Good Extraction Yield Research Articles

Insight into the influence of natural deep eutectic solvents on the extraction of phenolic compounds from poplar type propolis: Composition and in vitro biological activity

Natural deep eutectic solvents (NADESs) have been considered promising to replace traditional volatile and toxic organic solvents for the extraction of biologically active substances from natural sources. This work applied an efficient and ethanol-exclusion strategy for extraction of phenolic compounds from poplar type propolis using five known NADESs (lactic acid:1,2-propanediol 1:1, lactic acid:fructose 5:1, choline chloride:1,2-propanediol 1:3, choline chloride:1,2-propanediol:water 1:1:1 and betaine:malic acid:water 1:1:6). The selected NADESs' extractability was evaluated by measuring the concentrations of total phenolics and total flavones and flavonols in the propolis extracts obtained, which qualitative chemical composition was further determined in detail by gas chromatography-mass spectrometry (GC-MS) analysis. It demonstrated that the chemical profiles of NADES and 70% ethanolic propolis extracts are similar. To expand the knowledge about the role of the applied solvents in the poplar propolis extraction process, the in vitro antimicrobial, cytotoxic and genotoxic activity of both NADESs and liquid NADES extracts were evaluated. The results revealed that the use of the selected NADESs as an extraction media for phenolic compounds from poplar propolis not only delivered a good extraction yield in some cases, but generally led to the preservation of propolis extracts' biological activity and even to the enhancement of their antimicrobial effect in comparison with the hydroethanolic one. Besides, the tested NADESs except for lactic acid:fructose and betaine:malic acid:water exerted low to negligible toxicity against normal cells treated and apart from lactic acid:fructose the remaining solvents demonstrated concentration-dependent moderate to subtle genotoxicity. There is a probability that not the supramolecular structure of the NADESs, but their components, played a key role for the observed biological effects. The present study has demonstrated an alternative approach for extracting the biologically active complex from poplar type propolis using NADESs, which could be useful for further pharmaceutical and cosmeceutical applications.

Oil and protein extraction from fruit seed and kernel by-products using a one pot enzymatic-assisted mild extraction.

This research evaluated the application of a one-pot enzymatic extraction by using a protease for the concomitant and sustainable extraction of oils and proteins from fruit seeds/kernels of different species of stone, citrus and exotic fruits. The proteolysis improved the oil solvent-extractability of seeds/kernels of some fruit species compared to the use of acid and/or organic solvents and led to directly recover fat (10-33%) from mango, lemon and pumpkin seeds. Good protein extraction yields were obtained compared to conventional solvent extractions and with a good hydrolysis degree (almost 10%) in the case of lemon and pumpkin seed protein hydrolysates. The nutritional quality of all the protein hydrolysates was quite low, because of their limiting amino acids (histidine, methionine and lysine). On the contrary, the fruit seed/kernel oils resulted with high nutritional value, as they were mostly rich in unsaturated fatty acids, primarily oleic acid (>25%) and linoleic acid (till 40%).

Development of a new online SPE-HPLC-MS/MS method for the profiling and quantification of sphingolipids and phospholipids in red blood cells – Application to the study of Gaucher's disease

Red blood cells (RBCs) are the subject of clinical attention due to their biological importance. Recently, it has been shown that certain erythrocyte pathologies could be linked to an abnormal lipid composition. In this work, we have developed a simple and fast method using online sample preparation with liquid chromatography coupled to mass spectrometry (SPE-HPLC-MS/MS), to identify a large number of sphingolipids (SL) and phospholipids (PL). The use of online sample preparation considerably reduces analysis times (15 min including extraction and separation of lipids + 2 min for system re-equilibration) and facilitates experimentation while ensuring very good extraction yields. This method was then successfully applied to the quantification of 30 sphingolipids and phospholipids in plasma and erythrocyte extracts from a cohort of individuals with Gaucher disease, treated or not by enzymotherapy. Our results for the study of this disease, led us to establish the lipid profile of the healthy red blood cells, still not very well-known to date. For this, we adopted a semi-targeted approach, based on the use of a triple-quadrupole analyzer and identified more than two hundred different lipid species. These promising results will hopefully enable us to enrich our knowledge of the normal red blood cells lipidome.

