Cinnarizine is a weak base, which can produce supersaturation and precipitation during gastrointestinal transit, affecting its absorption in vivo. Therefore, it is necessary to investigate whether ...the oral bioavailability of cinnarizine can be improved after co‐administration with precipitation inhibitors or not. In order to evaluate the pharmacokinetic behavior of cinnarizine in rats, a simple, rapid, sensitive, and environmentally friendly supercritical fluid chromatography‐tandem mass spectrometric method was established and validated. In this method, flunarizine, a structural analogue of cinnarizine, was selected as the internal standard, and cinnarizine was extracted from rat plasma using evaporation‐free liquid–liquid extraction method. The analytes were separated on a Torus 1‐AA column (3.0 mm × 100 mm, 1.7 μm) within 2.0 min, using a gradient elution procedure. The transitions of cinnarizine and flunarizine were m/z 369.1 → 167.1 and m/z 405.1 → 203.1, respectively. Cinnarizine showed good linear correlation in the range of 1–500 ng/ml with a lower limit of quantification of 1 ng/ml. The intra‐ and interday precision and accuracy of all quality control samples were within ±15%. This high‐throughput, accurate, sensitive, and reproducible method has been successfully applied to study the effects of the precipitation inhibitor cinnarizine on the pharmacokinetics in rats.
In this study, 63 compounds measured as 10 individual mixtures containing in each case an active pharmaceutical ingredient and its relevant impurities, and additional set of 7 basic beta blockers ...were analyzed using ultra-high performance supercritical fluid chromatography with UV and mass spectrometry detection. The separations were accomplished using 8 different stationary phases (diol, diethylamine, 2-picolylamine, 1-aminoanthracene, BEH 2-ethylpyridine, BEH, CSH pentafluorophenyl, and HSS C18 SB), 6 modifiers (methanol, ethanol, isopropanol, methanol/acetonitrile, methanol/ethanol, ethanol/acetonitrile) and 5 additives in methanol (0.1% formic acid, 10 mmol/L ammonium formate, 10 mmol/L ammonium acetate, 0.4% ammonium hydroxide, and 2% water).
The resulting chromatograms were evaluated using 6 selected parameters: number of eluted peaks, number of separated peaks, resolution between active pharmaceutical ingredient and following impurity, peak symmetry, peak width at 50% of the peak height, and selectivity. Volatile additives such as ammonium formate, ammonium acetate, and especially ammonium hydroxide provided overall generic approach with very good chromatographic performance. Combined modifier methanol/acetonitrile (1:1) was important for separations of some critical pairs in case of neutral compounds. Diol stationary phase proved its suitability for wide range of applications when the separations of all mixtures were satisfactory on this column, except for vardenafil and beta blockers mixture. HSS C18 SB stationary phase offered unique complementary selectivity especially for analysis of structurally close compounds and/or isomers.
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•UHPSFC screening was carried out with 10 real quality control mixtures.•Eight stationary phases were tested using 6 modifiers and 5 additives in methanol.•Evaluating approach consisting of 6 parameters was developed and applied.•Recommendations for generic screening approach in UHPSFC were defined.
Introduction
The consumption of health‐promoting products such as oil seeds may improve human health and prevent certain diseases. Carvi seeds have the potential to produce oil with nutritional and ...functional properties rich in active compounds.
Objective
To extract bioactive lipids from Carum carvi seeds using green methodologies.
Material and methods
Supercritical‐carbon dioxide (Sc‐CO2) and ethanol as co‐solvent and bio‐based solvent 2‐methyltetrahydrofuran (MeTHF) were used to extract the oil from Carum carvi. The yield, the chemical composition, as well as antioxidant and anti‐inflammatory activities of green extracted oils were investigated and compared to those obtained with conventional methods (hexane and Folch system).
Results
MeTHF extraction gave higher oil yield than that obtained by hexane. Fatty acids composition of the two obtained green extracted oils was similar to conventional extracted ones where petroselinic (39–43%), linoleic (29–31%) and oleic (19–21%) acids were the major compounds. Furthermore, MeTHF and Sc‐CO2 green extracted oils were enriched of bioactive compounds including sterols (5.4 and 7.3 mg/g oil) and total polyphenols (9.3 and 7.6 mg GAE/g oil) which were correlated to enhanced antiradical capacity. Moreover, the green extracted oils exhibited high anti‐inflammatory capacity inhibiting nitric oxide (NO) release in lipopolysaccharide (LPS)‐induced RAW 264.7 macrophages with IC50 values of 28 and 24 μg/mL.
