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The molecularly imprinted polymer was synthesized using 3-aminopropylthiosilane-methacrylic acid monomer (APTES-MAA) as the functional monomer and 10-hydroxycamptothecin (HCPT) as the template, based on computer simulation. The hybrid molecularly imprinted polymers (HMIPs) were characterized using Fourier transform infrared spectroscopy, thermogravimetric analysis, particle size measurement, scanning electron microscopy and energy dispersive X-ray spectroscopy. It has been shown that HMIPs are irregularly shaped and porous, with particle sizes ranging mainly from 130 to 211 nm. At 298 K, the HMIPs exhibit a maximum adsorption capacity of 8.35 mg·g -1 for HCPT and demonstrate good adsorption specificity ( α  = 5.38). The pseudo-second-order reaction mechanism suggests that the equilibrium adsorption capacity of HCPT on HMIPs is 8.11 mg·g -1 . Finally, HCPT was successfully separated and enriched from the extract of Camptotheca acuminata Decne. seeds using HMIPs.

Traditional solid phase extraction (SPE) suffers from a lack of specific adsorption. To overcome this problem, a combination of adsorption method and molecular imprinting technology by polydopamine modification was proposed to realize specific recognition of target compounds in SPE, which is of great significance to improve the separation efficiency of SPE. Cellulose hydrogel beads were prepared by dual cross-linking curing method and modified with polydopamine to make them hydrophilic and biocompatible. Subsequently, cellulose hydrogel-based molecularly imprinted beads (MIBs) were synthesized by surface molecular imprinting technology and used as novel column fillers in SPE to achieve efficient adsorption (34.16 mg·g -1 ) with specific selectivity towards camptothecin (CPT) in 120 min. The simulation and NMR analysis revealed that recognition mechanism of MIBs involved hydrogen bond interactions and Van der Waals effect. The MIBs were successful used in separating CPT from Camptotheca acuminata fruits, exhibiting impressive adsorption capacity (1.19 mg·g -1 ) and efficient recovery of CPT (81.54 %). Thus, an environmentally friendly column filler for SPE was developed, offering a promising avenue for utilizing cellulose-based materials in the selective separation of natural products., Competing Interests: Declaration of competing interest The authors declare that they have no known competing financial interests or personal relationships that could have appeared to influence the work reported in this paper., (Copyright © 2024 Elsevier Ltd. All rights reserved.)

In a mixed forest, certain plants can release allelochemicals that exert allelopathic effects on neighboring plants, thereby facilitating interspecific coexistence of two species. Previous studies have demonstrated that allelochemicals released from Ficus carica Linn. roots in mixed forest of F. carica and Taxus cuspidata Sieb. et Zucc. has phase characteristics over time, which can improve the soil physicochemical properties, enzyme activity and microbial diversity, thus promoting the growth of T. cuspidata. Based on the irrigation of exogenous allelochemicals, changes in soil fertility (soil physical and chemical properties, soil enzyme activity and soil microelement content) were observed in response to variations in allelochemicals during five phases of irrigation: initial disturbance phase (0-2 d), physiological compensation phase (2-8 d), screening phase (8-16 d), restore phase (16-32 d) and maturity phase (32-64 d), which was consistent with the response of soil microorganisms. The allelopathic response of growth physiological indexes of T. cuspidata, however, exhibited a slight lag behind the soil fertility, with distinct phase characteristics becoming evident on the 4th day following irrigation of allelochemicals. The findings demonstrated that the allelochemicals released by the root of F. carica induced a synergistic effect on soil fertility and microorganisms, thereby facilitating the growth of T. cuspidata. This study provides a comprehensive elucidation of the phased dynamic response-based allelopathic mechanism employed by F. carica to enhance the growth of T. cuspidata, thus establishing a theoretical basis for optimizing forest cultivation through allelopathic pathways., Competing Interests: Declaration of competing interest All authors declare that they have no known competing financial interests or personal relationships that could have appeared to influence the work reported in this paper., (Copyright © 2024 Elsevier B.V. All rights reserved.)

The invasion of alien plant and the pollution caused by soil microplastics have emerged as significant ecological threats. Recent studies have demonstrated aggravating effect of non-biodegradable microplastics on plant invasion. However, the impact of biodegradable microplastics (BMPs) on plant invasion remains unclear. Therefore, it is imperative to explore the impact of BMPs on plant invasion. In this study, a 30-day potting experiment with Trifolium repens L. (an invasive plant) and Oxalis corniculata L. (a native plant) was conducted to evaluate the influence of BMPs on T. repens's invasion. The findings revealed that BMPs results in a reduction in available N and P contents, thereby facilitating the colonization of arbuscular mycorrhizal fungi on T. repens 's roots. Consequently, T. repens adjusted its N and P foraging strategy by increasing P absorption ratio, and enhancing the accumulation of N and P in leaves. This ultimately led to the decrease of relative neighbor effect index of T. repens, indicating an aggravated invasion by T. repens. This study significantly enhances and expands the understanding of mechanisms by which microplastics aggravate plant invasion., Competing Interests: Declaration of Competing Interest The authors declare that they have no known competing financial interests or personal relationships that could have appeared to influence the work reported in this paper., (Copyright © 2024 Elsevier B.V. All rights reserved.)

The migration and transformation of allelochemicals are important topics in the exploration of allelopathy. Current research on the migration of allelochemicals mostly uses soil column and thin layer methods and verifies it by sowing plant seeds. However, traditional methods inevitably ignore the flux caused by the movement of allelochemicals carried by water. In fact, the flux determines the amount of allelochemicals that directly affect plants. In this work, a method of microdialysis combined with a soil column and UPLC-MS/MS to detect the flux of allelochemicals was developed for the first time and successfully applied to the detection of five taxane allelochemicals in soil. Meanwhile, by adding taxane allelochemicals to the soil and detecting their transformation products using UPLC-MS/MS, the half-life of taxane in the soil was determined, and the transformation pathway of taxane allelochemicals in the soil was further speculated.

Chlorogenic acid (CGA), known as an important natural antioxidative compound in Ficus carica L, has valuable application prospects on health food, functional food, nutrition and dietary formulations. In this study, a surface multiple imprinting layers membrane (SMILM) was developed and applied to separate CGA from F. carica. Two different imprinting layers were integrated onto the membrane surface in sequence. The first imprinting layer was formed by dopamine polymerization and the second imprinting layer was fabricated by atom transfer radical polymerization (ATRP) and boronate affinity. The prepared SMILM with well-oriented multiple recognition sites exhibited high adsorption capacity (52.08 mg·g -1 in 60 min) for CGA and specific selectivity with imprinting factor (IF) of 3.06. Furthermore, the recognition mechanism of SMILM was clarified by molecular simulation and NMR. The SMILM was successfully applied to separate CGA from the fruits, peels and leaves of F. carica with recoveries of 90.22, 83.31 and 84.95 %, respectively., Competing Interests: Declaration of Competing Interest The authors declare that they have no known competing financial interests or personal relationships that could have appeared to influence the work reported in this paper., (Copyright © 2023 Elsevier Ltd. All rights reserved.)

