Determination of pesticides in honey by ultrasonic solvent extraction and thin-layer chromatography

A rapid method for quantitative determination of atrazine and simazine in honey samples was investigated. The procedure was based on the extraction of pesticides by sonication with benzene:water = 1:1 (v/v) mixture, thin-layer chromatographic separation and quantification by CAMAG Video Documentation system in conjunction with the Reprostar 3. The extraction procedure was optimized with regard to the amount of solvent, duration of sonication and the number of extraction steps. The apparent recovery of pesticides from honey was 92.3 ± 2.4 for atrazine and 94.2 ± 2.8 for simazine, when they were extracted in three steps for 20 min using 20 ml of solvent. Ultrasonic solvent extraction was compared with traditional shake-flask extraction method.     

Application of ultrasonic technique for extracting chlorogenic acid from Eucommia ulmodies Oliv. (E. ulmodies)

An ultrasonic method for the extraction of chlorogenic acid from fresh leaves of Eucommia ulmodies Oliv. was investigated and optimized. The influence of four extraction variables on extraction efficiency of chlorogenic acid was investigated. The optimum extraction conditions found were: 70% aqueous methanol; solvent: sample ratio=20:1 (v/w); extraction time 3 x 30 min. The recovery of chlorogenic acid was studied (HPLC) and the reproducibility of the extraction method was determined. The optimized ultrasonic extraction conditions were applied to extract chlorogenic acid from fresh leaves, fresh bark and dried bark of E. ulmodies and four traditional Chinese medicines. The application of sonication method was shown to be highly efficient in the extraction of chlorogenic acid from E. ulmodies and other Chinese medicines compared with classical methods.     

Continuous and pulsed ultrasound-assisted extraction of carob’s antioxidants: Processing parameters optimization and identification of polyphenolic composition

Polyphenols in carobs have recently attracted great attention due to their wide range of biological and health promoting effects. A comprehensive study was conducted to find an optimum method for the extraction, purification and characterization of these valuable bioactive substances. Under this framework, the ultrasound-assisted extraction (UAE) of polyphenols from carob pulp was optimized by the maximization of the yield in total phenolics using response surface methodology. In particular, the effects of solid-solvent ratio, solvent concentration, extraction time, sonication amplitude, and sonication mode were investigated and optimized using a complete experimental design. In comparison to conventional extraction techniques, UAE offered a higher yield of antioxidants and a shorter processing time. Solid-phase extraction was evaluated as a clean-up strategy prior to the electrophoretic analysis of extracts. The results from the analysis of real samples revealed the predominance of gallic acid and highlighted the great influence of the ripening stage on carobs composition.     

Ultrasound-assisted extraction of rutin and quercetin from Euonymus alatus (Thunb.) Sieb

An ultrasonic method for the extractions of rutin and quercetin from Euonymus alatus (Thunb.) Sieb was investigated. The influence of four extraction variables on extraction yield of rutin and quercetin was discussed. The optimum extraction conditions found were: 70% aqueous ethanol; solvent: sample ratio 40:1 (v/w); extraction time 3 x 30 min. The recovery of rutin and quercetin and the reproducibility of the extraction method were determined. The optimized ultrasonic extraction conditions were applied to extract rutin and quercetin from dried stalks of E. alatus (Thunb.) Sieb. The application of sonication method was shown to be highly efficient in the extraction of rutin and quercetin from E. alatus (Thunb.) Sieb, compared with classical methods. The scanning electron microscopy (SEM) micrographs provided evidence of more rapid opening of plant cells treated by UAE in contrast to maceration.     

Green ultrasound-assisted extraction of carotenoids based on the bio-refinery concept using sunflower oil as an alternative solvent

A green, inexpensive and easy-to-use method for carotenoids extraction from fresh carrots assisted by ultrasound was designed in this work. Sunflower oil was applied as a substitute to organic solvents in this green ultrasound-assisted extraction (UAE): a process which is in line with green extraction and bio-refinery concepts. The processing procedure of this original UAE was first compared with conventional solvent extraction (CSE) using hexane as solvent. Moreover, the UAE optimal conditions for the subsequent comparison were optimized using response surface methodology (RSM) and ultra performance liquid chromatography – diode array detector – mass spectroscopy (UPLC–DAD–MS). The results showed that the UAE using sunflower as solvent has obtained its highest β-carotene yield (334.75 mg/l) in 20 min only, while CSE using hexane as solvent obtained a similar yield (321.35 mg/l) in 60 min. The green UAE performed under optimal extraction conditions (carrot to oil ratio of 2:10, ultrasonic intensity of 22.5 W cm^?2, temperature of 40 °C and sonication time of 20 min) gave the best yield of β-carotene.     

