Ultrasound-assisted Extraction Procedure Research Articles

Stability of Propolis Phenolics during Ultrasound-Assisted Extraction Procedures.

Propolis has gained popularity in recent years as a potential preventive and therapeutic agent due to its numerous health benefits, which include immune system boosting, blood pressure lowering, allergy treatment, and skin disease treatment. The pharmacological activity of propolis is primarily attributed to phenolics and their interactions with other compounds. Given that phenols account for most of propolis's biological activity, various extraction methods are being developed. The resin-wax composition of the propolis matrix necessitates the development of an extraction procedure capable of breaking matrix-phenol bonds while maintaining phenol stability. Therefore, the aim of this study was to assess the stability of two major groups of phenolic compounds, flavonoids and phenolic acids, in propolis methanol/water 50/50 (v/v) extracts obtained after ultrasound-assisted extraction (USE) under different extraction parameters (extraction time and pH) and heat reflux extraction (HRE). The methodology involved varying the USE parameters, including extraction time (5, 10, and 15 min) and pH (2 and 7), followed by analysis using liquid chromatography-tandem mass spectrometry (LC-MS/MS) to quantify phenolic recoveries. Results revealed that benzoic acid and chlorogenic acid derivatives demonstrated excellent stability across all ultrasound extraction procedures. The recoveries of flavonoids were highly diverse, with luteolin, quercitrin, and hesperetin being the most stable. Overall, neutral pH improved flavonoid recovery, whereas phenolic acids remained more stable at pH = 2. The most important optimization parameter was USE time, and it was discovered that 15 min of ultrasound resulted in the best recoveries for most of the phenols tested, implying that phenols bind strongly to the propolis matrix and require ultrasound to break the bond. However, the high variability in phenol extraction and recovery after spiking the propolis sample shows that no single extraction method can produce the highest yield of all phenols tested. As a result, when working with a complex matrix like propolis, the extraction techniques and procedures for each phenol need to be optimized.

Choline chloride-L-lactic acid mixtures as solvents for extraction of Coumarin from cinnamon-containing foods

The determination of coumarin in generally available cinnamon-containing foods such as biscuits, cereals is important to ensure that the populations consuming these foods more frequently are not exposed to higher levels and are not at risk. This study describes the development of an analytical method for determination of coumarin in foods containing cinnamon. Solid-liquid phase extraction with conventional stirring-assisted and ultrasound-assisted extraction (UAE) procedures were used to prepare sample extracts for liquid chromatography analysis. The green solvent, a mixture of choline chloride:L-lactic acid (1:4, mol/mol)/water (50:50 v/v), as a deep eutectic solvent-like mixture, was selected as an extraction solvent. The extraction conditions were optimized by using the design of the experiment strategy obtaining parameters, temperature 47 °C, time 36 min, solvent volume 4 mL, sample amount 0.8 g, stirring speed 20 rpm for rotary stirring-assisted extraction procedure, and temperature 30 °C, time 5 min, solvent volume 3.5 mL, sample amount 0.8 g for UAE. High-performance liquid chromatography separation with a total analysis time of 12 min was performed with a stationary phase of octadecyl type and a gradient of mobile phase of methanol-1 % acetic acid. The methods were successfully validated to show the detection limit of 0.13 μg.mL−1, the linearity range of 0.4–50 µg.mL−1 (R2 = 0.999), recovery values more than 80 %, and the RSDs of less than 7 %. Rotary stirring-assisted extraction showed moderately higher recovery values than UAE, while lower RSD % was observed for UAE.

Microscopic characterization, TLC fingerprinting and optimization of total lipid content from Euphorbia neriifolia (L.) using response surface methodology.