Purification of synthetic oils using liquefied gases of reduced flammability

In this work we evaluate the technical feasibility of using liquefied CO2 + propane as a solvent for the purification of lubricant oils. A model lubricant made of a silicone oil (polydimethylsiloxane, MW ≈6000) and Decamethylcyclopentasiloxane (D5, MW: ≈371) is prepared to study the extraction process. The phase behavior of the CO2 +propane+silicone oil system is evaluated in a high-pressure view cell to set the window of operating conditions where the system exhibits partial liquid miscibility (298–323 K). Then, we add D5 monomer (2 mass % in the silicone oil) to the previous ternary mixture, and we assess the effect of solvent composition (CO2/propane: 60/40–90/10) over the fractionation process by means of new equilibrium measurements. The solvent-free distribution coefficient of D5 between the liquid phases is determined from experimental determinations. Results evidence that liquefied gases with propane concentrations between 10 and 26 mass % are suitable to remove the monomers from the raw lubricant oils with good selectivity and extraction yields. Conceptual engineering designs of the liquid-liquid fractionation process are performed to determine the suitable solvent composition that completely removes the monomer present in the lubricant oil and to assess the recovery of the lubricant oil.

HPLC Determination of Biperiden in Solid Dosage Forms

A rapid, new analytical method, based on liquid chromatography with UV detection, has been developed and utilised for the determination of biperiden hydrochloride in solid dosage forms. The chromatographic separation was performed on a conventional C18 reversed phase column with a mobile phase composed of acetonitrile-buffer mixture. Ultraviolet detection was carried out at 205 nm. A rapid extraction procedure using ultrasonic bath obtained good extraction yield values for the analyte (≥ 98.4%). The method was developed specifically for routine analysis of biperiden in solid dosage forms in the applicable concentration range. The linearity and range of the method investigated for the assay of biperiden is between 2–6 μg mL−1. The method is selective and sufficiently precise. Thus, the method developed is suitable for routine analysis of biperiden.

Protease-Assisted Mild Extraction of Soluble Fibre and Protein from Fruit By-Products: A Biorefinery Perspective.

By-products from the fruit supply chain, especially seeds/kernels, have shown great potential to be valorised, due to their high content of macronutrients, such as lipids, protein, and fibre. A mild enzymatic assisted extraction (EAE) involving the use of a protease was tested to evaluate the feasibility of a cascade approach to fractionate the main fruit by-products components. Protease from Bacillus licheniformis (the enzyme used in the AOAC 991.43 official method for dietary fibre quantification) was used, and besides protein, the conditions of hydrolysis (60 °C, neutral pH, overnight) allowed us to dissolve a portion of soluble fibres, which was then separated from the solubilized peptide fraction through ethanol precipitation. Good protein extraction yields, in the range 35-93%, were obtained. The soluble fibre extraction yield ranged from 1.6% to 71% depending on the by-product, suggesting its applicability only for certain substrates, and it was found to be negatively correlated with the molecular weight of the fibre. The monosaccharide composition of the soluble fibres extracted was also diverse. Galacturonic acid was present in a low amount, indicating that pectin was not efficiently extracted. However, a predominance of arabinose and galactose monomers was detected in many fractions, indicating the isolation of a fruit soluble fibre portion with potential similarity with arabinogalactans and gum arabic, opening up perspectives for technological applications. The residual solid pellet obtained after protease assisted extraction was found to be an excellent fibre-rich substrate, suitable for being subjected to more "hard" processing (e.g., sequential pectin and hemicellulose extraction) with the objective to derive other fractions with potential great added economic value.

A simple and easy non-derivatization gas chromatography-mass spectrometry method for simultaneous quantification of valproic acid, gabapentin, pregabalin, and vigabatrin in human plasma.

Immunoassays are currently not available in commercial kits for the quantification of valproic acid, vigabatrin, pregabalin, and gabapentin, which also cannot suffer the limitations of interferences of substances with similar structures. Chromatography is a good alternative to immunoassay. In this study, a simple and robust non-derivatization gas chromatography-mass spectrometry method for simultaneous determination of the above four drugs in human plasma was developed and validated for therapeutic drug monitoring purposes. This method employed benzoic acid as the internal standard with hydrochloric acid for plasma acidification and ACN for precipitate protein. The supernatant was directly injected into gas chromatography-mass spectrometry for analysis. Good linearity was obtained with linear correlation coefficients of the four analytes of 0.9988-0.9996. Extraction recoveries of valproic acid, vigabatrin, pregabalin, and gabapentin were respectively in the ranges of 91.3%-94.5%, 90.0%-90.9%, 90.0%-92.1%, and 88.0%-92.2% with the relative standard deviation values less than 12.6%. Intra- and inter-batch precision and accuracy, and stability assays were all acceptable. Taken together, the novel method developed in this study provided easy plasma pretreatment, good extraction yield, and high chromatographic resolution, which has been successfully validated through the quantification of valproic acid in the plasma of 46 patients with epilepsy.