The use of ultrasound in the extraction of Ilex paraguariensis leaves: a comparison with maceration

The objective of this work is to discuss the main parameters that influence the sonication extraction of Ilex paraguariensis leaves. For this purpose, the extraction time, solvent polarity, solvent volume, sample mass and particle size were evaluated. Results showed that the main variable affecting the extraction process was the solvent polarity. Though in a less extent, temperature and extraction time also demonstrated to be important parameters, while the other variables did not present a significant influence on the extraction yield. The extracts at the optimized condition were compared with those obtained by maceration, in terms of mass yield and chemical composition. The major compounds identified in the extracts were caffeine and palmitic acid. Some saturated hydrocarbons such as fatty acids, fatty acid methyl esters, phytosterols, and theobromine were also identified in the fractions.     

Ultrasonic energy enhanced the efficiency of advance extraction methodology for enrichment of trace level of copper in serum samples of patients having neurological disorders

An innovative dual dispersive ionic liquid based on ultrasound assisted microextraction (UDIL-μE), for the enrichment of trace levels of copper ion (Cu²⁺), in serum (blood) of patients suffering from different neurological disorders. The enriched metal ions were subjected to flame atomic absorption spectrometry (FAAS). In the UDIL-μE method, the extraction solvent, ionic liquid, 1-butyl-3-methylimidazolium hexafluorophosphate [C₄mim][PF₆], was dispersed into the aqueous samples using an ultrasonic bath. The(PAN) 1-(2-pyridylazo)-2-naphthol was used as ligand for the complexation of Cu ion in IL (as extracting solvent). The various variables such as sonication time, pH, concentration of complexing agent, time and rate of centrifugation, IL volume that affect the extraction process were optimized. The enhancement factor (EF) and detection limit (LOD) was found under favorable condition was 31 and 0.36 μg L⁻¹, respectively. Reliability of the proposed method was checked by relative standard deviation (%RSD), which was found to be <5%. The accuracy of developed procedure was assured by using certified reference material (CRM) of blood serum. The developed procedure was applied successfully to the analysis of concentration of Cu ion in blood serum of different neurological disorders subjects and referents of same age group. It was observed that the levels of Cu ion was two folds higher in serum samples of neurological disorders patients as related to normal referents of same age group.     

Effect of frequency and duration of ultrasonication on the extraction efficiency of selected isoflavones and trans-resveratrol from peanuts (Arachis hypogaea)

Plant derived phytochemicals have been the focus of recent research due to their health promoting effects. Previous studies to estimate the levels of these bioactive compounds made use of traditional solvent extraction procedures such as homogenization and soxhlet (reflux) methods. Recently, the ultrasonication technique has been shown to be an efficient non-thermal extraction method. The objective of this study was to investigate the effect of frequency and duration (time) of sonication on the extraction efficiency of selected phytochemicals from peanuts and to determine optimal conditions (sample-to-solvent ratio, frequency, and time) for their extraction. The results obtained showed that sample-to-solvent ratio, frequency, and duration of sonication had significant effect on the extraction efficiency of the phytochemicals from peanut. Sonication at 80 kHz facilitated the extraction of biochanin A and trans-resveratrol while 25 kHz was effective in the extraction of daidzein and genistein. Multi-frequency extractions were more efficient than single frequency.     