Euphorbia neriifolia (EN) is a medicinal plant used to treat a variety of ailments in traditional systems. Despite numerous studies on pharmacological activities, no information was available on the microscopic study of this plant. This is the first study that has been attempted to fill this need by performing the light and field emission scanning electron microscopy (FESEM) of leaf, stem, and latex. The powder microscopy of several organs (leaves, stem, and bark) and exudate (latex) of EN was carried out using safranine, fast green, phloroglucinol, and other standard solutions at different magnifications. The chemical fingerprinting of petroleum ether extract was accomplished by using thin layer chromatography. The optimization of total lipid content from the EN leaf under ultrasound-assisted extraction (UAE) and soxhlet extraction (SE) procedure was determined using response surface methodology (RSM). The studied factors that affect the lipid content were: solvent ratio, extraction temperature, and extraction time. Several notable characteristics observed in the leaf of EN are amphistomatic leaves with anticlinical cell walls, anomocytic stomata, spongy mesophyll cells, elongated palisade cells, angular collenchyma, and U-shaped vascular bundle. The plano-convex midrib is covered by polygonal to oval-shaped cuticles and contains anomocytic stomata. The circular petiole has no trichomes and contains laticifers, crystals, and idioblasts. The circular stem was observed with trichomes, hypodermis, collenchyma, parenchymatous cells, central pith, pentagonal stellar region, cambium, and 2-4 times more xylem that of phloem. All of the powdered plant parts and exudate under study contained trichomes, xylem vessels, wood fibers, cork cells, starch grains, calcium oxalate crystals, idioblasts, lignified cork, tannin content, stone cells, and oil globules. The blackish-green colored petroleum ether extract with semi-solid consistency showed the greatest percent (%) yield of 4% in the latex of EN. The thin layer chromatography (TLC) examination of petroleum ether extract of EN leaf produced a maximum 6 spots with Rf values of 0.16, 0.58, 0.62, 0.73, and 0.96 in the mobile phase of petroleum ether-acetone (8:2). In terms of optimization, the dark green colored UAE extract with semi-sticky consistency showed highest % yield of 4.5% whereas the yellowish green colored SE extract of sticky consistency showed the highest % yield of 4.9%. The findings showed that there were not many differences in the total lipid content between UAE (0.16%) and SE (0.11%). However, the best optimum condition for lipid content extraction analysis was obtained as follows: solvent ratio (PE:HE) 50:50, extraction temperature 50°C, extraction time 45 min for UAE, and solvent ratio (PE:HE) 60:40, extraction temperature 45°C, and extraction time of 24 h for SE. Hence, this study signifies the various noteworthy microscopic features along with the presence of different phytocompounds through TLC and best optimized condition for the extraction of lipids from different parts of EN. As no previous study has been reported, the outcomes obtained from the current study prove to be beneficial in the identification of species, quality control, and detection of any adulteration from the laboratory and commercial samples of EN. RESEARCH HIGHLIGHTS: The percent yield was found to be maximum in latex extract (4%). The leaf pet ether extract was separated into 6 bands with different Rf values. The extracted compounds from Euphorbia neriifolia leaves were categorized into non-polar heat tolerant. The highest total lipid yield (0.1119) was obtained at solvent ratios 60:40 of PE:HE (petroleum ether: petroleum hexane).

Optimization of experimental conditions for bioactive compounds recovery from raspberry fruits (Rubus idaeus L.) by using combinations of ultrasound-assisted extraction and deep eutectic solvents

Raspberry fruits (Rubus idaeus L.) have been reported to contain phenolic compounds, of which anthocyanins are the most abundant. A novel procedure of ultrasound-assisted extraction (UAE) using deep eutectic solvent (DES) for efficient extraction phenolic compounds and anthocyanins from raspberries is considered. Namely, the green approach for optimization by response surface methodology (RSM) based on Box-Behnken Design (BBD) was proposed in this study. Three carboxylic acid-based DES, like acetic acid/glucose (DESAAGLU), formic acid/glucose (DESFAGLU), and lactic acid/maltose (DESLAMA), were tested for their efficiency in the recovery of phenolic compounds and anthocyanins from raspberries. The optimum extraction parameters were obtained; extraction time of 60 min, a solvent volume of 35 mL, and added water on DES of 30 mL (v/v). The results of this study indicated that optimizing extraction conditions are critical for quantifying phenolic compounds and anthocyanins. The present model can contribute to finding a cheap way of delivering natural bioactive compounds in the food, cosmetic, and pharmaceutical industriesas well as a natural food colorant in dietary applications with potential health benefits.

Development of an Ultrasound-Assisted Extraction Procedure for the Simultaneous Determination of Anthocyanins and Phenolic Acids in Black Beans.