This study introduced the preparation of a novel HOF-loaded PU sponge (HOF-3 @ PU) composite for the sustainable and efficient purification of catalpol and ajugol from Rehmannia glutinosa leaves for the first time. HOF-3 was selected as the best adsorbent from the five synthesised HOFs. HOF-3 @ PU was prepared by ultrasonication, and the loading conditions were optimised. The results showed that the optimum adsorption conditions are as follows: adsorption liquid volume: 160 mL, flow rate: 3.0 mL/min, pH: 6.0, concentration: 1.62 mg/mL for catalpol and 2.18 mg/mL for ajugol. The optimum desorption conditions are as follows: desorption agent: ethanol, volume fraction: 60%, flow rate: 2.0 mL/min, volume: 300 mL and pH: 6.0. Under the optimal process conditions, the adsorption capacities of catalpol and ajugol were 75.62 and 68.41 mg/g, the desorption rates were 78.5 and 86.4% and the purities were 38.7 and 36.5%, respectively.

ES contains compounds known to have significant anti-fatigue activity. In recent years, it has received extensive attention because it is efficient. However, its active ingredients on antifatigue effect are still unclear. This study attempts to establish the spectrum-effect relationship of ES antifatigue activity to screen the effective components. The results showed that the similarity of 15 ES fingerprints obtained by LC-MS/MS was 0.533-0.992, and the chemical structures of 22 common peaks were identified. The anti-fatigue activity of 15 batches of ES was characterized by forced swimming test of mice and quantified by CAFI, among which S4, S1 and S5 had better activity. 9 components (caffeic acid, 5-(4- O -β-D-glucosylferoyl)-quinic acid, (±)13-HODE, isofraxidin, eleutheroside E, syringin, pinoresinol diglucoside or its isomer, 7,8-dihydrodehydrocarbinol alcohol-4- O- β-D-glucoside, secoisolariciresinol-4- O -β-D-glucoside) highly related to anti-fatigue activity may be the effective components of ES .

A kind of hydroxycamptothecin (HCPT) hybrid molecularly imprinted polymer (AT/MA-HMIPs) with high selectivity and hard silicon skeleton was successfully prepared based on double hybrid monomers. The relationship between templates and functional monomers was studied through computer molecular simulation and experiments. Three single-monomer molecularly imprinted polymers were prepared as controls. The Langmuir isotherm and pseudo-second-order kinetic models were found to fit well with the adsorption results. The maximum adsorption capacity was 18.79 mg/g, and equilibrium was reached within 20 min. Moreover, it shows excellent selectivity (imprinting factor is 10.73) and good recoverability (after 10 adsorption-desorption cycles, the adsorption capacity only decreases by 7.75%) for HCPT. The purity of HCPT can reach 80.86% after being put into a solid phase extraction column and used in an actual sample, and the yield was 61.43%. This study lays the fundament for the development of excellent HCPT molecularly imprinted composites., (© 2023. The Author(s), under exclusive licence to Springer-Verlag GmbH Austria, part of Springer Nature.)

In recent years, it has been found that changing ambient conditions (CO 2 /N 2 , temperature, pH) can trigger a switchable phase transition of deep eutectic solvents, and such solvents are known as responsive deep eutectic solvents. In this work, we present the development history, properties, and preparation of responsive deep eutectic solvents, followed by the application of responsive deep eutectic solvents in the extraction and separation of bioactive compounds are presented. Importantly, the mechanism of responsive deep eutectic solvents in the extraction of bioactive compounds is discussed. Finally, the challenges and prospects of responsive deep eutectic solvents in the extraction and separation of bioactive compounds are proposed. Responsive deep eutectic solvents are considered green and efficient solvents. Some methods for extraction and separation of bioactive compounds by responsive deep eutectic solvents can increase the possibility of recycling the deep eutectic solvents, and provide higher efficiency in the extraction and separation field. It is hoped that this will provide a reference for the green and sustainable extraction and separation of various bioactive compounds., (© 2023 Wiley-VCH GmbH.)

A novel endophytic fungus producing beta-glucosidase was isolated and characterized from pigeon pea (Cajanus cajan [L.] Millsp.), which has excellent properties in converting ginsenoside Rb1 to ginsenoside Rd in Panax notoginseng. According to the 16S rDNA gene sequence, the G11-7 strain was identified as Fusarium proliferatum, and the accession number KY303906 was confirmed in GenBank. The G11-7 immobilized spores, in which the activity of beta-glucosidase could reach 0.95 U/mL, were co-cultured with P. notoginseng plant material to obtain a continuous beta-glucosidase supply for the biotransformation of ginsenoside Rb1 to Rd. Under the liquid-solid ratio (20:1), initial pH (6.0), and temperature (30 °C) constituents, the maximum ginsenoside Rd yield was obtained as 9.15 ± 0.65 mg/g, which was 3.67-fold higher than that without fungal spore co-culture (2.49 ± 0.98 mg/g). Furthermore, immobilized G11-7 spores showed significant beta-glucosidase producing ability which could be recovered and reused for 6 cycles. Overall, these results suggested that immobilized G11-7 offered a promising and effective approach to enhance the production of ginsenoside Rd for possible nutraceutical and pharmaceutical uses., (© 2022. Institute of Microbiology, Academy of Sciences of the Czech Republic, v.v.i.)

To explore the effects of ultraviolet light supplementation on the photosynthetic characteristics and content of secondary metabolites in the leaves of Eucommia ulmoides Oliver ( E. ulmoides ), the effects of supplementary UV-B (sUV-B) radiation on the medicinally active components of E. ulmoides were comprehensively evaluated. In our study, we selected leaves of five-year-old E. ulmoides seedlings as experimental materials and studied the effect of supplemental ultraviolet-B (sUV-B) radiation on growth, photosynthetic parameters, photosynthetic pigments, fluorescence parameters, and secondary metabolites of E. ulmoides using multivariate analysis. The results showed that the leaf area and the number of branches increased after sUV-B radiation, which indicated that sUV-B radiation was beneficial to the growth of E. ulmoides . The contents of chlorophyll a and chlorophyll b increased by 2.25% and 4.25%, respectively; the net photosynthetic rate increased by 5.17%; the transpiration rate decreased by 35.32%; the actual photosynthetic efficiency increased by 10.64%; the content of the secondary metabolite genipin increased by 12.9%; and the content of chlorogenic acid increased by 75.03%. To identify the genes that may be related to the effects of sUV-B radiation on the growth and development of E. ulmoides leaves and important secondary metabolites, six cDNA libraries were prepared from natural sunlight radiation and sUV-B radiation in E. ulmoides leaves. Comparative analysis of both transcriptome databases revealed a total of 3698 differential expression genes (DEGs), including 1826 up-regulated and 1872 down-regulated genes. According to the KOG database, the up-regulated unigenes were mainly involved in signal transduction mechanisms [T] and cell wall/membrane biogenesis [M]. It is also involved in plant hormone signal transduction and phenylpropanoid biosynthesis metabolic pathways by the KEGG pathway, which might further affect the physiological indices and the content of chlorogenic acid, a secondary metabolite of E. ulmoides . Furthermore, 10 candidate unigenes were randomly selected to examine gene expression using qRT-PCR, and the six libraries exhibited differential expression and were identical to those obtained by sequencing. Thus, the data in this study were helpful in clarifying the reasons for leaf growth after sUV-B radiation. And it was beneficial to improve the active components and utilization rate of E. ulmoides after sUV-B radiation.

