and cosmetics industries due to their high antioxidant activity and fascinating flavor properties. Carnosic acid (CA) and rosmarinic acid (RA) are regarded as the characteristic antioxidant components of ROLs, and the selective separation of CA and RA remains a significant challenge. In this work, the feasibility of achieving the selective separation of CA and RA from ROLs by solid-phase extraction (SPE) and liquid-liquid extraction (LLE) was studied and compared. The experiments suggested that SPE with CAD-40 macroporous resin as the adsorbent was a good choice for selectively isolating CA from the extracts of ROLs and could produce raw CA with purity levels as high as 76.5%. The LLE with ethyl acetate (EA) as the extraction solvent was more suitable for extracting RA from the diluted extracts of ROLs and could produce raw RA with a purity level of 56.3%. Compared with the reported column chromatography and LLE techniques, the developed SPE-LLE method not only exhibited higher extraction efficiency for CA and RA, but can also produce CA and RA with higher purity.


Subject(s)
Plant Extracts , Rosmarinus , Plant Extracts/chemistry , Solid Phase Extraction/methods , Cinnamates/chemistry , Liquid-Liquid Extraction/methods , Rosmarinus/chemistry , Antioxidants/analysis , Chromatography, High Pressure Liquid , Rosmarinic Acid
8.
Molecules ; 28(2)2023 Jan 11.
Article in English | MEDLINE | ID: mdl-36677776

ABSTRACT

In this study, we aimed to develop and validate a pretreatment method for separating and analyzing the small amounts of biomarkers contained in topical cream formulations. Analyzing semisolid formulations that contain low concentrations of active ingredients is difficult. Cream formulations containing an aqueous ethanol extract of 0.1% Agrimonia pilosa is an example. Approximately 0.0013% of apigenin-7-O-glucuronide(A7OG) was contained as a biomarker in the cream. To determine the A7OG content present in the cream formulation, liquid-liquid extraction using dichlormethane was applied. In addition, the volume of the distribution liquid was measured using the peak ratios of the indicator component, A7OG, and an internal standard, baicalin. Subsequently, the A7OG content in the cream formulation was calculated. Using this time-saving method, A7OG can be simply analyzed without additional pretreatment steps, such as evaporation and reconstitution. Moreover, the validation results confirmed that this analytical method met all of the criteria. Consequently, A7OG was successfully isolated from the cream, analyzed, and quantified using the developed method.


Subject(s)
Agrimonia , Plant Extracts , Chromatography, High Pressure Liquid , Water , Ethanol , Liquid-Liquid Extraction
9.
Environ Sci Pollut Res Int ; 30(2): 3432-3439, 2023 Jan.
Article in English | MEDLINE | ID: mdl-35948794

ABSTRACT

Olive oil mill wastewater (OMW) is a major waste stream generated in olive oil industry. It is highly polluted due to phenolic compounds. The present study focused on the physicochemical properties of OMW as well as the quantitative and qualitative effects of two extraction methods of phenolic compounds which were liquid-liquid and maceration methods. Spectrophotometry and high-performance liquid chromatography-electrospray ionization-mass spectrometry (HPLC-ESI-MS) were adopted to quantify the phytochemical contents and the phenolic compounds. The extract obtained by the maceration method showed the highest yields of total polyphenol, flavonoid, and tannin contents. The LC-MS results revealed the presence of 16 phenolic compounds in the macerated, and only 12 phenolic compounds were found in the extract of the second method. Quinic acid was identified as the most abundant compound. Moreover, the macerated extracts possessed the highest antioxidant potential as evidenced by their strong ferric reducing antioxidant power (FRAP) and their 2,2-diphenyl-1-picrylhydrazyl (DPPH), 2,2'-azino-bis(3-ethylbenzothiazoline-6-sulfonate) (ABTS) radical scavenging activities. The phytochemical contents, as well as the antioxidant potentials of OMW after extraction using maceration, were significantly greater than using liquid-liquid method. Therefore, maceration seemed to be the most effective method for extracting phenolic compounds from OMW. The OMW constitute a rich source of natural phenolic compounds that could be used as a potential source of natural antioxidants.