Beans are an essential source of nutritional components such as plant proteins, minerals and dietary fiber, as well as of antioxidants such as phenolic compounds. Phenolic compounds are praised for their biological activities and possible benefits on human health. Since no official methods are available for phenolic compound extraction, the optimization of extraction parameters via Response Surface Methodology (RSM) has become a commonly used methodological approach for reliable determinations. This study aimed to apply RSM to optimize the ultrasound-assisted extraction procedure of phenolic compounds, including anthocyanins, from black beans. A Generally Recognized As Safe solvent (ethanol) was used. Solvent concentration, extraction time, and solvent/sample ratio were optimized to maximize two responses: Total Anthocyanin Content (TAC) and Total Phenolic Content (TPC). An ethanol concentration of 64%, 30 min extraction time, and a 50 mL/g solvent/sample ratio were identified as the optimal extraction conditions. The TAC was 71.45 ± 1.96 mg cyanidin-3-O-glucoside equivalents 100 g-1 dm, and the TPC was 60.14 ± 0.89 mg gallic acid equivalents 100 g-1 dm. Among the pigmented phenolic compounds, cyanidin-3-O-glucoside and peonidin-3-O-glucoside were identified in the extracts. Regarding phenolic acids, caffeic, sinapic, and t-ferulic acids were detected.

New selective and sustainable ultrasound-assisted extraction procedure to recover carnosic and rosmarinic acids from Rosmarinus officinalis by sequential use of bio-based solvents

Carnosic (CA) and rosmarinic (RA) acids are the primary phenolic acids in hydrophilic rosemary extracts. Their combination exhibits high antioxidant activity and can be explored in several applications. This study aimed to develop an extraction procedure using bio-based solvents to recover two rosemary extracts, one rich in CA and the other in RA. By using ultrasound-assisted extraction (UAE) and a pool of 34 solvents, we evaluated nominal power (W), extraction time (min), and solvent water percentage (% H2O) regarding yield and selectivity. The authors propose a sequential UAE procedure validated by applying ethanol 99.5 % (v/v), 240 W, and 5 min to recover a rich fraction of 24.0 mgCA.gbiomass−1; followed by a second step using AmAc:LA (1:2 M ratio), 20 % H2O (m/m), 320 W, and 5 min that resulted in 8.4 mgRA.gbiomass−1. Our results indicate that modulating the solvent composition and process temperature is critical to increasing extraction yields and selectivity.

Determination of releasing plasticizers from dental floss using ultrasound–assisted extraction–dispersive liquid–liquid microextraction followed by gas chromatography–flame ionization detector

Recently, the wide existenceof phthalate esters in healthcare products has attracted great attention from scientists due to their negative effects on human health. As a result, the current study was carried out to determine the presence of some plasticizers in dental floss such as di-n-butyl phthalate, diethyl phthalate, di-2-ethylhexyl phthalate, di-iso-butyl phthalate, and bis-2-ethylhexyl adipate. The studied analytes were extracted from dental floss by an ultrasound–assisted extraction procedure and then enriched by a dispersive liquid–liquid microextraction method. For this purpose, a piece of dental floss was immersed in acetonitrile under sonication to extract the analytes. Then, the acetonitrile phase containing the extracted analytes was mixed with a proper extraction solvent at µL–level and injected into sodium chloride solution. The extracted analytes were determined by gas chromatography–flame ionization detector and gas chromatography–mass spectrometry. Under the best extraction conditions, limits of detection and quantification were found in the ranges 0.20–0.33 and 0.67–1.1 µg/L in solution and 0.06–0.10 and 0.19–0.33 µg g−1 in dental floss, respectively. Relative standard deviations were in the ranges 4.0–6.5% and 5.1–7.9% for intra-day and inter-day precisions for five replicates at 60 µg/L of each analyte. Enrichment factors and extraction recoveries of the analytes ranged from 350 to 460 and 70–92%, respectively.

Green and fast ultrasound-assisted extraction procedures for Fe, Mn, Mg and Ca analysis in cane syrups by FAAS

New methodologies for the analysis of Fe, Mn, Mg, and Ca content in cane syrups using FAAS combined with ultrasound-assisted extraction (UAE) were developed and validated. For multivariate optimization of UAE, a simplex-centroid mixture design and individual desirability functions were applied to achieve the best composition of extraction solvents (HNO3, HCl, and water). Under optimal conditions of ultrasound-assisted extraction (100 W, 37 kHz, 10 min, 5.0 mL of extraction solvent (ultrapure water for Fe and Mn and HNO3:H2O (75:25%, v/v), corresponding to a 1.19 mol L−1 HNO3 solution for Mg and Ca)), method validation showed good linearity, confirmed by regression analysis, and low LOD and LOQ values of 0.266–0.284 μg g−1 and 0.114–0.861 μg g−1. Estimates of repeatability and mean precision (RSD = 0.44–2.11%), Horrat values (0.07–0.26), and assessment of trueness by comparing sample preparation methods using a paired t-test demonstrated the excellent precision and trueness of the developed methods. The methods were applied to twenty-five cane syrup samples, and the results of the multivariate analysis showed that the metal ions can be used as indicators of geographical origin or contamination during manufacturing or processing, thus helping to ensure the food quality and safety of this sweetener.