Background: Velvetleaf (Abutilon theophrasti Medik.), primarily a cropland weed, exerts adverse impacts on the productivity of various crops, including soybean (Glycine max L.), wheat (Triticum aestivum L.), and maize (Zea mays L.), by hindering their vegetative growth. However, the interference mechanism of velvetleaf on the three crops remains unclear., Results: The inhibitory effect of velvetleaf water extract on the germination and growth of soybean, wheat, and maize was determined in pot experiments and field trials. Four phenolic acids were identified as allelochemicals: protocatechuic acid (PA), gallic acid (GA), chlorogenic acid (CHA), and vanillic acid (VA). These allelochemicals were detected in different parts (leaves, roots, and stems) of velvetleaf, and in the rhizosphere soil of tested crops over the range of 1.19-556.23 μm kg -1 . These allelochemicals were administered in approximate concentrations as in velvetleaf roots and rhizosphere soil, and their effects varied with crop species and velvetleaf parts. The allelochemicals generally had low-dose stimulation and high-dose inhibition effects on the growth of soybean, wheat, and maize. Furthermore, the biomass distribution of these crops was affected by allelochemicals in the soil. In field trials, the allelochemicals significantly (P < 0.05) inhibited the growth of all tested crops over the whole growth period, and PA showed a significant (P < 0.05) inhibitory effect on the yield of soybean, wheat, and maize., Conclusion: GA, PA, CHA, and VA in velvetleaf aqueous extracts were identified as allelochemicals that play an inhibitory role on three crops. © 2022 Society of Chemical Industry., (© 2022 Society of Chemical Industry.)

In this study, ethylenediaminetetraacetic acid (EDTA) disodium was first chosen as catalyst to convert psoralenoside (PO) to psoralen (PSO) for increasing the extraction yield of PSO. An efficient continuous system for synchronous transformation and extraction of PSO from fig leaves applying microwave-assisted EDTA disodium (MAE-EDTA) was developed. The optimal MAE-EDTA condition was obtained: EDTA disodium concentration of 0.07 mol·L -1 , ethanol volume fraction of 56%, extraction time of 16 min, and extraction temperature of 70 °C by single factor experiments and response surface method (RSM). Under the optimal condition, the yield of PSO reached 27.24 mg·g -1 . Compared with microwave-assisted ethanol extraction (MAE) and reflux extraction (RE), the yield of PSO by MAE-EDTA is 2.03-fold higher than RE and 1.70-fold higher than MAE. Therefore, MAE-EDTA is an efficient method for extracting PSO from fig leaves, and it might provide references for the extraction of PSO from other medicinal plants.

In this study, a switchable temperature-responsive ionic liquid-based surfactant-free microemulsion (TRIL-SFME) for extraction and in-situ separation of hydrophilic and lipophilic compounds from Camptotheca acuminata was firstly developed and systematically characterized. This TRIL-SFME was obtained using 1-hexyl-3-methylimidazolium tetrafluoroborate ([HMIM][BF 4 ]), 1,2-propanediol and H 2 O. The prepared TRIL-SFME presented low viscosity and rapid response to temperature. Firstly, the effect of temperatures on TRIL-SFME phase behavior was studied followed by determination of effect of liquid/solid ratio and extraction time on the extraction yields of the targeted compounds. The TRIL-SFME demulsified rapidly by thermal stimulus, resulting in in-situ separation and enrichment of compounds with varying polarity. The results of present study revealed that TRIL-SFME had higher extraction yields (1.50-5.79 folds) compared to traditional solvents and individual components of TRIL-SFME. Besides, in-situ separation and enrichment of hydrophilic compounds (phenolic acids) and lipophilic compounds (alkaloids) was accomplished in short time (within 3 min) by cooling the system to 4 ℃. Furthermore, the mesoscopic behavior between TRIL-SFME and targeted compounds was simulated by dissipative particle dynamics (DPD) to explore the extraction mechanism for the first time. The results illustrated the formation of W/IL structure of TRIL-SFME and clarified solubilization mechanism of TRIL-SFME system for targeted compounds, which is related to its special "water pool" structure. This novel and switchable TRIL-SFME is an environmentally friendly and promising alternative to simultaneously extract, in-situ separate and enrich the natural active compounds with different polarity from plant matrices., Competing Interests: Declaration of Competing Interest The authors declare that they have no known competing financial interests or personal relationships that could have appeared to influence the work reported in this paper., (Copyright © 2022 Elsevier B.V. All rights reserved.)

The action of allelopathy need that allelochemicals exist in the soil and reach a certain concentration. Also, the detection of allelochemicals in the soil is one of the most important research topics in the process of exploring allelopathy. To solve the problem of the simultaneous detection of allelochemicals with low concentrations and different polarities, a novel strategy for the quick detection of the allelochemicals in Taxus soil by microdialysis combined with UPLC-MS/MS on the basis of in situ detection without destroying the original structure of soil was developed for the first time in the work. The dialysis conditions were optimized by the Box-Behnken design (BBD): 70% methanol, 3 μL/min flow rate, and 3 cm long membrane tube. A reliable UPLC-MS/MS program was systematically optimized for the simultaneous detection of nine allelochemicals with different polarities. The results proved the differences in the contents and distributions of nine allelochemicals in three different Taxus soils.

Biomimetic nanozyme with natural enzyme-like activities has drawn extensive attention in cancer therapy, while its application was hindered by the limited catalytic efficacy in the complicated tumor microenvironment (TME). Herein, a hybrid biomimetic nanozyme combines polydopamine-decorated CuO with a natural enzyme of glucose oxidase (GOD), among which CuO is endowed with a high loading rate (47.1%) of GOD due to the elaborately designed hollow mesoporous structure that is constructed to maximize the cascade catalytic efficacy. In the TME, CuO could catalyze endogenous H 2 O 2 into O 2 for relieving tumor hypoxia and improving the catalytic efficacy of GOD. Whereafter, the amplified glucose oxidation induces starvation therapy, and the generated H 2 O 2 and H + enhance the catalytic activity of CuO. Significantly, the tumor-specific chemodynamic therapy (CDT) could be realized when CuO degraded into Cu 2+ in acidic and reductive TME. Furthermore, the photothermal therapy with high photothermal conversion efficiency (30.2%) is achieved under NIR-II laser (1064 nm) excitation, which could reinforce the generation of reactive oxygen species (•OH and •O 2 - ). The TME initiates the biochemical reaction cycle of CuO, O 2 , and GOD, which couples with an NIR-II-induced thermal effect to realize O 2 -promoted starvation and photothermal-chemodynamic combined therapy. This hybrid biomimetic nanozyme enlightens the further development of nanozymes in multimodal cancer therapy.

Fig ( Ficus carica L.) leaves are produced each year and often disposed, resulting in a waste of resources. Fig waste leaves are rich in flavonoids, which have strong antioxidant activity; however, the variety and chemical structure of antioxidants in fig leaves have not been reported in detail. To take full advantage of fig waste leaves, antioxidant capacity of different extracts (petroleum ether, ethyl acetate, and water) was evaluated by 1, 1-diphenyl-2-picrylhydrazyl (DPPH), 2,2'-azino-bis(3-ethylbenzothiazoline-6-sulfonic) acid (ABTS), and ferric-ion-reducing antioxidant power (FRAP) methods. The results showed that flavonoids in ethyl acetate extraction had the highest content (83.92 ± 0.01 mg/g), maximum DPPH scavenging activity (IC 50 0.54 mg/mL), highest ABTS scavenging rate (80.28%), and FRAP (3.46 mmol/g). Furthermore, an HPLC-QTOF-MS/MS-DPPH method was developed to identify 11 flavonoids in fig waste leaves. This rapid and efficient method can not only be used for screening the antioxidant components in fig waste leaves, but also can be combined with mass spectrometry to identify the compounds with antioxidant capacity. There are three flavonoids with significant antioxidant capacity, which are 3-O-(rhamnopyranosyl-glucopyranosyl)-7-O-(glucopyranosyl)-quercetin, isoschaftoside, and rutin. The results confirmed that fig waste leaves contain a variety of antioxidant components, which contributed to increase the value of fig waste leaves as antioxidants.