Ultrasound and deep eutectic solvents: An efficient combination to tune the mechanism of steviol glycosides extraction

Ultrasound-assisted extraction is widely recognized as an eco-friendly technique due to low solvent consumption and time extraction as well as enhanced extraction efficiency with respect to conventional methods. Nevertheless, it would be convenient to avoid the usually used organic solvents to reduce the environment pollution. In this regard, Deep Eutectic Solvents (DES) represent nowadays a green and sustainable alternative for the extraction of bioactive compounds from natural sources. In this study, an efficient extraction of stevioside and rebaudioside A from Stevia rebaudiana coupling ultrasound with DES was developed. A solvent screening was performed using the predictive approach COnductor-like Screening MOdel for Real Solvent (COSMO-RS). The effect of three independent variables, namely % of water, temperature, and sonication amplitude, were investigated by the response surface methodology (RSM). Comparing ultrasound-assisted extraction (UAE) with conventional extraction, it has been demonstrated that the amount of steviol glycosides through UAE is almost three times higher than that obtained by the conventional method. Possible physicochemical factors involved in the UAE mechanism were discussed.     

响应面法优化超声辅助提取-原子荧光法快速测定茶叶痕量汞

研究了一种使用超声波辅助提取(UAE)-原子荧光法测定茶叶痕量汞的快速方法.采用Plackett-Burman设计从6个影响汞提取率的因素中筛选出3个显著因素—超声时间St,超声温度T和HNO3:H2O2(1:1,δ)体积A2,并采用中心组合设计和响应面法优化参数.结果表明,最优提取条件为,浸泡时间6 min,St 8...     

Comparison of hydrodistillation and ultrasonic solvent extraction for the isolation of volatile compounds from two unifloral honeys of Robinia pseudoacacia L. and Castanea sativa L

A comparative study of ultrasound-assisted extraction (USE) with the mixture pentane:ether (1:2) and hydrodistillation (HD) with the same trapping mixture is presented for the isolation of volatile compounds from two unifloral honeys of Robinia pseudoacacia L. and Castanea sativa L. All HD isolates contained many thermally derived artefacts (especially phenylacetaldehyde with lower percentages of furfural, cis- and trans-linalool oxides and others). USE method gave the most representative profile of all honey volatiles (without artefacts). In addition, USE enabled extraction of low molecular weight semivolatile markers (especially benzoic, vanillic and phenylacetic acids) that were not extracted by HD. In this regard, low percentage of benzoic acid (0.7–7.4%), vanillic acid (0.0–1.6%) and phenylacetic acid (0.5–4.1%) was determined in Rp USE extracts, while Cs USE extracts contained phenylacetic acid (20.2–23.5%) as the major constituent with low percentage of benzoic acid (2.5–5.5%).     

超声波辅助溶剂萃取-电感耦合等离子体质谱法测定生物样品中的总汞和甲基汞

建立了超声波辅助溶剂萃取联用电感耦合等离子体质谱法(ICP-MS)测定生物样品中总汞(T-Hg)和甲基汞(MeHg)的分析方法。实验优化了萃取溶剂种类,溶剂浓度,各种辅助方法和超声波振荡时间等各种萃取条件。选择6 mol·L-1 HCl作为溶剂,超声2 h, 以有机溶剂萃取,再以水反萃,稀释后直接进行测量MeHg的含量。此方法可用于同时测定T-Hg和MeHg, 检出限为0.01 ng·mL-1,相对标准偏差为3.44％,线性范围为1～50 ng·mL-1,加标回收率为80%～97%。在此条件下测定了5种不同类型生物标准参考物质的T-Hg和MeHg,测定值与标准值吻合。该法综合了超声波辅助萃取和溶剂微萃取以及ICP-MS的优点,操作简便快速,灵敏度高,适合于各种生物样品中痕量MeHg快速萃取分离和分析。     

Molecular diversity of volatile compounds in rare willow (<Emphasis Type="BoldItalic">Salix</Emphasis> spp.) honeydew honey: identification of chemical biomarkers

Salix spp. honeydew honey volatiles were analyzed for the first time by headspace solid-phase microextraction (HS-SPME) and ultrasonic solvent extraction (USE) followed by gas chromatography and mass spectrometry (GC, GC-MS). The use of HS-SPME and USE had advantageous results over the use of one single technique, as it provided different complementary chromatographic profiles for a comprehensive screening of the honeydew volatile composition. The volatiles with different functionality, molecular weight, and polarity were extracted and identified. High percentages of benzoic acid, phenylacetic acid, 2-hydroxybenzoic acid, 4-hydroxyphenylacetic acid with minor percentages of 4-methoxybenzoic acid, 4-hydroxyphenylethanol, and 4-hydroxybenzoic acid from USE extracts can be emphasized as volatile biomarkers of this honeydew that probably originated from Salix spp., as well as methyl salicylate identified only by HS-SPME. The application of heat treatment at 80 °C for 2 h did not change significantly the volatile composition of this honeydew.     