A Validated Method for the Determination of Carnosic Acid and Carnosol in the Fresh Foliage of Salvia rosmarinus and Salvia officinalis from Greece

In the framework of a project aiming at identifying genotypes of Greek rosemary and sage producing high amounts of carnosic acid, an HPLC-PDA method was developed for the determination of the main antioxidant in the fresh leaves. To this end, an effective and repeatable extraction process of the labile diterpene was developed to ensure a good extraction yield. A fast RP-HPLC protocol was developed and optimized to allow for a short and reliable analysis of the unstable target constituent. The HPLC-PDA method was validated for precision and accuracy according to ICH guidelines. Finally, the overall method was validated for precision and accuracy at three concentration levels. The precision was acceptable with % RSD values ranging between 1.42 and 4.35. The recovery ranged between 85.1% and 104.6% with RSD values < 5%, within the acceptable limits. The developed assay was fast and simple and allowed for the fast and accurate determination of carnosic acid and carnosol in the fresh herbs. The methodology was applied to the quantitative analysis of several cultivated samples of S. rosmarinus and S. officinalis, and some of them were revealed to be promising starting materials for the development of Greek genotypes rich in carnosic acid.

A Non-aqueous Capillary Electrophoresis for Determination of Eugenol in Cloves and Dental Preparations

A total non-aqueous capillary electrophoresis method was developed and applied for the first time for the quantification of eugenol in cloves and dental preparations. The optimized conditions included a buffer consisting of 150 mM sodium acetate and 300 μL 1 M acetic acid methanol solution (30 mM), an applied voltage of 25 kV, and a temperature of 25 °C and an applied wavelength of 214 nm. The developed method of determining the eugenol was characterized by the following parameters: a detection time within 1.97 min, good linearity (R2 = 0.9989–0.9999), detection limit at the level from 0.19 to 0.35 µg mL−1, very good extraction yield of 99.6–100.6% from both methanol standard solutions, clove buds’ matrix, and dental preparations. Limit of quantitation at the level from 0.81 to 0.98 µg mL−1. The method is based on the developed one-step extraction procedure. Moreover, the developed method does not require the use of any eugenol solubility enhancers such as SDS.

Micro sampling, a new trend in toxicological screening?

Develop and validate a toxicological screening by High Resolution mass spectrometry (HR/MS) on whole blood taken from MITRA®, a volumetric micro-sampling system (VAMS). In both clinical and forensic toxicology, screening remains an essential element in the management of the patient and the search for the cause of death. Performed on urine and/or plasma, it uses chromatographic methods coupled with different detection systems such as HR/MS. The reduction in sample volumes and the grouping of analyses in specialized laboratories explain the search for new analytical approaches to develop toxicological screening on alternative matrices such as VAMS. Six whole blood solutions were overloaded with 85 licit and illicit drugs to optimize the pre-analytical phase and to determine the detection limits (LD) of drugs. Twenty microliters of each solution are sampled to MITRA® (Neoteryx). After drying 24 hours at room temperature, MITRA® elution is carried out in 500 μL of a solvent mixture by stirring and sonication. After evaporation, the dry extracts were taken up by 50 μL of solvents and 10 μL injected into the chromatographic system (Vanquish® LC) coupled to a QExactive Focus® mass spectrometer equipped with an electrospray ionization. The identification of the compounds is carried out from the TraceFinder® 4.0 software (ThermoFisher Scientific) compared to our library including 1500 referenced compounds. To study the feasibility in clinic, we sampled at the same time, 20 μL of plasma, whole blood and MITRA® fingertip blood to perform screenings in ten patients hospitalized in Toxicological Critical Care for acute poisonings. Our extraction protocol coupled with HR screening has among detect/identify 76 compounds out of the 85 present in overloaded solutions. Cannabis derivatives are not detected and barbiturates are poorly (LD = 250 ng/mL). For other compounds, detection limits are less than 25 ng/ml for opiates, 12.5 ng/mL for amphetamines and benzodiazepines, 2.5 ng/mL for tramadol, mephedrone and benzoylecgonine, 1.25 ng/mL for norfentanyl. In ten poisonned patients, screenings performed on plasma, whole blood and MITRA®, show similar résults. Analogy of detection corresponding to 100% for whole blood compared to plasma, and 98% for MITRA® compared to whole blood. In MITRA®, ethylglucuronide was detected but not identified in two patients. MITRA® extraction yields/whole blood ranged from 80.6 to 108.7% for licit and illicit drugs and their metabolites. Our study reports an excellent concordance (R2 = 0.9997) between the areas of the molecules obtained on 20 μL MITRA® and those obtained from 20 μL whole blood sample. We report for the first time an original method of toxicological screening on VAMS. Our pre-analytical phase is still long but allows us to extract 90% of the molecules present in the overloaded solutions. In MITRA®, the detection/identification of molecules is similar to that on whole blood with very good extraction yields and satisfactory detection limits for the majority of the compounds tested. The lack of sensitivity for some compounds, as cannabis derivatives and barbiturates, is not related to the sampling on MITRA® but to the poor detection of acidic compounds in our HR/MS method. The excellent concordance in patients between whole blood and MITRA® samples shows a comparable distribution of substances between capillary and peripheral streams. This study confirms the major interest of VAMS in toxicology fields, opening up new perceptives, in paediatrics or in addictology by fingertip sampling, in forensics with the possibility of working on very small volumes, such as bloodstains, to carry out mass screening during events, to monitor environmental epidemiology and occupational health studies or to exchange samples due to MITRA® samples stability and their easy transport by post.