A quality assessment method based on quantitative analysis of multi-components by single marker (QAMS) and fingerprint was constructed from 15 batches of dandelion ( Taraxacum mongolicum ), using multivariate chemometric methods (MCM). MCM were established by hierarchical cluster analysis (HCA) and factor analysis (FA). HCA was especially performed using the R language and SPSS 22.0 software. The relative correction factors of chlorogenic acid, caffeic acid, p-coumaric acid, luteolin and apigenin were calculated with cichoric acid as a reference, and their contents were determined. The differences between external standard method (ESM) and QAMS were compared. There was no significant difference ( t -test, p > 0.05) in quantitative determination, proving the consistency of the two methods (QAMS and ESM). Dandelion material from Yuncheng, Shandong was used as a reference chromatogram. The fingerprints in 15 batches of dandelion were established by HPLC analysis. The similarity of the fingerprints in different batches of dandelion material was greater than or equal to 0.82. A total of 10 common peaks were identified. This strategy is simple, rapid and efficient in multiple component detection of dandelion. It is beneficial in simplifying dandelion's quality control processes and providing references to enhance quality control for other herbal medicines., (© 2021 The Authors.)

Metal-coordinated supramolecular nanoassemblies have recently attracted extensive attention as materials for cancer theranostics. Owing to their unique physicochemical properties, metal-coordinated supramolecular self-assemblies can bridge the boundary between traditional inorganic and organic materials. By tailoring the structural components of the metal ions and binding ligands, numerous multifunctional theranostic nanomedicines can be constructed. Metal-coordinated supramolecular nanoassemblies can modulate the tumor microenvironment (TME), thus facilitating the development of TME-responsive nanomedicines. More importantly, TME-responsive organic-inorganic hybrid nanomaterials can be constructed in vivo by exploiting the metal-coordinated self-assembly of a variety of functional ligands, which is a promising strategy for enhancing the tumor accumulation of theranostic molecules. In this review, recent advancements in the design and fabrication of metal-coordinated supramolecular nanomedicines for cancer theranostics are highlighted. These supramolecular compounds are classified according to the order in which the coordinated metal ions appear in the periodic table. Furthermore, the prospects and challenges of metal-coordinated supramolecular self-assemblies for both technical advances and clinical translation are discussed. In particular, the superiority of TME-responsive nanomedicines for in vivo coordinated self-assembly is elaborated, with an emphasis on strategies that enhance the accumulation of functional components in tumors for an ideal theranostic outcome., (© 2021 The Authors. Advanced Science published by Wiley-VCH GmbH.)

A comprehensive method for the evaluation of Acanthopanax senticosus (AS) was established by the quantitative analysis of multiple components by single marker (QAMS), fingerprint, similarity analysis (SA), hierarchical cluster analysis (HCA), and factor analysis (FA) based on high performance liquid chromatography (HPLC). A total of 27 common peaks were identified in the standard fingerprint of 20 batches of AS from different regions in China, of which 8 peaks were identified as protocatechuic acid, syringin, chlorogenic acid, caffeic acid, eleutheroside E, hyperoside, isofrqxidin, and acacetin, and the concentrations of these eight components were determined simultaneously by QAMS. The results showed that the QAMS method was effective and feasible compared with the external standard method (ESM) (RD < 3.3 %, P ≤ 0.01). Sample 1 (S1) was used as the reference chromatogram, the similarity of other samples was between 0.765 and 0.968. Through HCA, AS could be mainly divided into two production areas, the north Liaoning (including Liaoning) and the south Liaoning areas. Furthermore, FA showed that the quality of AS in the north Liaoning area was better than that in the south Liaoning area. In summary, the method established in this study can comprehensively and systematically evaluate quality differences in AS samples, and may be used to help to improve the quality control of AS., Competing Interests: Declaration of Competing Interest The authors report no declarations of interest., (Copyright © 2021 Elsevier B.V. All rights reserved.)

In the present study, an efficient ultrasonic/microwave-assisted extraction (UMAE) procedure for the polysaccharides from the fruit of Camptotheca acuminata (CAFP) was investigated and optimized. Under the optimum conditions (ratio of liquid to raw material 30 mL/g, microwave irradiation time of 20 min, microwave irradiation power of 570 W and a fixed ultrasonic power of 50 W obtained by the response surface analysis with Box-Behnken design, satisfactory yields of CAFP (6.81 ± 0.04%) were achieved. The development UMAE technique produced higher yields in a shorter time than conventional hot water extraction (HWE): 20 vs. 120 min. In addition, in vivo CAFP at suitable dose is effective on H22 murine hepatoma strains, and CAFP significantly inhibited the proliferation of human oral carcinoma KB, pancreatic carcinoma BXCP-3 and gastric carcinoma SGC-7901 cells in vitro, indicating CAFP might be suitable for nature antitumor therapeutic agent development., (Copyright © 2018. Published by Elsevier Ltd.)

Volatile essential oils (EOs), non-volatile rutin (RU), quercetin (QU), kaempferol (KA) and isorhamnetin (IS) were effectively extracted and isolated from seabuckthorn ( Hippophae rhamnoides L.) leaves by ionic liquid-based ultrasound/microwave-assisted simultaneous distillation extraction (ILUMASDE). After optimization by response surface methodology, EOs, RU, QU, KA and IS were separated under the following optimum conditions: an ionic liquid of 1.0 M 1-butyl-3-methyl imidazole bromine salt ([C4mim]), liquid/solid ratio of 12 ml g -1 , extraction time of 34 min, microwave power of 540 W and a fixed ultrasonic power of 50 W. Under the optimized conditions of ILUMASDE, the extraction yields of RU, QU, KA, IS and EOs were 9.18 ± 0.35, 5.52 ± 0.23, 3.03 ± 0.11, 5.64 ± 0.24 mg g -1 and 0.095 ± 0.004%, respectively. The yield of EOs obtained using ILUMASDE was 1.07-fold higher than that obtained by conventional hydrodistillation extraction (HDE). In addition, the components of the EOs obtained using ILUMASDE and HDE were similar. The extraction yields of RU, QU, KA, IS obtained by ILUMASDE were 1.03-1.35-fold higher than that obtained by the ethanol ultrasonic-assisted extraction (EUAE), ionic liquid-based ultrasonic-assisted extraction (ILUAE) and ionic liquid-based microwave-assisted extraction (ILMAE). And the extraction time used by ILUMASDE was 34 min, which is 14.17%, 56.67%, 56.67% and 85.00% less than those used by HDE, EUAE, ILUAE and ILMAE, respectively. Therefore, ILUMASDE can be considered a rapid and efficient method for extracting flavonoids and EO from seabuckthorn ( Hippophae rhamnoids L.) leaves., Competing Interests: The authors declare no competing interests.