Improvement of ultrasound-assisted extraction of polyphenolic content of the plant Cytisus triflorus L'Her as a natural resource using artificial neural network modeling and multi-objective optimization

The improvement of environmental performance of production processes is a critical problem right now. Processes that are effective in terms of productivity and environmental effects are the center of interest of researchers. This study established such a method for an ultrasound-assisted extraction procedure. The plant Cytisus triflorus L'Her was used to extract polyphenolic chemicals using ultrasound-assisted extraction as a quick, less energy consuming, high-yield technology. This work offers a new experimental planning approach using Artificial Neural Networks, that enables the extraction process to be optimized using multi-objective optimization in order to identify the best extraction conditions to obtain the maximum polyphenolic compounds possible. Advanced modeling using Artificial intelligence and statistical optimization techniques was used to determine the best combinations of ethanol concentration, extraction temperature and time for the maximum extraction of total phenols, total flavonoids, total flavonols, and total tannins. An artificial neural network (ANN) was used to build the models for each of the four goals, then they were multi-objectively optimized using a genetic algorithm technique. The maximum polyphenolic contents including TPC (4.986 ± 0.006 mg GA/g DE), TFC (14.026 ± 0.070 mg Q/g DE), TFolC (5.225 ± 0.010 mg R/g DE), and TTC (6.240 ± 0.021 mg C/g DE) were obtained using an extraction process under optimal conditions, which included a solvent concentration of 78%, an extraction temperature of 52 °C, and an extraction time of 55 min which were obtained using the MOO Pareto optimum solution selection approach Gray Relational Analysis GRA.

An aqueous olive leaf extract (OLE) ameliorates parameters of oxidative stress associated with lipid accumulation and induces lipophagy in human hepatic cells.

Fatty liver is a disease characterized by a buildup of lipids in the liver, often resulting from excessive consumption of high-fat-containing foods. Fatty liver can degenerate, over time, into more severe forms of liver diseases, especially when oxidative stress occurs. Olive leaf extract (OLE) is a reliable source of polyphenols with antioxidant and hypolipidemic properties that have been successfully used in medicine, cosmetics, and pharmaceutical products. Using "green" solvents with minimal impact on the environment and human health, which simultaneously preserves the extract's beneficial properties, represents one of the major challenges of biomedical research. In the present study, we assayed the potential antioxidant and lipid-lowering effect of a "green" OLE obtained by a water ultrasound-assisted extraction procedure, on the human hepatic HuH7 cell line, treated with a high concentration of free fatty acids (FFA). We found that high FFA concentration induced lipid accumulation and oxidative stress, as measured by increased hydrogen peroxide levels. Moreover, the activity of antioxidant enzymes, catalase, superoxide dismutase, and glutathione peroxidase, was reduced upon FFA treatment. Coincubation of high FFA with OLE reduced lipid and H2O2 accumulation and increased the activity of peroxide-detoxifying enzymes. OLE ameliorated mitochondrial membrane potential, and hepatic parameters by restoring the expression of enzymes involved in insulin signaling and lipid metabolism. Electron microscopy revealed an increased autophagosome formation in both FFA- and FFA + OLE-treated cells. The study of the autophagic pathway indicated OLE's probable role in activating lipophagy.

Chemical Profile and Skin-Beneficial Activities of the Petal Extracts of Paeonia tenuifolia L. from Serbia.