Subject(s)
Antioxidants , Wastewater , Antioxidants/pharmacology , Olive Oil , Phenols/chemistry , Flavonoids/analysis , Liquid-Liquid Extraction , Plant Extracts/pharmacology , Phytochemicals/analysis
10.
Toxins (Basel) ; 14(9)2022 08 28.
Article in English | MEDLINE | ID: mdl-36136531

ABSTRACT

The two main methods for partitioning crude methanolic extract from Amphidinium carterae biomass were compared. The objective was to obtain three enriched fractions containing amphidinols (APDs), carotenoids, and fatty acids. Since the most valuable bioproducts are APDs, their recovery was the principal goal. The first method consisted of a solid-phase extraction (SPE) in reverse phase that, for the first time, was optimized to fractionate organic methanolic extracts from Amphidinium carterae biomass using reverse-phase C18 as the adsorbent. The second method consisted of a two-step liquid-liquid extraction coupled with SPE and, alternatively, with solvent partitioning. The SPE method allowed the recovery of the biologically-active fraction (containing the APDs) by eluting with methanol (MeOH): water (H2O) (80:20 v/v). Alternatively, an APD purification strategy using solvent partitioning proved to be a better approach for providing APDs in a clear-cut way. When using n-butanol, APDs were obtained at a 70% concentration (w/w), whereas for the SPE method, the most concentrated fraction was only 18% (w/w). For the other fractions (carotenoids and fatty acids), a two-step liquid-liquid extraction (LLE) method coupled with the solvent partitioning method presented the best results.


Subject(s)
Dinoflagellida , Methanol , 1-Butanol , Biomass , Carotenoids , Fatty Acids , Liquid-Liquid Extraction , Plant Extracts , Solid Phase Extraction , Solvents , Water
11.
J Oleo Sci ; 71(2): 177-185, 2022.
Article in English | MEDLINE | ID: mdl-35110462

ABSTRACT

Phosphoric acid is used in the refining of palm oil for the removal of phosphatides. The high concentration of phosphorus in solvent extracted palm-pressed mesocarp fiber oil hinders palm oil mills to recover this phytonutrients-rich residual oil in pressed fiber which typically contains 0.1 to 0.2% of total oil yield. This study aimed to refine the palm-pressed mesocarp fiber oil and determine the optimum dosage of phosphoric acid for acid-degumming of palm-pressed mesocarp fiber oil while retaining its phytonutrients. The refining process was carried out with combination of wet degumming, acid degumming, neutralisation, bleaching and deodorization. The optimum dose of phosphoric acid was identified as 0.05 wt.% by incorporating the wet degumming process. The refined palm-pressed mesocarp fiber oil showed a reduction in phosphorus content by 97% (from 901 ppm to 20 ppm) and 97% free fatty acid content removal (from 6.36% to 0.17%), while the Deterioration of Bleachability Index increased from 1.76 to 2.48, which showed an increment of 41%. The refined oil retained the key phytonutrients such as carotenoids (1,150 ppm) and vitamin E (1,540 ppm) that can be further developed into high-value products. The oil meets the quality specification of refined, bleached, and deodorized palm oil while preserving the heat-sensitive phytonutrients, which in turn provides a new resource of nutritious oil.


Subject(s)
Food Handling/methods , Liquid-Liquid Extraction/methods , Palm Oil/chemistry , Phospholipids/isolation & purification , Phosphorus/isolation & purification , Phytochemicals/analysis , Carotenoids/analysis , Food Quality , Palm Oil/analysis , Phospholipids/analysis , Phosphoric Acids/chemistry , Phosphorus/analysis , Solvents , Vitamin E/analysis
12.
Molecules ; 27(4)2022 Feb 17.
Article in English | MEDLINE | ID: mdl-35209151