A novel and efficient ultrasonic assisted-reflux synergistic extraction (UARSE) method for extracting camptothecin (CPT) and betulinic acid (BA) from Camptotheca acuminata Decne. fruits has been developed in this study. The advantages of the ultrasonic and reflux extraction methods have been combined in the UARSE method and used to extract CPT and BA for the first time. The parameters influencing the efficiency of UARSE were optimized using the Box-Behnken design (BBD) to obtain the maximum extraction yield of CPT and BA. The optimal extraction conditions were as follows: 225 W for the ultrasonic power; 24 min for the extraction time; and 32 mL/g for the liquid-solid ratio. The extraction yields obtained by UARSE were 2.386 ± 0.112 mg/g for CPT and 17.192 ± 0.808 mg/g for BA, which were 1.43-fold and 1.33-fold, respectively, higher than by using heating reflux extraction (HRE) and ultrasonic-assisted extraction (UAE). In addition, the 24-min extraction time using UARSE was 80% and 60% less than those provided by HRE and UAE, respectively. Therefore, UARSE can be considered a rapid and efficient method for extracting CPT and BA from the fruits of C. acuminata Decne., Competing Interests: The authors declare no conflict of interest.

The simultaneous ultrasonic/microwave-assisted extraction (UMAE) method is potentially useful for the extraction of polysaccharides from Taxus chinensis var. mairei fruits (TCFPs). In this study, we used a response surface methodology to identify optimal TCFPs extraction conditions. Optimal parameters were determined as follows: a liquid to raw material ratio of 33 mL/g, an extraction time of 10 min, a microwave power level of 560 W, and a fixed ultrasonic power of 50 W. Under the optimized conditions, TCFPs yields obtained by UMAE were 4.33 ± 0.15%, a 1.79-fold increase compared with conventional heating reflux extraction (HRE). In addition, the extraction time used in UMAE was shorter than that required for HRE: 10 versus 90 min. UMAE is therefore a rapid and efficient method for the extraction of TCFPs. The inhibitory effect of TCFPs on S180 tumor growth in vivo was also studied. The tumor inhibition rate of TCFPs was 76.33%, indicating a tumor-inhibiting effect. Analysis of organ weights demonstrated that TCFPs exhibited no toxicity to liver, kidney, spleen, heart, or lung relative to a positive control group. TCFPs thus show antitumor activity with no organ toxicity., (Copyright © 2015 Elsevier B.V. All rights reserved.)

We evaluated an ionic-liquid-based ultrasound/microwave-assisted extraction method for the extraction of 2,4-dihydroxy-7-methoxy-1,4-benzoxazin-3-one and 6-methoxy-benzoxazolin-2-one from etiolated maize seedlings. We performed single-factor and central composite rotatable design experiments to optimize the most important parameters influencing this technique. The best results were obtained using 1.00 M 1-octyl-3-methylimidazolium bromide as the extraction solvent, a 50°C extraction temperature, a 20:1 liquid/solid ratio (mL/g), a 21 min treatment time, 590 W microwave power, and 50 W fixed ultrasonic power. We performed a comparison between ionic-liquid-based ultrasound/microwave-assisted extraction and conventional homogenized extraction. Extraction yields of 2,4-dihydroxy-7-methoxy-1,4-benzoxazin-3-one and 6-methoxy-benzoxazolin-2-one by the ionic-liquid-based ultrasound/microwave-assisted extraction method were 1.392 ± 0.051 and 0.205 ± 0.008 mg/g, respectively, which were correspondingly 1.46- and 1.32-fold higher than those obtained by conventional homogenized extraction. All the results show that the ionic-liquid-based ultrasound/microwave-assisted extraction method is therefore an efficient and credible method for the extraction of 2,4-dihydroxy-7-methoxy-1,4-benzoxazin-3-one and 6-methoxy-benzoxazolin-2-one from maize seedlings., (© 2014 WILEY-VCH Verlag GmbH & Co. KGaA, Weinheim.)

In this study, epigallocatechin gallate (EGCG) palmitate was synthesized and its anti-porcine reproductive and respiratory syndrome virus (PRRSV) activity was studied. Specifically, EGCG palmitate was evaluated for its ability to inhibit PRRSV infection in MARC-145 cells when administered as pre-, post-, or co-treatment. EGCG and ribavirin were used as controls. The results showed that a 50% cytotoxic concentration (CC50) of EGCG, EGCG palmitate, and ribavirin was achieved at 2,359.71, 431.42, and 94.06 μM, respectively. All three drugs inhibited PRRSV in a dose-dependent manner regardless of the treatment protocol. EGCG palmitate exhibited higher cytotoxicity than EGCG, but lower cytotoxicity than ribavirin. EGCG palmitate anti-PRRSV activity was significantly higher than that of EGCG and ribavirin, both as pre-treatment and post-treatment. Under the former conditions and a tissue culture infectious dose of 10 and 100, the selectivity index (SI) of EGCG palmitate in the inhibition of PRRSV was 3.8 and 2.9 times higher than that of ribavirin when administered as a pre-treatment, while the SI of EGCG palmitate in the inhibition of PRRSV was 3.0 and 1.9 times higher than ribavirin when administered as a post-treatment. Therefore, EGCG palmitate is potentially effective as an anti-PRRSV agent and thus of interest to the pharmaceutical industry.

Total polyphenol content, catechins content, and antioxidant capacities of green, dark, oolong, and black teas made from Camellia sinensis in China were evaluated. The total polyphenol content of 20 samples of tea was in the range of 7.82-32.36%. Total catechins content was in the range of 4.34-24.27%. The antioxidant capacity of tea extract was determined by the oxygen radical absorbance capacity (ORAC) test and the 1,1-diphenyl-2-picrylhydrazyl (DPPH) radical-scavenging test. Total polyphenol content, catechins content, and antioxidant capacity decreased in the following order: green > oolong > black > dark tea. A positive correlation existed between the antioxidant capacity and total polyphenol content or catechins content (R (2) = 0.67-0.87). The antioxidant capacities of five major catechins (epigallocatechin gallate (EGCG), epicatechin gallate (ECG), epicatechin, epigallocatechin, and catechin) were determined by online HPLC DPPH radical-scavenging; the antioxidant activity of tea was mainly attributed to the esterified catechins (EGCG or ECG).

An ionic liquids based simultaneous ultrasonic and microwave assisted extraction (ILs-UMAE) method has been proposed for the extraction of rutin (RU), quercetin (QU), from velvetleaf leaves. The influential parameters of the ILs-UMAE were optimized by the single factor and the central composite design (CCD) experiments. A 2.00 M 1-butyl-3-methylimidazolium bromide ([C4mim]Br) was used as the experimental ionic liquid, extraction temperature 60°C, extraction time 12 min, liquid-solid ratio 32 mL/g, microwave power of 534 W, and a fixed ultrasonic power of 50 W. Compared to conventional heating reflux extraction (HRE), the RU and QU extraction yields obtained by ILs-UMAE were, respectively, 5.49 mg/g and 0.27 mg/g, which increased, respectively, 2.01-fold and 2.34-fold with the recoveries that were in the range of 97.62-102.36% for RU and 97.33-102.21% for QU with RSDs lower than 3.2% under the optimized UMAE conditions. In addition, the shorter extraction time was used in ILs-UMAE, compared with HRE. Therefore, ILs-UMAE was a rapid and an efficient method for the extraction of RU and QU from the leaves of velvetleaf.