Without being aware of its chemical makeup, many ancient societies have used Steppe peony in their traditional medicine. Given that modern phytopreparation intended for use on human skin requires, above all, knowledge of its chemical composition, the goal of this study was to make a screening of the composition of aqueous and methanolic extracts of the petals of P. tenuifolia L. and to examine them for various skin-beneficial properties. The extracts were prepared by maceration, ultrasound-assisted, and microwave-assisted extraction procedures. The chemical profiling was conducted by the use of UHPLC-LTQ-OrbiTrap MS and UHPLC/MS, and spectrophotometric methods for the determination of total polyphenol and total flavonoid contents. The biological activities entailed antioxidant ABTS, DPPH, CUPRAC (Cupric Ion Reducing Antioxidant Capacity), and FRAP (Ferric Reducing Antioxidant Power) assays, antimicrobial (antibacterial and antifungal) and antibiofilm activities, cytotoxicity, wound healing potential, as well as the adhesion and invasion of Staphylococcus lugdunensis. The results showed that the petals are rich in phenolic acids and flavonoids, which are commonly associated with numerous biological activities. The aqueous extracts were more efficient in the majority of the bioactivity assays then the methanolic ones, whereas the optimal extraction method varied between the assays. This study is the first step towards the safe use of the aqueous extracts of P. tenuifolia petals for therapeutic skin treatments.

Sourcing New Ingredients for Organic Cosmetics: Phytochemicals of Filipendula vulgaris Flower Extracts

Plant extracts are well known for their beneficial cosmetic properties based on bioactive phytochemicals with highly demonstrated antimicrobial and antioxidant capacities as phenolic compounds. This work presents the polyphenolic characterization of different extracts from organically grown Filipendula vulgaris. An ultrasound-assisted extraction procedure is proposed for obtaining ethanolic extracts at the laboratory level, both from dried and fresh plants, to be compared with those obtained by classical flower processing techniques for cosmetic purposes. The individual quantification of target phenolic compounds was carried out using liquid chromatography-mass spectrometry (LC-MS/MS). The results revealed the presence of 24 phenolic compounds in the analyzed samples, ranging in concentrations from 0.1 to 71.64 µg g−1. The total phenolic content (TPC) ranging from 1163 to 6114 mg GAE L−1, and the antioxidant activity (AA), from 6 to 52 mmol TRE L−1, were also evaluated. The differences were established between the plant material and extraction technique.

Effects of ultrasound-assisted extraction procedure on total phenolics, catechin and caffeine content of green tea extracts

This study was conducted to investigate the changes encountered in water soluble dry matter (ºBrix), total phenolics, caffeine and some important catechins of green tea extracts extracted through ultrasound-assisted extraction procedures. Extractions were conducted at 70°C temperature, different tea: water ratios (5:100; 10:100) and brewing times (5, 10 and 20 min) and resultant extracts were also supplemented with tannase enzyme. Total phenolics of green tea extracts varied between 2.68 - 3.87 g GAE/100 g dry green tea. The greatest total phenolics (3.87 g GAE/100 g dry green tea) was obtained from 20 min brewing at 70°C and 10:100 tea: water ratio of tannase enzyme-supplemented extract. As compared to the control samples, decreasing EGCG and ECG contents and increasing EGC and EC contents were observed with tannase enzyme supplementations.

Evaluation of different extraction procedures for the quantification of seven cannabinoids in cannabis-based edibles by the use of LC-MS

Although still illegal in many countries, food products containing cannabis or marijuana extracts have become very popular in recent years. In the present study, an LC-MS method was developed for the quantitative analysis of seven cannabinoids in various solid and liquid cannabis-based goods. The proposed analytical approach demonstrated satisfactory performance characteristics in terms of linearity (R2≥0.995), accuracy (recovery: 70.0–110 %), precision (intraday RSD: 0.950–6.03 %, interday RSD: 1.02–6.94 %), sensitivity (LOD≤2.19 ng/mL, LOQ≤6.59 ng/mL) and carry-over effect (average carryover signals ≤3.90 %). Solid-phase extraction (SPE), and ultrasound-assisted extraction (UAE) were utilized for the extraction of the analytes from liquid cannabis edibles (beer and energy drink), while Soxhlet and ultrasound-assisted extraction (UAE) were used for solid products (chocolates, hemp seeds, hemp tea). Infusion and decoction processes were followed for cannabis hemp tea and roasted coffee, respectively. UAE provided higher extraction efficiencies for cannabis-based edibles in solid form, while infused-cannabis beverages were extracted more efficiently using the SPE procedure. Cannabidiol (CBD) and cannabigerol (CBG) were the most detectable cannabinoids in all examined samples. Significantly high levels of cannabinoids were detected in cannabis tea extract prepared by the UAE procedure (total cannabinoids: 5440 μg/g). According to the suppliers, all examined samples were supposed to be free of Δ9-tetrahydrocannabinol (Δ9-THC). However, five products were found to contain considerable amounts of this compound (0.600–180 μg/g). Only in the case of cannabis beer, cannabis roasted coffee, and cannabis energy drink, Δ9-THC was not detected.