Multiobjective decision making strategy for selective albumin extraction from a rapeseed cold-pressed meal based on Rough Set approach

This article proposes the application of multiobjective decision making strategy for selective albumin extraction by Pareto’s domain determination and ranking by Decision Engineering tool based on the Rough Set approach. In this study, both competing process performance indicators of rapeseed albumin extraction and quality of the solid residue remaining from this process were considered for an overall valorization of the rapeseed cold-pressed meal. The impact of extraction pH and NaCl concentration on three process performance indicators including the albumin extraction yield, the albumin content in the extract, and the phytic acid content in the remaining solid residue was studied. The results of the optimization approach showed that the high selectivity of rapeseed albumin extraction was to the detriment of the productivity of the process and the quality of the solid residue. The optimal conditions for selective rapeseed albumin extraction while producing a high-quality solid residue were identified at pH 2.0 and 0.11molL−1 of NaCl concentration. Upon these conditions, good albumin extraction yield was achieved (55.5%) with a high selectivity (97.9% of albumins in the extract). The isolate obtained after purification exhibited suitable color, high solubility, promising emulsifying properties and good foaming properties, which is of interest for food applications. Besides, the identifying extraction conditions yielded a protein-rich solid residue (35.6% on dry matter basis) with reduced phytic acid content (3.6% on dry matter basis), which can be used for feed applications.

Phytochemical Analysis and Evaluation of Bioactivities of Cola acuminata Extracts

Background: From centuries of evolution, knowledge and technological progress for mankind to one day rediscover nature. Currently, the control of bacterial infections is becoming complex due to the concern of antibiotic resistance, which has been a significant global health problem. The aim was to determine and compare phytochemical constituents and in the in vitro evaluation of antimicrobial and antioxidant activities of aqueous, methanol, acetate, dichloromethane extracts from Cola acuminata nuts grown in the Nord Ubangi Province, DRC. Methods: The nuts of Cola acuminata were harvested in April 2016 at Yakoma city, Nord-Ubangi, DRC. The microscopic features of this species were performed in order to identify specific histological structures. Three bacterial strains notably Staphylococcus aureus ATCC 25923, Escherichia coli ATCC 8739 and Pseudomonas aeroginosa ATCC 9027 were used for the assessment of the antibacterial activity. The qualitative and quantitative phytochemical screening were used for compound identification using different fractions and fractions which presented a good extraction yield was used for further analysis. The antioxidant activity was evaluated using ABTS and DPPH scavenging tests while the antibacterial activity was performed using the diffusion method. Findings: The micrography of C. acuminata revealed the presence of following histological elements of which: fibers, spiral vessels, trichomes, ovoid starch grains, sclerenchyma and the fragments of endosperm. Only the methanol and aqueous extracts presented a good extraction yield. The phytochemistry shows the presence of flavonoids, anthocyanins, terpenes, iridoids and tannins. All fractions showed IC50 values lower than 10 µg/mL in the ABTS test and lower than 100 µg/mL in the DPPH test. The antibacterial activity of this plant was low against the three strains used. Conclusion: Seeing the potency of C. acuminata and different biological activities displayed, further analysis are required in order to identify and purify the active ingredients, to study the toxicity of cell lines in vitro, to perform the in vivo experiments and to test for other activities such as the anti-hypoglycemic and anti-inflammatory.