In the present study, the main natural estrogen-agonist/antagonist from Pigeonpea roots was studied by the estrogen receptor α-dependent signaling pathway in human prostate cancer cell. First, the natural products with estrogenic activity in Pigeonpea roots were screened by pER8-GFP transgenic Arabidopsis, and cajanol (5-hydroxy-3-(4-hydroxy-2-methoxyphenyl)-7-methoxychroman-4-one) was confirmed as the active compound. Further study showed that cajanol significantly arrested the cell cycle in the G1 and G2/M phase and induced nuclei condensation, fragmentation and the formation of apoptotic bodies. Western blotting showed that cajanol modulated the ERα-dependent PI3K pathway and induced the activation of GSK3 and CyclinD1 closely following the profile of PI3K activity. Based on above results, we proposed a mechanism through which cajanol could inhibit survival and proliferation of estrogen-responsive cells (PC-3 cells) by interfering with an ERα-associated PI3K pathway, following a process that could be dependent of the nuclear functions of the ERα. Above all, we conclude that cajanol represents a valuable natural phytoestrogen source and may potentially be applicable in health food industry., (Copyright © 2013 John Wiley & Sons, Ltd.)

An ionic liquids-based ultrasonic-assisted extraction (ILUAE) method was successfully developed for extracting eleutheroside B and E from Radix Acanthopanax senticosus. Thirteen 1-alkyl-3-methylimidazolium ionic liquids with different cations and anions were investigated and 1-butyl-3-methylimidazolium bromide ([C4mim]Br) solution was selected as the solvent. The conditions for ILUAE, including the ionic liquid concentration, soaking time, ultrasonic power, ultrasonic time, solid-liquid ratio and number of extraction cycles, were optimized. With the proposed method, the energy consumption time was reduced to 30 min, whereas conventional method requires about 4h. The proposed method had good recovery (97.96-103.39%) and reproducibility (RSD, n=5; 3.3% for eleutheroside B, 4.6% for eleutheroside E). ILUAE was an efficient, rapid and simple sample preparation technique that showed high reproducibility and was environmental friendly., (Copyright © 2013 Elsevier Ltd. All rights reserved.)

Cajaninstilbene acid (CSA), an active compound separated from pigeon pea leaves, possesses the highly efficient antioxidant activities. Transcription factor nuclear factor-erythroid 2-related factor 2 (Nrf2) is an important regulator of cellular oxidative stress. This study examined the role of Nrf2 in CSA-mediated antioxidant effects on human hepatocarcinoma (HepG2) cell line. The generation of reactive oxygen species (ROS) upon H2O2 and CSA treatment was lower than that of H2O2 alone. CSA activated Nrf2 as evaluated by Western blotting. A luciferase reporter assay also demonstrated that CSA-activated signaling resulted in the increased transcriptional activity of Nrf2 through binding to the antioxidant response element (ARE) enhancer sequence. Our study indicated that treatment of HepG2 cells with CSA induces Nrf2-dependent ARE activity and gene expression of heme oxygenase-1 (HO-1), NAD(P)H quinone oxidoreductase 1 (NQO1), and glutamate-cysteine ligase modifier subunits by activation of PI3K/AKT, ERK and JNK signaling pathways. Inhibition of Nrf2 by siRNA reduced CSA-induced upregulation of these Nrf2-related enzymes. These results suggest that the Nrf2/ARE pathway plays an important role in the regulation of CSA-mediated antioxidant effects in HepG2 cells., (Crown Copyright © 2013. Published by Elsevier Ireland Ltd. All rights reserved.)

Dihydroquercetin (DHQ) is a well-known antioxidant agent. In the present investigation, we reported for the first time that DHQ stimulates the expression of phase II detoxifying enzymes through the Nrf2-dependent signaling pathway. The IC50 values of DHQ for reduction of 2,2-diphenyl-1-picrylhydrazol (DPPH), reducing power assay, lipid peroxidation assay, and xanthine oxidase inhibition were 5.96, 4.31, 2.03, and 13.24 μM, respectively. DHQ possessed considerable protective activity from oxidative DNA damage. A luciferase reporter assay also demonstrated that DHQ-activated signaling resulted in the increased transcriptional activity of Nrf2 through binding to the ARE (antioxidant response element) enhancer sequence. Furthermore, Western blotting and luciferase assay revealed DHQ activated ERK1/2, Akt, and JNK signaling pathways, subsequently leading to Nrf2 nuclear translocation. DHQ upregulated the Nrf2-related antioxidant genes heme oxygenase-1 (HO-1), NAD(P)H quinone oxidoreductase-1 (NQO1), and glutamate-cysteine ligase modifier subunits. Inhibition of Nrf2 by siRNA reduced DHQ-induced upregulation of these antioxidant genes.

An efficient homogenate extraction technique was employed for extracting shikonin from Arnebia euchroma. The homogenate extraction procedure was optimized and compared with other conventional extraction techniques. The proposed method gave the best result with the highest extraction efficiency in the shortest extraction time. Based on single-factor experiments, a three-factor-three-level experimental design has been developed by Box-Behnken design. The optimal conditions were 78% ethanol as solvent, homogenate extraction time of 4.2 min, 10.3 liquid to solid ratio and two extraction cycles. Moreover, the proposed method was validated by stability, repeatability and recovery experiments. The developed homogenate extraction method provided a good alternative for the extraction of shikonin from A. euchroma. The results indicated that the proposed homogenate extraction was a convenient, rapid and efficient sample preparation technique and was environmental friendly. Furthermore, homogenate extraction has superiority in the extraction of thermally sensitive compounds from plant matrices.

Cortex cinnamomi is associated with many health benefits and is used in the food and pharmaceutical industries. In this study, an efficient ionic liquid-based microwave-assisted simultaneous extraction and distillation (ILMSED) technique was used to extract cassia oil and proanthocyanidins from Cortex cinnamomi; these were quantified by gas chromatography/mass spectrometry (GC-MS) and the vanillin-HCl colorimetric method, respectively. 0.5M 1-butyl-3-methylimidazolium bromide ionic liquid was selected as solvent. The optimum parameters of dealing with 20.0 g sample were 230 W microwave irradiation power, 15 min microwave extraction time and 10 liquid-solid ratio. The yields of essential oil and proanthocyanidins were 1.24 ± 0.04% and 4.58 ± 0.21% under the optimum conditions. The composition of the essential oil was analysed by GC-MS. Using the ILMSED method, the energy consumption was reduced and the extraction yields were improved. The proposed method was validated using stability, repeatability, and recovery experiments. The results indicated that the developed ILMSED method provided a good alternative for the extraction of both the essential oil and proanthocyanidins from Cortex cinnamomi., (Copyright © 2012 Elsevier Ltd. All rights reserved.)