ABSTRACT

Conventional extraction methods of proanthocyanidins (PAC) are based on toxic organic solvents, which can raise concerns about the use of extracts in supplemented food and nutraceuticals. Thus, a PAC extraction method was developed for grape seeds (GS) and grape seed powder using food-grade ethanol by optimizing the extraction conditions to generate the maximum yield of PAC. Extraction parameters, % ethanol, solvent: solid (s:s) ratio, sonication time, and temperature were optimized by the central composite design of the response surface method. The yields of PAC under different extraction conditions were quantified by the methylcellulose precipitable tannin assay. The final optimum conditions were 47% ethanol, 10:1 s:s ratio (v:w), 53 min sonication time, and 60 °C extraction temperature. High-performance liquid chromatography analysis revealed the presence of catechin, procyanidin B2, oligomeric and polymeric PAC in the grape seed-proanthocyanidin extracts (GS-PAC). GS-PAC significantly reduced reactive oxygen species and lipid accumulation in the palmitic-acid-induced mouse hepatocytes (AML12) model of steatosis. About 50% of the PAC of the GS was found to be retained in the by-product of wine fermentation. Therefore, the developed ethanol-based extraction method is suitable to produce PAC-rich functional ingredients from grape by-products to be used in supplemented food and nutraceuticals.


Subject(s)
Grape Seed Extract/isolation & purification , Grape Seed Extract/pharmacology , Liquid-Liquid Extraction/methods , Proanthocyanidins/isolation & purification , Proanthocyanidins/pharmacology , Animals , Cell Line , Chromatography, High Pressure Liquid , Dose-Response Relationship, Drug , Ethanol , Fermentation , Grape Seed Extract/chemistry , Hepatocytes/drug effects , Hepatocytes/metabolism , Hepatocytes/pathology , Mice , Palmitic Acid/pharmacology , Proanthocyanidins/chemistry , Seeds/chemistry , Solvents , Structure-Activity Relationship , Ultrasonic Waves
13.
J Oleo Sci ; 71(2): 201-213, 2022 Feb 03.
Article in English | MEDLINE | ID: mdl-35034941

ABSTRACT

Baru (Dipteryx alata) almond is an emerging nut from the Brazilian savannah, that presents unique flavor and an interesting specialty oil. In this study, we aimed at investigating the effects of pressure, temperature, type (alcohol and/or water), and concentration of polar cosolvent on the extraction yield and tocopherol contents of baru oil obtained by supercritical-CO2 extraction (SC-CO2); and to investigate the effect of temperature and pressure on phytosterol, phenolic, and volatile compounds' profile in the oil when H2O was the cosolvent. Baru oil extracted with SC-CO2 using alcohol as a cosolvent showed a higher extraction yield (20.5-31.1%) than when using H2O (4.16-22.7%). However, when 0.3% H2O was used as cosolvent, baru oils presented the highest γ-tocopherol (107 and 43.7 mg/100 g) and total tocopherol (212 and 48.7 mg/100 g) contents, depending on the temperature and pressure used (50°C and 10 MPa or 70°C and 30 MPa, respectively). Consequently, the lowest pressure (10 MPa) and temperature (50°C) values resulted in baru oils with better γ/α-ratio, and the highest contents of ß-sitosterol (107 mg/100 g) and phenolic compounds (166 mg/100 g). However, the highest pressure (30 MPa) and temperature (70°C) values improved the volatile profile of oils. Therefore, although alcohol as a cosolvent improved oil yield, small amounts of H2O provided a value-added baru oil with either high content of bioactive compounds or with a distinctive volatile profile by tuning temperature and pressure used during SC-CO2 extraction.


Subject(s)
Carbon Dioxide/chemistry , Dipteryx/chemistry , Liquid-Liquid Extraction/methods , Plant Oils/chemistry , Plant Oils/isolation & purification , Solvents/chemistry , Tocopherols/analysis , Water/chemistry , Alcohols/chemistry , Hydroxybenzoates/analysis , Phytosterols/analysis , Pressure , Temperature , Volatile Organic Compounds/analysis
14.
J Ethnopharmacol ; 282: 114560, 2022 Jan 10.
Article in English | MEDLINE | ID: mdl-34454053