Conclusion
Green solvents are a good alternative to petroleum solvents to recover oil from carvi seeds with high amount of nutritionally important fatty acids, along with significant antioxidant and anti‐inflammatory potential.
This study showed that supercritical CO2 and bio‐based solvent 2‐methyltetrahydrofuran (MeTHF) are green alternative for lipid extraction from carvi seeds. Green extracted oils are a source of sterols and polyphenols and exhibited enhanced antioxidant and anti‐inflammatory activities.
This contribution proposes an enzyme-assisted eco-friendly process for the extraction of non-extractable polyphenols (NEPPs) from black tea leftover (BTLO), an underutilized tea waste. BTLO ...hydrolyzed with various enzyme formulations was extracted using supercritical carbon dioxide and ethanol as co-solvent (SC-CO
2
+ EtOH). A conventional solvent extraction (CSE) was performed using EtOH + H
2
O (80:20,
v
/
v
) for comparison purposes. The results revealed that hydrolysis of BTLO with 2.9% (
w
/
w
) kemzyme at 45 °C and pH 5.4 for 98 min improved the liberation of NEPPs offering 5-fold higher extract yield (g/100 g) as compared with non-treated BTLO. In vitro antioxidant evaluation and LC-MS characterization of extracts revealed the presence of phenolic acids (mainly caffeic and
para
-coumaric acid) of high antioxidant value. Scanning electron micrograph of the hydrolyzed BTLO samples indicated noteworthy changes in the ultrastructure of BTLO. Moreover, polyphenol extracts obtained by SC-CO
2
+ EtOH extraction were found to be cleaner and richer in polyphenols as compared to CSE. The devised enzyme-assisted SC-CO
2
+ EtOH extraction process in the present work can be explored as an effective biotechnological mean for the optimal recovery of antioxidant polyphenols.
Graphical abstract
Enzymatic pretreatment can effectively liberate non-extractable polyphenols (NEPPs) while hydrolyzing the cellulosic and hemicellulosic framework of black tea left overs (BTLO)
The activities linked to the fishing sector generate substantial quantities of by-products, which are often discarded or used as low-value ingredients in animal feed. However, these marine ...by-products are a prominent potential good source of bioactive compounds, with important functional properties that can be isolated or up-concentrated, giving them an added value in higher end markets, as for instance nutraceuticals and cosmetics. This valorization of fish by-products has been boosted by the increasing awareness of consumers regarding the relationship between diet and health, demanding new fish products with enhanced nutritional and functional properties. To obtain fish by-product-derived biocompounds with good, functional and acceptable organoleptic properties, the selection of appropriate extraction methods for each bioactive ingredient is of the outmost importance. In this regard, over the last years, innovative alternative technologies of intensification, such as ultrasound-assisted extraction (UAE) and supercritical fluid extraction (SFE), have become an alternative to the conventional methods in the isolation of valuable compounds from fish and shellfish by-products. Innovative green technologies present great advantages to traditional methods, preserving and even enhancing the quality and the extraction efficiency, as well as minimizing functional properties' losses of the bioactive compounds extracted from marine by-products. Besides their biological activities, bioactive compounds obtained by innovative alternative technologies can enhance several technological properties of food matrices, enabling their use as ingredients in novel foods. This review is focusing on analyzing the principles and the use of UAE and SFE as emerging technologies to valorize seafoods and their by-products.
A comparative study of chiral separation of pantoprazole and rabeprazole is carried out using supercritical fluid chromatography and high‐performance liquid chromatography. The columns used were ...Chiralpak IA and Chiralpak IE. The best mobile phase in supercritical fluid chromatography was carbon dioxide‐0.2% triethylamine in methanol (60:40) and 0.1% triethylamine in n‐hexane‐ethanol (50:50) in high‐performance liquid chromatography. For supercritical fluid chromatography, values of the retention factor of pantoprazole enantiomers were 3.97 and 4.88. These values for rabeprazole enantiomers were 6.10 and 7.52. The values of separation and resolution factor for pantoprazole and rabeprazole were 1.23 and 1.23 and 2.20 and 3.36, respectively. Similarly, for high‐performance liquid chromatography, the values of retention factor for enantiomers of pantoprazole were 4.02 and 7.32. These values for rabeprazole enantiomers were 5.32 and 7.88, respectively. The values of separation and resolution factor for pantoprazole and rabeprazole were 1.82 and 1.48 and 9.22 and 6.58, respectively. A comparison was carried out, which confirmed supercritical fluid chromatography as the best method due to its fastness, eco‐friendly, and inexpensiveness. The reported methods are effective, efficient, and reproducible and may be used to separate and identify pantoprazole and rabeprazole in any unknown samples.