Temperature-responsive deep eutectic solvent as eco-friendly and recyclable media for the rapid assessment of pyrethroid pesticide residues in surface soil sample

In the modern agricultural model, more and more attention has been paid to green production and sustainable agriculture practices. In this study, a simple and eco-friendly extraction method for the rapid assessment of nine different pyrethroid pesticides in surface soil samples was developed by the temperature-responsive deep eutectic solvent-based ultrasound assisted extraction. Three different temperature-responsive deep eutectic solvent systems of various classes were prepared to extract pyrethroid pesticides from spiked soil samples. The total spiked recovery displayed that temperature-responsive deep eutectic solvent composed of ethanolamine and o-cresol with molar ratio 1:1 was the optimum extraction solvent for temperature-responsive deep eutectic solvent-based ultrasound assisted extraction procedure. Based on Box-Behnken Design, the maximum extraction recovery (%) of total pyrethroid pesticides was 94.23% under the following conditions: extraction temperature of 68 °C, extraction time of 35 min, and solid–liquid ratio of 21 mg/mL. Meaningfully, the extraction recovery of pyrethroid pesticides was still more than 80% after fifth cycles of temperature-responsive deep eutectic solvent, demonstrating that temperature-responsive deep eutectic solvent could be repeatedly used. The detection results of actual soil samples indicated that the pyrethroid pesticide residues (8.42–28.72 μg/kg) in vineyard region were the most serious, which may be due to the high incidence of insect pests and the abuse of pesticides. The temperature-responsive deep eutectic solvent-based ultrasound assisted extraction method with the advantages of fast, trace, and high efficiency could be successfully applied to pyrethroid pesticide residues analysis in surface soil samples.

Multivariate approaches applied to optimization of an ultrasound-assisted extraction procedure for determination of essential elements in guarana samples by ICP OES

In the present work, a simple and high-throughput analytical procedure based on ultrasound-assisted extraction with diluted acid was proposed for the determination of Ca, Mg, K, P, S, Fe, Cu and Mn in guarana samples using inductively coupled plasma optical emission spectrometry. Two multivariate approaches were employed for optimization of the extraction procedure: mixture and Doehlert designs. The best experimental conditions were established by application of a multi-response function (overall desirability). An extractor medium composed of diluted nitric acid was selected for analytes extraction. Optimized conditions for ultrasound-assisted extraction followed the temperature of 60 °C, sonication time of 10 min and power of 100% applied to the ultrasonic bath. After the analytical validation step, the proposed procedure was successfully employed for determination of essential elements in thirty-three guarana samples from the state of Bahia, Brazil. Mass fractions higher than 0.42% (m m-1) were found for potassium in all analyzed samples. For the other macro-elements, the mass fraction ranged from 514 mg kg-1 (magnesium) to 0.19% m m-1 (calcium). The mass fraction of micro-elements ranged from 5.1 to 91.3 mg kg-1 for cooper and iron, respectively.

Titanium dioxide nanoparticles assessment in seaweeds by single particle inductively coupled plasma – Mass spectrometry

In this study, a first attempt for isolating and determining (characterising) background levels of titanium dioxide nanoparticles (TiO2 NPs) in seaweed has been developed by using single particle inductively coupled plasma – mass spectrometry (SP-ICP-MS). Seaweeds were processed using an optimised ultrasound assisted extraction (UAE) procedure based on tetramethylammonium hydroxide (TMAH) before dilution and SP-ICP-MS analysis. The effect of the TMAH percentage in the extracting solution, as well as the volume of extracting solution and sonication (extraction) time, has been fully assessed. Additional experiments also showed that TiO2 NPs were quantitatively released from the seaweed matrix in one UAE step since the analysis of residues gave TiO2 NPs concentrations lower than the limit of quantification (LOQ) of the method. Validation of the method with 50 and 100 nm TiO2 NPs (10 μg L−1 as Ti) showed good analytical recovery (115% and 112% for 50 and 100 nm TiO2 NPs, respectively), and good reproducibility (2% for size and 16% for number of TiO2 NPs). Experiments regarding TiO2 NPs stability showed that the extracted NPs are stable since there were not changes on the number of TiO2 NPs and TiO2 NPs size distributions when exposing TiO2 NPs standards to the optimised extractive conditions.