ABSTRACT

ETHNOPHARMACOLOGICAL RELEVANCE: Nauclea officinalis, a widely used Li medicine, has been used for the treatment of cold, fever, bronchitis, pneumonia, acute tonsillitis, and other ailments. Modern pharmacological studies have demonstrated that the most abundant and active components in N. officinalis are alkaloids, which possess various biological properties such as antibacterial and antitumor activities. AIM OF THE STUDY: To investigate the phytochemical profile of a selected group of alkaloids from the N. officinalis total alkaloids, and to determine the chemical profile of the alkaloids extracted from rat plasma. Further investigation was conducted to determine the pharmacokinetic behaviors of 11 selected major alkaloids, including pumiloside, naucleoxoside A, naucleoxoside B, nauclefine, angustidine, angustoline, (3S,19S)-3,14-dihydroangustoline,[α]D20: (-)191°, (3S,19R)-3,14-dihydroangustoline, [α]D20: (-) 294.7°, strictosamide, angustine, and 3,14-dihydroangustine. MATERIALS AND METHODS: N. officinalis total alkaloids were extracted with 79% ethanol and enriched with AB-8 macroporous resin. The phytochemical profile of alkaloids from the N. officinalis total alkaloids and the chemical profile of the alkaloids extracted from rat plasma were first analyzed by UPLC-Q-TOF-MS/MS. A simple, convenient, and sensitive LC-ESI-MS/MS method was subsequently developed and validated for the simultaneous determination of major active alkaloids in rat plasma after oral administration of N. officinalis total alkaloids. After addition of an internal standard (verapamil), plasma samples were pretreated first by protein precipitation with methanol and then underwent liquid-liquid extraction with ethyl acetate. Chromatographic separation was achieved using a Waters BEH C18 column (2.1 mm × 100 mm, 1.7 µm) at 30 °C, with gradient elution using a mobile phase consisting of 0.1% formic acid aqueous solution (A) and acetonitrile (B), a flow rate of 0.2 mL/min, and a total run time of 30 min. The detection was performed using an electrospray ionization triple quadrupole tandem mass spectrometer with multiple reaction monitoring and positive ionization mode. RESULTS: Based on the fragmentation patterns of 11 authentic alkaloids and previous reports, 55 alkaloids were identified or tentatively identified in the N. officinalis total alkaloids. Among them, 25 alkaloids were absorbed through the gastrointestinal tract in rats after administration of the N. officinalis total alkaloids. The 11 alkaloids were selected for quantitative analysis. The established quantitative method was fully validated and proved to be sensitive and specific. Satisfactory linearity of the 11 alkaloids obtained in the respective concentration ranges (r > 0.9931). The lower limits of quantification for strictosamide was 20.86 ng/ml, and the other ten alkaloids were all less than 4.47 ng/ml in rat plasma. The intra-and inter-day precision was less than 15% for all 11 alkaloids in terms of relative standard deviation, and the accuracies ranged from -11.4% to 11.1% in terms of relative error. Extraction recovery, matrix effect, and stability were within the required limits in rat plasma. CONCLUSION: The validated method was successfully applied to investigate the pharmacokinetics of the 11 alkaloids in rat plasma after oral administration of N. officinalis total alkaloids. Eleven alkaloids were rapidly absorbed to achieve a maximum plasma concentration with Tmax from 0.25 h to 1.5 h after oral administration. The pharmacokinetic parameters and plasma concentration-time profiles will prove valuable in pre-clinical and clinical investigations on the disposition of N. officinalis total alkaloids.


Subject(s)
Alkaloids , Plant Extracts , Rubiaceae , Administration, Oral , Alkaloids/chemistry , Alkaloids/classification , Alkaloids/pharmacokinetics , Animals , Chromatography, High Pressure Liquid/methods , Chromatography, Liquid/methods , Drugs, Chinese Herbal/chemistry , Drugs, Chinese Herbal/pharmacokinetics , Evaluation Studies as Topic , Liquid-Liquid Extraction/methods , Plant Extracts/chemistry , Plant Extracts/pharmacology , Rats , Rats, Sprague-Dawley , Spectrometry, Mass, Electrospray Ionization/methods , Tandem Mass Spectrometry/methods
15.
J Chromatogr A ; 1661: 462717, 2022 Jan 04.
Article in English | MEDLINE | ID: mdl-34864236