Extraction with environmentally friendly solvents Płotka-Wasylka, Justyna; Rutkowska, Małgorzata; Owczarek, Katarzyna ...
TrAC, Trends in analytical chemistry (Regular ed.),
June 2017, 2017-06-00, Letnik:
91
Journal Article
Recenzirano
The ever-increasing demand for determining compounds at low concentration levels in complex matrices requires a preliminary step of analytes isolation/enrichment in order to employ a detection ...technique characterized by high sensitivity at low LOQ. Sample preparation is considered as crucial part of analytical procedures. Previously the parameter of “greenness” is as important as selectivity in order to avoid using harmful organic solvents in sustainable extraction techniques. These solvents can generate hazardous, toxic waste while consuming large resources volume. Developing new green solvents is one of the key subjects in Green Chemistry in order to reduce the intensity of anthropogenic activities related to analytical laboratories. A lot of new, more eco-friendly media have been employed as extractant phases. These media, besides of being more eco-friendly, provide shorter extraction times, simplicity, low cost, better selectivity in some cases. The most promising, most widely used green extraction solvents are described in this review.
•Replacement of VOCs by eco-friendly solvents is becoming increasingly important.•Several new solvents have been developed and introduced in analytical practice.•Solvents environmental impact assessment is becoming increasingly important.•Analytical chemistry requires solvents “greenness” assessment systems to be comprehensive.
Chiral separation of β‐blockers is performed by utilizing the supercritical fluid chromatographic method. The chiral columns utilized were Chiralpak IG and Chiralpak IBN‐5. The finest mobile phase ...was CO2 −0.2% TEA in methanol (60:40). The values atenolol enantiomers retention factors were 6.39 and 8.98. These values for propranolol enantiomers were 3.39 and 4.06. These values for betaxolol enantiomers were 4.08 and 4.68. The separation and resolution factor values for atenolol, propranolol, and betaxolol were 1.41 and 3.33, 1.19 and 2.23, and 1.15 and 1.87, separately and respectively. By comparison, it was observed that Chiralpak IG column is better than Chiralpak IBN‐5 column. Supercritical fluid chromatography has been found as the best analytical technique due to its high speed, being eco‐friendly, and being economic. The various most probable interactions responsible for the chiral resolution are hydrogen bonding, dipole–dipole interactions, steric effect, and π–π interactions. The reported methods are effective, efficient, and reproducible and may be used to separate and identify atenolol, propranolol, and betaxolol in any unknown samples.
► SFE is an advantageous process for obtaining oil from freeze-dried, low fat, fish by-products. ► SFE can prevent lipid oxidation and reduce extraction of certain pollutants. ► Closed circulation ...SFE may provide extracts with high volatile content. ► On-line fractionation SFE can provide enhanced quality fish oil with low FFA and oxidation products content.
Fish and fish by-products are the main natural source of omega-3 polyunsaturated fatty acids, especially EPA (eicosapentaenoic acid) and DHA (docosahexaenoic acid), both of them with a great importance in the food and pharmaceutical industries. Comparing to conventional fish oil extraction processes such as cold extraction, wet reduction or enzymatic extraction, supercritical fluid extraction with carbon dioxide under moderate conditions (25MPa and 313K) may be useful for reducing fish oil oxidation, especially when fish oil is rich in omega-3 such as salmon oil, and the amount of certain impurities, such as some species of arsenic. Furthermore, taking profit of the advantages of supercritical carbon dioxide as extractive solvent, a coupled extraction-fractionation process is proposed as a way to remove free fatty acids and improve fish oil quality, alternatively to physical and chemical refining procedures.
Sustainable solvents are a topic of growing interest in both the research community and the chemical industry due to a growing awareness of the impact of solvents on pollution, energy usage, and ...contributions to air quality and climate change. Solvent losses represent a major portion of organic pollution, and solvent removal represents a large proportion of process energy consumption. To counter these issues, a range of greener or more sustainable solvents have been proposed and developed over the past three decades. Much of the focus has been on the environmental credentials of the solvent itself, although how a substance is deployed is as important to sustainability as what it is made from. In this Review, we consider several aspects of the most prominent sustainable organic solvents in use today, ionic liquids, deep eutectic solvents, supercritical fluids, switchable solvents, liquid polymers, and renewable solvents. We examine not only the performance of each class of solvent within the context of the reactions or extractions for which it is employed, but also give consideration to the wider context of the process and system within which the solvent is deployed. A wide range of technical, economic, and environmental factors are considered, giving a more complete picture of the current status of sustainable solvent research and development.
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