Simultaneous determination of multi-class active pharmaceutical ingredients by UHPLC-HRMS

In this work, a UHPLC-HRMS method using a quadrupole-orbitrap mass spectrometer has been developed for the detection and quantification of 47 compounds. These compounds include a range of chemical structures and properties and are popularly referred to as active pharmaceutical ingredients (API). The APIs selected have historically been incorporated into a variety of products commonly marketed towards acne, hair loss, male erectile dysfunction, and skin whitening. A fast ultrasound-assisted extraction (UAE) procedure without sample cleanup was developed and a high-resolution product ion spectral library was generated for compound verification in complex matrices. Collision energies were optimized for all analytes to overcome the limitations by applying stepped collision energies, such as insufficient fragmentation and excessive fragmentation without molecular ion information. Higher HRMS2 spectra matching scores (0.6 or above) were obtained for the analytes in the tested complex matrices. Eleven representative stable isotopically labeled API analogs were used as internal standards to compensate for the influence of complex matrices, such as shampoo and creams, and as an instrument quality control. One-hundred products with complex matrices were analyzed using the validated UHPLC-HRMS method. Eight APIs (ketoconazole, hydroquinone, salicylic acid, benzocaine, progesterone, azelaic acid, lidocaine, and minoxidil) were identified in 26 out of 100 products ranging from 103 μg/g to 156,000 μg/g.

An Ultraperformance Liquid Chromatography Tandem-Mass Spectrometry Method for Determination of Multiclass Pharmaceuticals in Water Sample by Dispersive Liquid-Liquid Microextraction Combined with Ultrasound Assisted Reverse Extraction from Solidified Floating Organic Droplets.

A novel, simple, and reliable ultraperformance liquid chromatography tandem-mass spectrometry (UPLC–MS/MS ) assay based on dispersive liquid–liquid microextraction followed by ultrasound-assisted reverse extraction from solidified floating organic droplets was established for determination of multiclass pharmaceuticals in the water sample. Six commonly used drugs of various therapeutic classes: ibuprofen, ketorolac, lamotrigine, propranolol, pantoprazole, and losartan were extracted from water samples by using 50 μL 1-undecanol as extracting solvent and 400 μL acetonitrile as dispersive solvent. After collecting the floating organic droplets by cold centrifugation, an ultrasound-assisted back extraction procedure was performed to make the sample compatible for UPLC–MS/MS analysis. Acquity BEH C18 column (2.1 × 100; 1.7 μm) was used for separation of target analytes that were eluted by a gradient mobile phase composition of 15 mM ammonium acetate and acetonitrile at a flow rate of 0.25 mL/min. The sample ionization was performed by using electrospray ionization in positive mode, and multiple reaction monitoring was used for quantification of target analytes. After optimizing the assay conditions, all calibration curves were found to be linear with limit of detection and limit of quantification were ranged in between 0.06–0.15 and 0.16–0.41 ng/mL, respectively. The enrichment factor was found to be 172–192-fold and the relative recovery was ranged between 93.1 and 109.4% between target analytes. These satisfactory results confirmed that the proposed method is specific and reliable for application of trace analysis of target analytes in waste water samples.

Extraction of Gallic Acid from Chromolaena sp. Using Ultrasound-assisted Extraction

Chromolaena sp. is believed to have phytochemical components namely alkaloids, flavonoids, flavone, essential oils, phenolics, saponins, tannins and terpenoids. In this study, ultrasound-assisted extraction (UAE) procedure was performed to extract the gallic acid extraction from the Chromolaena sp. UAE is known to be an environmentally green extraction method. The experiment was carried out with two different parameters which are sonication time and duty cycle. Phytochemical screening, High performance Liquid Chromatography (HPLC) and Fourier-transform infrared spectroscopy (FT-IR) was employed to determine the optimum condition for the extraction method. Phytochemical screening result showed the presence of phenolic compound when the dark-green colour of solution was observed. The optimum extraction conditions were as follows: sonication time of 80 minutes with yield of 3.0060 mg/mL and duty cycle of 10% with yield of 3.7641 mg/mL. The FT-IR result shows that presence of O-H and alkene group in the extraction sample. From the result, it can be concluded that UAE is an effective method to extract gallic acid from Chromolaena sp. The implication in this study were reducing the extraction time for the production of herbs medicine from natural resource like plant.