Extraction of curcumin from Curcuma longa using meglumine and pyroglutamic acid, respectively, as solubilizer and hydrotrope

In preceding papers, it could be shown that mixtures of water, ethanol, and triacetin can significantly boost the extraction of curcuminoids out of Curcuma longa, compared to the usually applied water–ethanol mixtures. To further improve it, additives can be beneficial. We show that meglumine and pyroglutamic acid are among the most promising of these additives. First, the influence of meglumine and pyroglutamic acid on the phase diagram of ternary mixtures consisting of water, ethanol and triacetin has been investigated: the addition of meglumine to the water phase only slightly increases the miscibility gap, whereas pyroglutamic acid increases it significantly in the oil-rich region. The solubility of curcumin could be significantly enhanced through the addition of meglumine. Extractions were successfully conducted extracting ~ 18 mg of curcuminoids per g Curcuma longa by adding 15 wt% of meglumine to the amount of water in the extraction mixtures consisting of water, ethanol and triacetin, which is an increase of ~ 20% compared to the best extraction mixture water/ethanol/triacetin from the previous study. A simple water/meglumine extraction was also investigated. Around 13 mg curcuminoids per g Curcuma longa could be extracted. Bisdemethoxycurcumin contributes 3.46 mg to the total amount, which is a very good extraction yield (increase of 19% compared to the best extraction mixture from the previous study). The purity of the extract reached 87% just by extracting with water and meglumine. For comparison, the same purity was achieved using the ternary water/ethanol/triacetin system, but only after freeze drying of the rhizomes before extraction.

Mechanical Processing of Hermetia illucens Larvae and Bombyx mori Pupae Produces Oils with Antimicrobial Activity.

Simple SummaryInsect rearing and processing are widely studied to provide solutions to the increasing demand for proteins caused by a growing human population. It has been demonstrated that insect meal can be introduced into the feed ratio of livestock and its exploitation can limit the environmental impact of animal husbandry. When their ecological footprint is analyzed, insects are considered “biorefineries” able to generate multiple economic outputs for the food industry. Fat and antimicrobial peptides contained in the insect oil can represent important resources to treat animal diseases, e.g., allowing to reduce antibiotic overuse. In this paper we focused on two insects exploitable both for protein and oil production: the black soldier fly larvae (BSFL) and the domestic silkworm. As the diet regimen remarkably affects the fat composition of the insects, both BSFL and silkworm larvae were reared on plant-based diets. Silkworms were fed mulberry leaves, while BSFL were reared on a diet composed of leftover vegetables and fruit, in the perspective of their bioconversion and valorization. The best technique to maximize the oil extraction yield was defined for BSFL and applied to the silkworm pupae. An antimicrobial activity of the oil against some bacterial species was demonstrated in both insects and compared.The aim of this work was to develop processing methods that safeguard the quality and antimicrobial properties of H. illucens and B. mori oils. We adopted a vegetable diet for both insects: leftover vegetables and fruit for H. illucens and mulberry leaves for B. mori. First, alternative techniques to obtain a good oil extraction yield from the dried biomass of H. illucens larvae were tested. Traditional pressing resulted to be the best system to maximize the oil yield and it was successfully applied to B. mori pupae. Oil quality resulted comparable to that obtained with other extraction methods described in the literature. In the case of B. mori pupae, different treatments and preservation periods were investigated to evaluate their influence on the oil composition and quality. Interestingly, agar diffusion assays demonstrated the sensitivity of Gram-positive Bacillus subtilis and Staphylococcus aureus to H. illucens and B. mori derived oils, whereas the growth of Gram-negative Pseudomonas aeruginosa and Escherichia coli was not affected. This study confirms that fat and other active compounds of the oil extracted by hot pressing could represent effective antimicrobials against bacteria, a relevant result if we consider that they are by-products of the protein extraction process in the feed industry.