Ultrasound-assisted deep eutectic solvents extraction of glabridin and isoliquiritigenin from Glycyrrhiza glabra: Optimization,extraction mechanism and in vitro bioactivities

Licorice (Glycyrrhiza glabra) is extensively used owing to the superior pharmacological effects. However, its maximum application potential has not been fully exploited due to the limitation of currently available extraction solvent and methods. In this study, an eco-friendly deep eutectic solvent (NADESs) based ultrasound-assisted extraction (DES-UAE) method was applied to prepare licorice extracts. The DES-UAE using choline chloride and lactic acid as solvent was optimized and modeled by using response surface methodology to maximize the extraction yields of glabridin (GLA) and isoliquiritigenin (ISL). The optimized extracts possessed higher contents of GLA and ISL than available extraction methods, and the enriched products showed superior pharmacological activities in vitro. Furthermore, scanning electron microscopy (SEM) and molecular dynamic simulation analyses were performed to deeply investigate the interaction between solvent and targeted compounds. This study not only provides an eco-friendly method for high-efficient extraction of GLA and ISL from licorice but also illustrates the mechanism of the increased extraction efficacy, which may contribute to the application of licorice and deep insight into extraction mechanism using DES.     

加速溶剂萃取-液相色谱-原子荧光法同时测定动物源性食品中阿散酸、硝苯砷酸与洛克沙砷的残留量

研究建立了加速溶剂萃取-液相色谱-原子荧光(ASE-LC-AFS)测定动物源性食品中阿散酸(ASA)、硝苯砷酸(NIT)与洛克沙砷(ROX)的残留量的方法。比较了超声离心提取和加速溶剂萃取技术,并优化了加速溶剂萃取技术的提取溶剂比例、提取温度、提取时间和提取次数。优化了液相色谱流动相和原子荧光的工作条件。在0～2.0 mg·L-1范围内内阿散酸、硝苯砷酸和洛克沙砷的线性关系良好,线性相关系数大于0.999,阿散酸、硝苯砷酸、洛克沙砷检出限(S/N=3)分别为2.4,7.4,4.1 μg·L-1。2种样品在0.5,2,5 mg·kg-13个加标水平下的平均回收率为阿散酸87.1%～93.2%, 硝苯砷酸85.2%～93.9%, 洛克沙砷84.2%～93.7%,相对标准偏差(RSD)分别为1.3%～4.6%,1.2%～4.2%,1.1%～4.5%。本方法操作简便,重现性好,适用于动物源性食品中ASA,NIT和ROX的分析。     

Comparison of distillation and ultrasound-assisted extraction methods for the isolation of sensitive aroma compounds from garlic (Allium sativum)

A comparative study of traditional simultaneous distillation extraction (SDE), microwave assisted hydrodistillation extraction (MWHD) and ultrasound-assisted extraction (USE) is presented, for the extraction of essential oils from fresh garlic (Allium sativum) cloves. Each method is evaluated in terms of qualitative and quantitative composition of the isolated essential oil. The highly reactive sulfur molecules of the garlic volatile fraction show variable response to the different isolation methods. The application of ultrasound for the extraction of the essential oil is considered to cause a lesser damage of thermal-sensitive molecules, thus, providing a better approach of the compounds primarily responsible for the characteristic odor and taste of freshly chopped garlic. All heat-involving isolation procedures have been shown to differentiate the volatile-fraction profile as analyzed by GC-MS. Especially when grouping the compounds into cyclic and acyclic, the percentage concentrations drop from 77.4% to 8.7% for the acyclic while that of the cyclic compounds increase from 4.7% to 70.8%. The observed fact may be attributed to the effect of the heat applied, which changes from harsh thermal treatment (SDE) to short time thermal (MWHD) and room-temperature isolation (USE). The use of USE proves to be crucial in order to provide reliable insight into garlic's chemistry.     