ABSTRACT

Large-scale preparation of target compounds from complex samples is facing great challenges. In the present study, an efficient strategy for large-scale preparation of target compound was proposed and successfully applied in the separation of active components from Toona sinensis. The pretreatment technology of liquid-liquid refining extraction (LLRE) combined with consecutive high-speed counter-current chromatography (HSCCC) was used to process hundred grams of extractions. Firstly, two phase solvent systems composed of n-hexane-ethyl acetate-methanol-water (5:5:5:5, v/v) and (2:5:2:5, v/v) were used to remove low polar and high polar impurities from 100 g crude extracts of T. sinensis, respectively, and 9.25 g of crude sample was obtained. And then, n-hexane-ethyl acetate-methanol-water (2.5:5:2.5:5, v/v) was used as the solvent system for HSCCC separation. The isocratic elution mode with max loading and consecutive injections mode were investigated to obtain more target compound. As a result, ethyl gallate with purity of 97% was successfully separated by 5 times consecutive counter-current chromatography. The separation was repeated once. Finally, ethyl gallate (3.73 g) was isolated from 9.25 g of crude sample (100 g crude extracts). The results demonstrated that the yield increased from 0.26 g/h/L of untreated crude extract to 0.93 g/h/L of LLRE pre-treated sample for single injection, and further increased to 1.62 g/h/L for 5 consecutive injections mode with the present method.


Subject(s)
Countercurrent Distribution , Toona , Chromatography, High Pressure Liquid , Liquid-Liquid Extraction , Methanol , Plant Extracts , Solvents
16.
J Ethnopharmacol ; 285: 114787, 2022 Mar 01.
Article in English | MEDLINE | ID: mdl-34756971

ABSTRACT

ETHNOPHARMACOLOGICAL RELEVANCE: The sclerotium of Lignosusrhinocerus (Cooke) Ryvarden is highly valued for its purported medicinal properties. The decoction and macerated materials prepared from the sclerotium are used for treating cancer and other ailments based on extensive traditional knowledge. Scientific evidence from in vitro cytototoxicity, anti-inflammatory and immunomodulatory analyses showed the effectiveness of sclerotial water extracts but toxicity assessment of such preparations has not been reported. AIM OF THE STUDY: This study aimed to compare the differential toxicity and teratogenicity (if any) of the hot water (HW) and cold water (CW) extracts of both wild and cultivated sclerotium on zebrafish (Danio rerio) embryos. MATERIALS AND METHODS: Zebrafish embryos were treated with varying concentrations of the sclerotial HW and CW extracts (0.3-500 µg/mL) for 72 h until hatching. The hatching, mortality and heartbeat rate of the embryos as well as the potential teratogenic effect of the extracts were assessed in embryos post-treatment with the extracts. RESULTS: While the sclerotial HW extracts were nontoxic (LC50 > 500 µg/mL), the sclerotial CW extracts delayed the hatching of the embryos up to 48 h and showed slight toxicity with LC50 values of 398.4 µg/mL and 428.3 µg/mL for the cultivated and wild sclerotium, respectively. The sclerotial CW extracts also induced minor tachycardia in zebrafish larvae. Phenotypic assessment revealed that, while yolk sac edema was observed at high concentrations (300 and 500 µg/mL) of all extracts, curved trunk and bent tail were only observed in the embryos treated with CW extracts of wild sclerotium (300 and 500 µg/mL) but not for CW extracts of cultivated sclerotium at similar concentrations. CONCLUSION: The sclerotial water extracts of L.rhinocerus prepared using different methods have varying degree of toxicity and teratogenicity in zebrafish embryos with the sclerotial CW extracts showed higher toxicity than the HW extracts.


Subject(s)
Biological Products , Cold Temperature , Hot Temperature , Liquid-Liquid Extraction/methods , Polyporaceae , Water , Abnormalities, Drug-Induced/etiology , Animals , Antineoplastic Agents/chemistry , Antineoplastic Agents/pharmacology , Antineoplastic Agents/toxicity , Biological Products/chemistry , Biological Products/pharmacology , Biological Products/toxicity , Embryo, Nonmammalian/drug effects , Ethnopharmacology/methods , Teratogenesis/drug effects , Teratogens/chemistry , Toxicity Tests , Zebrafish
17.
Acta Chim Slov ; 68(4): 765-772, 2021 Dec 15.
Article in English | MEDLINE | ID: mdl-34918749