Triple role of sodium salicylate in solubilization, extraction, and stabilization of curcumin from Curcuma longa

Solubility, extraction and stabilization of curcumin extracted from Curcuma longa are still a challenge. Either the solubility power of the extracting solvent mixture is not at its optimum or non-sustainable solvents are used or the curcumin instability against oxidation is a problem. In order to tackle these problems, we consider here a promising alternative solvent medium, which is a ternary system composed of water/sodium salicylate (an anionic, preservative hydrotrope)/ethyl acetate. The effects of the structuring of the system are also studied. The position of the new critical point and the orientation of tie-lines in the liquid/liquid area were determined and further examined via interfacial tension and diffusion ordered spectroscopy (DOSY NMR) measurements. The critical point between the mono-phasic region and the liquid/liquid area is a classical one, around which no special nano-structuring is found, in contrast to some other ternary mixtures with hydrotropes. The system was investigated in terms of its curcumin solubility and its extraction power thereof. Good extraction yields (~90% of the Soxhlet reference) could be achieved in the area of best solubility. Surprisingly, the hydrophobic curcumin shows a significant solubility in systems that contain a significant amount of water in presence of sodium salicylate. These mixtures are far from the critical point but show significant structuring. The solubility is even higher than in pure ethyl acetate. At the point of highest solubility (water/sodium salicylate/ethyl acetate 7/13/80 w/w/w) 15.48 mg of curcuminoids per g Curcuma longa are successfully extracted.The partition coefficient in the lower liquid/liquid two-phasic region was determined for a subsequent purification of curcumin by precipitation. Surprisingly, curcumin accumulates at the “oil-water” interface in the more polar phase. Sodium salicylate could be removed from the precipitated curcumin by washing it with water (no trace of sodium salicylate has been detected with NMR after the washing process).The preservative effect of salicylate against the oxidative effect of light on curcumin was found to be significant. A better stabilization of curcumin was observed far away from the critical point and was most efficient in the region, where aggregates could be detected. So, extraction, solubilization, and chemical stabilization of a light sensitive substance could be performed using an anti-oxidative hydrotrope.

Perfil químico e atividades antioxidante e antifúngica dos óleos essenciais de Raulinoreitzia crenulata (Spreng.) R. M. King &amp; H. Rob

Raulinoreitzia crenulata é uma espécie vegetal pertencente à família Asteraceae, apresentando compostos aromáticos nos galhos, folhas e flores. O objetivo deste trabalho foi avaliar o perfil químico e as atividades antioxidante pela redução do DPPH e antifúngica frente à Sclerotinia sclerotiorum, Colletotrichum gloeosporioides e Colletotrichum acutatum pelos óleos essenciais dos galhos, folhas e flores de R. crenulata. O material biológico foi coletado em uma área no município de Rio Verde, Goiás, Brasil. O óleo essencial foi extraído e o rendimento determinado. O perfil químico dos óleos essenciais foi determinado por CG-EM, a atividade antioxidante pela redução do radical livre DPPH e a atividade antifúngica por sucessivas diluições do óleo essencial em Dimetilsulfóxido. Os rendimentos dos óleos essenciais foram de 0,82; 0,64 e 0,09% para galhos, folhas e flores respectivamente. O perfil químico apresentou 33 compostos para o óleo dos galhos, 29 para o óleo das folhas e 28 compostos para o óleo das flores. A atividade antioxidante apresentou redução entre 100 a 25,09% para o óleo dos galhos, de 86,09 a 17,21% para o óleo das folhas e de 20,55 a 15,12% para o óleo das flores. A inibição de crescimento micelial para S. sclerotiorum apresentou os melhores resultados, seguido de C. gloeosporioides e em menor atividade fungistática para C. acutatum. Os resultados obtidos neste estudo apresentaram bons rendimentos de extração de óleo, eficientes atividades antioxidante e antifúngica. Os óleos essenciais de Raulinoreitzia crenulata apresentaram bons indicadores através dos ensaios laboratoriais para uso agrícola, biológico, farmacêutico e alimentício.

Multi-Targeted Metabolic Profiling of Carotenoids, Phenolic Compounds and Primary Metabolites in Goji (Lycium spp.) Berry and Tomato (Solanum lycopersicum) Reveals Inter and Intra Genus Biomarkers.