Ultrasound-assisted extraction of capsaicinoids from Capsicum frutescens on a lab- and pilot-plant scale

The influence of operating parameters (solvent type, powder to solvent ratio and temperature) on the ultrasonically assisted extraction of capsaicinoids from dried Capsicum frutescens (fruit) was studied. From the economic perspective, the suitable condition for capsaicinoid extraction by indirect sonication in an ultrasonic bath with a working frequency of 35 kHz was at a ratio of 1g of solid material: 5 ml of 95% (v/v) ethanol, 45 degrees C, where 85% of the capsaicinoids were removed from the raw material in 3h. In an experimental pilot study in 20-l extraction tank at the fixed ultrasonic frequency of 26 kHz and 70 kHz, the recovery of capsaicinoids was 76% and 70%, respectively. It was shown that the ultrasonic extraction produced a significant reduction in extraction time at a lower operational temperature than under a conventional industrial hot maceration process.     

Shock wave-assisted extraction of phenolic acids and flavonoids from Eysenhardtia polystachya heartwood: A novel method and its comparison with conventional methodologies

Phenolic compounds, obtained from plants are important in the food, biomaterial and pharmaceutical industries; however current extraction methods, such as Soxhlet (solid-liquid) extraction, liquid-liquid extraction, microwave-assisted extraction, and ultrasonic extraction (USE), have the disadvantages of large processing times, contamination by solvents, and degradation of analytes. This study demonstrates that shock wave-assisted extraction can be used as a more efficient, eco-friendly and rapid method. Extraction of powdered samples of Eysenhardtia polystachia heartwood, a plant with high concentration of phenolic compounds, exposed to different doses of underwater shock waves, was compared with the conventional methods. Our results revealed that shock wave-assisted extraction (1500 shock waves with a peak positive pressure of approximately 88 MPa) produced 34.54% and 31.95% higher contents than Soxhlet and USE, respectively. Extraction times using shock waves were much shorter than with all other methods tested, proving that it is an attractive method to obtain both phenolic acids and flavonoids without the need for organic solvents. Furthermore, shock waves produced a significantly higher content of total reducing sugars than Soxhlet extraction and less phenolic acids which gives the insight of a more selective extraction of components.     

在线流动注射液-液萃取非水介质汞还原原子荧光光谱法的研究及应用

提出了一种流动注射在线液－液萃取有机相汞还原原子荧光光谱法测定汞的新方法。该法以KI＋HNO3＋（NH2）2CS／TBP为萃取体系，将汞萃取到有机相中，汞还原反应是在金属络合萃取液与含NaBH4的N，N－二甲基甲酰铵（DMF）溶液和冰乙酸中发生。应用流动注射技术实现了液－液萃取非水介质汞还原反应原子荧光测定的在线分析。研究了反应的最佳条件和流动注射流路及运行程序。该法提高了测定灵敏度并消除了干扰。用于地质样品中汞的测定得到好的准确度和精密度。     

Optimization of ultrasonic extraction of 23 elements from cotton

Optimization of ultrasonic extraction of 23 elements from cotton was performed with different solvent volume ratios. For this purpose nitric acid, hydrochloric acid and water were mixed and applied in a mixture for the extraction of elements adsorbed on cotton material. The elements chosen for the extraction procedure (Al, As, Be, Bi, Ca, Cd, Co, Cr, Cu, Fe, Hg, K, Mg, Mn, Mo, Na, Ni, Pb, Sb, Si, Sn, Tl and Zn) were those that are important in textile processing. Some of them cause problems during fiber processing, dyeing or bleaching. The removal of elements from the processed fabric can be successfully done with ultrasonic extraction in the ultrasonic bath. Extraction procedure was optimized by software package Design Expert 6 (DX6) and the optimum of ultrasonic extraction was achieved with the mixture of 1M HCl-1M HNO(3)-H(2)O=3.32/2.83/93.85 (v/v). Ultrasonic extraction was a fast and efficient extraction procedure easily applied on cotton textile material.