In this work, a multivariate study based on Box-Behnken Design was used to evaluate the influence of three major variables affecting the performance of the extraction process of Schisandra chinensis anthocyanins. The optimum parameters were 5.5 h extraction time; 1:19 solid-liquid ratio and 260 r/min stirring rate, respectively. The extraction yield of anthocyanins was 29.06 mg/g under the optimum conditions. Moreover, many factors on the impact of heating, ultrasound, microwave treatment and ultraviolet irradiation on content and color stability of anthocyanins from Schisandra chinensis fruit were investigated. The results show that thermal degradation reaction of anthocyanins complies with the first order reaction kinetics, and the correlation coefficient is greater than 0.9950 at 40-80°C. Ultrasound and microwave treatment has little effect on the stability of anthocyanins, and the extraction time of ultrasound and microwave should be no more than 60 min and 5 min, respectively. The anthocyanins degradation effect of UVC ultraviolet radiation is greater than UVA and UVB; after 9 h ultraviolet radiation, the anthocyanins content degradation of UVC is 23.9 ± 0.7%, and the ∆E* was changed from 62.81 to 76.52 ± 2.3. Through LC-MS analysis, the major composition of Schisandra chinensis anthocyanins was cyanidin-3-O-xylosylrutinoside.

The aim of this study was to investigate the antioxidant and free-radical scavenging activity of extract and fractions from various parts of Elsholtzia ciliata. The inflorescences, leaves, stems and roots of E. ciliata were extracted separately and two phenolic component enrichment methods: ethyl acetate-water liquid-liquid extraction and macroporous resin adsorption-desorption, were adopted in this study. The antioxidant activities of water extracts and fractions of E. ciliata were examined using different assay model systems in vitro. The fraction root E (purified by HPD300 macroporous resin) exhibited the highest total phenolics content (497.2 ± 24.9 mg GAE/g), accompanied with the highest antioxidant activity against various antioxidant systems in vitro compared to other fractions. On the basis of the results obtained, E. ciliata extracts can be used potentially as a ready accessible and valuable bioactive source of natural antioxidants.

In this study, novel endophytic fungi producing cajaninstilbene acid (CSA) from pigeon pea [ Cajanus cajan (L.) Millsp.] were investigated and screened. CSA has prominent pharmacological activities. A total of 110 endophytic fungi isolates were grouped into 8 genera on the basis of morphological characteristics, and CSA-producing fungi were screened by liquid chromatography-tandem mass spectrometry (LC-MS/MS). According to ITS-rDNA sequences analysis, the CSA-producing fungi were identified as Fusarium solani (ERP-07), Fusarium oxysporum (ERP-10), and Fusarium proliferatum (ERP-13), respectively. The amount of CSA produced by the ERP-13 reached 504.8 ± 20.1 μg/L or 100.5 ± 9.4 μg/g dry weight of mycelium. In a DPPH radical-scavenging assay, when the concentration of fungal CSA was 500 μg/mL, inhibition percentage could reach 80%, which was almost the same as that of standard CSA. This study first reported the natural antioxidant CSA from endophytic fungi F. solani and F. proliferatum isolated from pigeon pea.

The objective of the study was to prepare ursolic acid (UA) nanoparticles using the supercritical anti-solvent (SAS) process and evaluate its physicochemical properties and oral bioavailability. The effects of four process variables, pressure, temperature, drug concentration and drug solution flow rate, on drug particle formation during SAS process, were investigated. Particles with mean particle size ranging from 139.2±19.7 to 1039.8±65.2nm were obtained by varying the process parameters. The UA was characterised by scanning electron microscopy, X-ray diffraction, Fourier-transform infrared spectroscopy, thermal gravimetric analysis, specific surface area, dissolution test and bioavailability test. It was concluded that physicochemical properties and bioavailability of crystalline UA could be improved by physical modification, such as particle size reduction and generation of amorphous state using SAS process. Further, SAS process was a powerful methodology for improving the physicochemical properties and bioavailability of UA., (Copyright © 2011 Elsevier Ltd. All rights reserved.)

In this study, glycyrrhizic acid (GA) microparticles were successfully prepared using a supercritical anti-solvent (SAS) process. Carbon dioxide and ethanol were used as the anti-solvent and solvent, respectively. The influences of several process parameters on the mean particle size (MPS), particle size distribution (PSD) and total yield were investigated. Processed particle sizes gradually decreased as temperature and solution flow rate increased. In addition, processed particle sizes increased from 119 to 205 nm as GA concentration increased. However, CO(2) flow rate did not significantly affect particle size. The optimized process conditions were applied, those included temperature (65 °C), pressure (250 bar), CO(2) and drug solution flow rate (15 and 8 mL min(-1)), drug concentration in ethanol (20 mg mL(-1)). Microparticles with a span of PSD ranging from 95 and 174 nm, MPS of 128 nm were obtained, and total yield was 63.5%. The X-ray diffraction patterns of glycyrrhizic acid microparticles show apparent amorphous nature. Fourier transform infrared (FT-IR) spectroscopy results show that no chemical structural changes occurred. The in vitro dissolution tests showed that the GA microparticles exhibited great enhancement of dissolution performance when compared to GA original drug. Furthermore, the in vivo studies revealed that the microparticles provided improved pharmacokinetic parameter after oral administration to rats as compared with original drug., (Copyright © 2011 Elsevier B.V. All rights reserved.)

Ionic liquid based, microwave-assisted extraction (ILMAE) was successfully applied to the extraction of proanthocyanidins from Larix gmelini bark. In this work, in order to evaluate the performance of ionic liquids in the microwave-assisted extraction process, a series of 1-alkyl-3-methylimidazolium ionic liquids with different cations and anions were evaluated for extraction yield, and 1-butyl-3-methylimidazolium bromide was selected as the optimal solvent. In addition, the ILMAE procedure for the proanthocyanidins was optimized and compared with other conventional extraction techniques. Under the optimized conditions, satisfactory extraction yield of the proanthocyanidins was obtained. Relative to other methods, the proposed approach provided higher extraction yield and lower energy consumption. The Larix gmelini bark samples before and after extraction were analyzed by Thermal gravimetric analysis, Fourier-transform infrared spectroscopy and characterized by scanning electron microscopy. The results showed that the ILMAE method is a simple and efficient technique for sample preparation.

In order to screen a suitable resin for the preparative simultaneous separation and purification of syringin, eleutheroside E and isofraxidin from Acanthopanax senticosus, the adsorption and desorption properties of 17 widely used commercial macroporous resins were evaluated. According to our results, HPD100C, which adsorbs by the molecular tiers model, was the best macroporous resin, offering higher adsorption and desorption capacities and higher adsorption speed for syringin, eleutheroside E and isofraxidin than other resins. Dynamic adsorption and desorption tests were carried out to optimize the process parameters. The optimal conditions were as follows: for adsorption, processing volume: 24 BV, flow rate: 2 BV/h; for desorption, ethanol-water solution: 60:40 (v/v), eluent volume: 4 BV, flow rate: 3 BV/h. Under the above conditions, the contents of syringin, eleutheroside E and isofraxidin increased 174-fold, 20-fold and 5-fold and their recoveries were 80.93%, 93.97% and 93.79%, respectively.

The Brönsted acidic ionic-liquid [HO(3)S(CH(2))(4)mim] HSO(4), a novel dual catalyst-solvent, has been successfully applied in simultaneous microwave-assisted extraction and hydrolysis for the determination of flavonol glycosides in Ginkgo foliage. The parameters, namely the [HO(3)S(CH(2))(4)mim]HSO(4) concentration, microwave-irradiation power, microwave-irradiation time, and solid-liquid ratio, were optimized. The optimum conditions were: an amount of 1.5 M [HO(3)S(CH(2))(4)mim]HSO(4), a microwave-irradiation power of 120 W, an irradiation time of 15 min, and a solid-liquid ratio of 1:30 g/mL. Compared with traditional methods the proposed approach demonstrates higher efficiency in a shorter operating time, and is an efficient, rapid, and simple sample preparation method.