Metabolic profile is a key component of fruit quality, which is a challenge to study due to great compound diversity, especially in species with high nutritional value. This study presents optimized analytical methods for metabolic profiling in the fruits of three Solanaceae species: Lycium barbarum, Lycium chinense and Solanum lycopersicum. It includes the most important chemical classes involved in nutrition and taste, i.e., carotenoids, phenolic compounds and primary compounds. Emphasis has been placed on the systematic achievement of good extraction yields, sample stability, and high response linearity using common LC-ESI-TQ-MS and GC-EI-MS apparatuses. A set of 13 carotenoids, 46 phenolic compounds and 67 primary compounds were profiled in fruit samples. Chemometrics revealed metabolic markers discriminating Lycium and Solanum fruits but also Lycium barbarum and Lycium chinense fruits and the effect of the crop environment. Typical tomato markers were found to be lycopene, carotene, glutamate and GABA, while lycibarbarphenylpropanoids and zeaxanthin esters characterized goji (Lycium spp.) fruits. Among the compounds discriminating the Lycium species, reported here for the first time to our knowledge, chlorogenic acids, asparagine and quinic acid were more abundant in Lycium chinense, whereas Lycium barbarum accumulated more lycibarbarphenylpropanoids A-B, coumaric acid, fructose and glucose.

Physicochemical evaluation and antioxidant and antifungal activities of essential oils from Bauhinia forficata Link. and Bauhinia variegata L. flowers

&lt;em&gt;Bauhinia forficata&lt;/em&gt; essential oil showed good extraction yield. The CG-MS analysis showed 5 major compounds α-copaene, geraniol, α-bisabolene, caryophyllene and germacrene A. The percentage of mycelial inhibition in vitro showed higher sensitivity for &lt;em&gt;S. sclerotiorum&lt;/em&gt; and &lt;em&gt;A. flavus&lt;/em&gt; strains, the opposite was observed in &lt;em&gt;C. gloeosporioides&lt;/em&gt; that showed to be more resistant to essential oil concentrations. Future work may be carried out by evaluating the essential oil of &lt;em&gt;B. forficata&lt;/em&gt; flowers in a greenhouse and in the field by sprinkling or encapsulated micro or nano.

Blood and Plasma Volumetric Absorptive Microsampling (VAMS) Coupled to LC-MS/MS for the Forensic Assessment of Cocaine Consumption.

Reliable, feasible analytical methods are needed for forensic and anti-doping testing of cocaine and its most important metabolites, benzoylecgonine, ecgonine methyl ester, and cocaethylene (the active metabolite formed in the presence of ethanol). An innovative workflow is presented here, using minute amounts of dried blood or plasma obtained by volumetric absorptive microsampling (VAMS), followed by miniaturized pretreatment by dispersive pipette extraction (DPX) and LC-MS/MS analysis. After sampling 20 µL of blood or plasma with a VAMS device, the sample was dried, extracted, and loaded onto a DPX tip. The DPX pretreatment lasted less than one minute and after elution with methanol the sample was directly injected into the LC-MS/MS system. The chromatographic analysis was carried out on a C8 column, using a mobile phase containing aqueous formic acid and acetonitrile. Good extraction yield (> 85%), precision (relative standard deviation, RSD < 6.0%) and matrix effect (< 12%) values were obtained. Analyte stability was outstanding (recovery > 85% after 2 months at room temperature). The method was successfully applied to real blood and plasma VAMS, with results in very good agreement with those of fluid samples. The method seems suitable for the monitoring of concomitant cocaine and ethanol use by means of plasma or blood VAMS testing.

Optimization of SPE method for the extraction of 12 neurotransmitters from sheep brain

Abstract The present paper presents our attempts concerning the development of an extraction method for catecholamines. In order to achieve the extraction of all the selected solutes using a single SPE cartridge, several types of support were tested, among them: cation exchange supports, hydrophilic-lipophilic supports, C18 supports and PGC supports. As unfortunately none of the supports tested offered us the possibility of carrying out the extraction of 12 catecholamines from our standard mixture, we chose to use a coupling of two different cartridges: Oasis HLB and PGC which together ensure the extraction of all the compounds of the mixture with good extraction yields and with simple protocols. The selected cartridges were successfully tested for the extraction of a sample spiked from sheep brain with the 12 catecholamines in our mixture. The SPE method that we have developed allows the purification of the samples (a significant part of the components of the matrix is eliminated during this step) and also a preconcentration of the samples.