ABSTRACT

Phytochemicals in the water extract of Eurycoma longofolia roots were identified using both solid-liquid and liquid-liquid extraction based fractionation techniques. A reversed phase C18 solid phase extraction (SPE) was used as solid-liquid extraction, whereas solvent partition was applied as liquid-liquid extraction. Total saponin was increased after fractionation. A few known quassinoids; eurycomanone, 13a(21)-epoxyeurycomanone, pasakbumin D, 13ß,18-dihydroeurycomanol and 13ß,21-dihydroxyeurycomanol were identified from the 40% and 60% methanol fractions of SPE. Solvent partition extract using ethyl acetate was found to have the highest saponin content compared to butanol and chloroform fractions. Subsequent acetone precipitation of the organic fractions recovered a formylated hexose trimer and other saccharide-containing compounds. Ethyl acetate effectively recovered saponins from E. longofolia water extract using liquid-liquid extraction followed by acetone precipitation.


Subject(s)
Eurycoma/chemistry , Phytochemicals/chemistry , Plant Extracts/chemistry , Chromatography, High Pressure Liquid , Eurycoma/metabolism , Liquid-Liquid Extraction , Phytochemicals/analysis , Phytochemicals/isolation & purification , Plant Extracts/analysis , Plant Extracts/isolation & purification , Plant Roots/chemistry , Plant Roots/metabolism , Quassins/analysis , Quassins/isolation & purification , Solid Phase Extraction , Solvents/chemistry , Tandem Mass Spectrometry , Water/chemistry
18.
J Oleo Sci ; 70(12): 1693-1706, 2021 Dec 03.
Article in English | MEDLINE | ID: mdl-34759110

ABSTRACT

Palm oil is the world's most commonly used vegetable oil and extracted both from fruit and seed of palm tree. However, its high saturated fatty acid content raised controversies over consumption of the oil. Few scientific findings suggest it as a risk factor for cardiovascular disease and increased consumer's awareness over healthy diet raised claim over it. So that, this article aimed to review literatures on palm oil extraction process and its positive and negative health consequences and besides suggest strategies for healthy diet. Literature search of relevant articles was conducted by using Google scholar, PubMed, Web of science, MEDLINE, World Health Organization library online catalogue, UNICEF library, Open access thesis and dissertations published between 2009 and 2021 explored. Study reports recommend that palmitic acid from vegetable source has less effect on blood total cholesterol and low density lipoprotein cholesterol level as compared to palmitic acid from animal source. In contrary tocotrienols of palm oil lowers blood bad cholesterol level by 7-38%. Moreover, palm oil triacylglycerol arrangement does not have a cardiovascular risk and evidences from available in vitro and in vivo studies are not sufficient enough to conclude palm oil as a causative agent for cardiovascular disease. For healthy diet consumers should avoid trans fatty acids, solid and semi solid oils. Finally, further studies recommended on mitigation strategies to minimize process induced toxicants of palm oil to acceptable level.


Subject(s)
Cardiovascular Diseases/etiology , Diet, Healthy , Fatty Acids/adverse effects , Fatty Acids/analysis , Food Handling/methods , Palm Oil/chemistry , Cardiovascular Diseases/prevention & control , Cholesterol/blood , Cholesterol, LDL/blood , Consumer Behavior , Humans , Liquid-Liquid Extraction/methods , Palmitic Acids/pharmacology , Risk Factors , Trans Fatty Acids/adverse effects
19.
J Oleo Sci ; 70(11): 1575-1583, 2021 Nov 03.
Article in English | MEDLINE | ID: mdl-34645745

ABSTRACT

Physicochemical properties and chemical composition of Chinese perilla seed oil has been characterized in this study. The result showed that both the cold press oil and the solvent extracted oil possessed low acid value and peroxide value. The fatty acid composition result showed that the oil has high content of linolenic acid (C18:3) up to 66.4 g/100 g, followed by linoleic acid (C18:2) of 15.3 g/100 g. The total triacylglycerol (TAG) profiles results showed that the oil contained 20 TAGs including 17 regioisomers, including LnLnLn (35.8 g/100 g), LLnLn (20.2 g/100 g), LLLn (17.7 g/100 g) and PLnLn (14.9 g/100 g) (Ln, linolenic acid; L, linoleic acid; P, palmitic acid). With content of only 0.57 g/100 g oil, the unsaponifiable matters were mainly composed of phytosterols, squalene, tocopherol, alcohols and hydrocarbons. The total phytosterols content was 0.39 g/100 g oil, in which ß-sitosterol has high content of 0.31 g/100 g oil.