An ultrasound and microwave assisted alternant extraction method (UMAE) was applied for extracting dihydroquercetin (DHQ) from Larix gmelinii wood. This investigation was conducted using 60% ethanol as solvent, 1:12 solid to liquid ratio, and 3 h soaking time. The optimum treatment time was ultrasound 40 min, microwave 20 min, respectively, and the extraction was performed once. Under the optimized conditions, satisfactory extraction yield of the target analyte was obtained. Relative to ultrasound-assisted or microwave-assisted method, the proposed approach provides higher extraction yield. The effect of DHQ of different concentrations and synthetic antioxidants on oxidative stability in soy bean oil stored for 20 days at different temperatures (25 °C and 60 °C) was compared. DHQ was more effective in restraining soy bean oil oxidation, and a dose-response relationship was observed. The antioxidant activity of DHQ was a little stronger than that of BHA and BHT. Soy bean oil supplemented with 0.08 mg/g DHQ exhibited favorable antioxidant effects and is preferable for effectively avoiding oxidation. The L. gmelinii wood samples before and after extraction were characterized by scanning electron microscopy. The results showed that the UMAE method is a simple and efficient technique for sample preparation.

The aim of this study was to prepare micronized taxifolin powder using the supercritical antisolvent precipitation process to improve the dissolution rate of taxifolin. Ethanol was used as solvent and carbon dioxide was used as an antisolvent. The effects of process parameters, such as temperature (35-65 °C), pressure (10-25 MPa), solution flow rate (3-6 mL/min) and concentration of the liquid solution (5-20 mg/mL) on the precipitate crystals were investigated. With a lower temperature, a stronger pressure and a lower concentration of the liquid solution, the size of crystals decreased. The precipitation temperature, pressure and concentration of taxifolin solution had a significant effect. However, the solution flow rate had a negligible effect. It was concluded that the physicochemical properties and dissolution rate of crystalline taxifolin could be improved by physical modification such as particle size reduction using the supercritical antisolvent (SAS) process. Further, the SAS process was a powerful methodology for improving the physicochemical properties and radical scavenging activity of taxifolin.

Ionic liquid based, ultrasound-assisted extraction was successfully applied to the extraction of phenolcarboxylic acids, carnosic acid and rosmarinic acid, from Rosmarinus officinalis. Eight ionic liquids, with different cations and anions, were investigated in this work and [C(8)mim]Br was selected as the optimal solvent. Ultrasound extraction parameters, including soaking time, solid-liquid ratio, ultrasound power and time, and the number of extraction cycles, were discussed by single factor experiments and the main influence factors were optimized by response surface methodology. The proposed approach was demonstrated as having higher efficiency, shorter extraction time and as a new alternative for the extraction of carnosic acid and rosmarinic acid from R. officinalis compared with traditional reference extraction methods. Ionic liquids are considered to be green solvents, in the ultrasound-assisted extraction of key chemicals from medicinal plants, and show great potential.

Ionic liquid-based microwave-assisted extraction (ILMAE) has been successfully applied in extracting essential oil and four kinds of biphenyl cyclooctene lignans from Schisandra chinensis Baill. 0.25 M 1-lauryl-3-methylimidazolium bromide ionic liquid is selected as solvent. The optimum parameters of dealing with 25.0 g sample are 385 W irradiation power, 40 min microwave extraction time and 1:12 solid-liquid ratio. The yields of essential oil and lignans are 12.12±0.37 ml/kg and 250.2±38.2 mg/kg under the optimum conditions. The composition of the essential oil extracted by hydro-distillation, steam-distillation and ILMAE is analyzed by GC-MS. With ILMAE method, the energy consumption time has not only been shortened to 40 min (hydro-distillation 3.0 h for extracting essential oil and reflux extraction 4.0 h for extracting lignans, respectively), but also the extraction efficiency has been improved (extraction of lignans and distillation of essential oil at the same time) and reduces the environmental pollution. S. chinensis materials treated by different methods are observed by scanning electronic microscopy. Micrographs provide more evidence to prove that ILMAE is a better and faster method. The experimental results also indicate that ILMAE is a simple and efficient technique for sample preparation., (Copyright © 2011 Elsevier B.V. All rights reserved.)

The ground state and the spectral structure of lower-lying excited states of a dissipative two-level system coupled to a sub-Ohmic bath (s = 1/2) with nonzero bias have been studied using the unitary transformation method. By calculating the ground-state entanglement entropy, the ground-state average of σ(z)(G), and the static susceptibility of the two-level system, we explore the nature of the transition (crossover) between the delocalized and localized state of the two-level system. Furthermore, we calculate the time-dependent expectation (σ(z)(t)) and the time evolution of the entanglement entropy to show that, when the system undergoes a transition (crossover) from the delocalized to the localized state, the time evolution of the two-level system changes from coherent to decoherent dynamics.

A rapid and sensitive liquid chromatography-tandem mass spectrometry (LC-MS/MS) method with multiple reaction monitoring (MRM) was developed for the determination of solanesol in Nicotiana tabacum. Sample preparation was performed by ultrasonic extraction with methanol for 20 min and then supernatant was extracted with hexane. The method used atmospheric pressure chemical ionization (APCI) detection in positive-ion mode. The separation of solanesol was performed on a Symmetry Shield RP18 column with a mixture of acetonitrile and isopropanol (1:1, v/v) containing 2mM ammonium acetate as mobile phase. Quantification of solanesol was performed by the standard addition method. The limit of quantification (LOQ) and limit of detection (LOD) of solanesol were, respectively, 5.0 ng/ml (S/N=10) and 1.5 ng/ml (S/N=3). The relative standard deviations of peak area were 0.89 and 1.12% for intra-day and inter-day, respectively. The recoveries of solanesol ranged from 97.72 to 99.67% and the corresponding R.S.D.s were less than 2.7%. Analysis took 5 min, making the method suitable for rapid determination of solanesol in N. tabacum. The proposed method has been successfully applied to the analysis of solanesol in various organs of N. tabacum.

A rapid and sensitive liquid chromatography-tandem mass spectrometry method with multiple reaction monitoring has been proposed for the analysis of coenzyme Q10 in (CoQ10) tobacco leaves. The method used electrospray ionization with detection in positive ion mode. Sample pretreatment involved ultrasonic extraction of fresh tobacco leaves with anhydrous ethanol for 15 min and followed by extraction of the supernatant with hexane. The separation of CoQ10 was performed on a Symmetry Shield RP18 column with a mixture of acetonitrile and isopropanol (8:7, v/v) containing 0.5% formic acid as mobile phase. Quantification of CoQ10 was performed by the standard addition method. The limit of detection and limit of quantitation of CoQ10 were, respectively, 1.2 ng/mL (S/N = 3) and 4.0 ng/mL (S/N = 10). The relative standard deviations of peak area were 0.91% and 1.21% for intra-day and inter-day, respectively. The recoveries of CoQ10 ranged from 98.2 to 99.3% and the corresponding RSDs were less than 2.4%. Analysis took 5 min, making the method suitable for rapid determination of CoQ10 in tobacco leaves. The proposed method has been successfully applied to the analysis of CoQ10 in the leaves from eight varieties of tobacco.