Subject(s)
Chemical Phenomena , Linoleic Acid/analysis , Perilla frutescens/chemistry , Phytosterols/analysis , alpha-Linolenic Acid/analysis , Alcohols/analysis , Antioxidants/analysis , Hydrocarbons/analysis , Isomerism , Liquid-Liquid Extraction/methods , Palmitic Acid/analysis , Plant Oils/chemistry , Plant Oils/isolation & purification , Squalene/analysis , Tocopherols/analysis , Triglycerides/analysis , alpha-Linolenic Acid/chemistry , alpha-Linolenic Acid/isolation & purification
20.
Sci Rep ; 11(1): 19027, 2021 09 24.
Article in English | MEDLINE | ID: mdl-34561493

ABSTRACT

In the present study, and for the waste valorization, Moringa oleifera seeds-removed ripened pods (SRRP) were used for papersheet production and for the extraction of bioactive compounds. Fibers were characterized by SEM-EDX patterns, while the phytoconstituents in ethanol extract was analyzed by HPLC. The inhibition percentage of fungal mycelial growth (IFMG) of the treated Melia azedarach wood with M. oleifera SRRP extract at the concentrations of 10,000, 20,000, and 30,000 µg/mL against the growth of Rhizoctonia solani and Fusarium culmorum was calculated and compared with fluconazole (25 µg). The produced papersheet was treated with the ethanol extract (4000, 2000, and 1000 µg/mL) and assayed for its antibacterial activity against Agrobacterium tumefaciens, Erwinia amylovora, and Pectobacterium atrosepticum by measuring the inhibition zones and minimum inhibitory concentrations (MICs). According to chemical analysis of M. oleifera SRRP, benzene:alcohol extractives, holocellulose, lignin, and ash contents were 7.56, 64.94, 25.66 and 1.53%, respectively, while for the produced unbleached pulp, the screen pulp yield and the Kappa number were 39% and 25, respectively. The produced papersheet showed tensile index, tear index, burst index, and double fold number values of 58.8 N m/g, 3.38 mN m2/g, 3.86 kPa m2/g, and 10.66, respectively. SEM examination showed that the average fiber diameter was 16.39 µm, and the mass average of for elemental composition of C and O by EDX were, 44.21%, and 55.79%, respectively. The main phytoconstituents in the extract (mg/100 g extract) by HPLC were vanillic acid (5053.49), benzoic acid (262.98), naringenin (133.02), chlorogenic acid (66.16), and myricetin (56.27). After 14 days of incubation, M. oleifera SRRP extract-wood treated showed good IFMG against R. solani (36.88%) and F. culmorum (51.66%) compared to fluconazole, where it observed 42.96% and 53.70%, respectively. Moderate to significant antibacterial activity was found, where the minimum inhibitory concentration (MIC) values were 500, 650, and 250 µg/mL against the growth of A. tumefaciens, E. amylovora, and P. atrosepticum respectively, which were lower than the positive control used (Tobramycin 10 µg/disc). In conclusion, M. oleifera SRRP showed promising properties as a raw material for pulp and paper production as well as for the extraction of bioactive compounds.


Subject(s)
Chromatography, High Pressure Liquid/methods , Liquid-Liquid Extraction/methods , Moringa oleifera/chemistry , Paper , Plant Extracts/chemistry , Plant Extracts/pharmacology , Agrobacterium tumefaciens/drug effects , Benzoic Acid , Drug Resistance, Microbial , Erwinia amylovora/drug effects , Flavanones , Fusarium/drug effects , Plant Extracts/isolation & purification , Rhizoctonia/drug effects , Seeds , Vanillic Acid
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