Green electrochemical sensors based on ionic liquid nanocomposites for detection of environmental pollutants

Industrialization and globalization have caused a huge burden on the limited natural resources, which releases various environmental pollutants such as toxic metal ions and pesticides. World Health Organisation (WHO) has set a maximum permissible limit for these toxic pollutants in water, above which, it is unsuitable for drinking purpose. There are various techniques available for the determination of such pollutants like ICP-MS, HPLC, FAAS etc. that are costly, cumbersome, and time consuming. Whereas, electrochemical sensors are portable, fast and can perform multi-analyte sensing. Electrochemical sensor can be made selective by fabricating with nanocomposites having different functional groups. Nowadays, trend of utilizing greener materials in research field is being highly appreciated in accordance with the principles of green chemistry for the application and development of electrochemical sensors. Ionic liquids having non-volatility, low toxicity, wide potential window, high electrochemical stability and conductivity have shown sustainable electrochemical sensing applications. Nanocomposite of these ionic liquids as a sensing platform have been extensively used in electrochemical detection of various pollutants. This work provides a literature survey of different ionic liquid nanocomposite based sensing platform for electrochemical detection of toxic pesticides and heavy metals. They have demonstrated good sensitivity with detection limit below WHO guidelines.

The applications of ionic liquids in drug delivery / 药学学报

Ionic liquids (ILs) are liquid mixtures formed by anions and cations in a certain stoichiometric ratio under certain conditions. They are widely used in various fields because of their simple preparation process, low volatility, high stability, high conductivity and non-flammability. Here, we firstly introduce their formation principles, classification, and physical and chemical properties in detail. Then, we summarize their functions in pharmaceutical preparations, such as improving the solubility of insoluble drugs, enhancing the stability of drugs, and promoting the permeability of drugs, as well as their role as active pharmaceutical ingredients (API) to fabricate new drug delivery systems of API-ILs. Finally, we reviewed the applications of ILs in different administration routes, including oral, transdermal, mucosal, and injection routes, and meanwhile offer perspectives for the further use of ILs.

Chiral separation of four acidic drugs by micellar electrokinetic chromatography with ionic liquid-based surfactant / 中国药科大学学报

@#In this paper, micellar electrokinetic chromatography (MEKC) with glucose-β-cyclodextrin (Glu-β-CD) as chiral selector and ionic liquid surfactant N-butyl-N-methyl pyrrolidine lauryl sulfate ([C4MP] [C12SO4]) micelles formed at low pH as a pseudo stationary phase was applied for the chiral separation of four acidic drugs naproxen,warfarin, ketoprofen and ibuprofen.Under the same conditions,significantly improved separation of tested drug enantiomers was achieved with the MEKC system based on [C4MP][C12SO4] compared with the system based on the conventional surfactant sodium dodecyl sulfate (SDS).Several primary parameters affecting enantioseparation such as type and proportion of organic modifier, concentration and pH of the running buffer, concentration of chiral selector,concentration of ionic liquid surfactant and applied voltage were systematically investigated.

Application of natural deep eutectic solvents in pharmaceutics / 药学学报

Natural deep eutectic solvent (NDES) is a kind of deep eutectic solvents (DESs) which is composed of natural substances with good biocompatibility. Those substances can function as hydrogen bond donor and acceptor, such as choline, amino acids, sugars, etc. NDES have been widely used in many fields due to their advantages of low cost, easy preparation and environmental friendliness. It is especially suitable for the pharmaceutical industry because of its good biocompatibility and safety for use. In this paper, we firstly review the molecular simulation methods for current design of DESs from the formation principle. And then, the materials and preparation of NDES are reviewed and the physicochemical properties are further described. Finally, we review the current application of NDES in pharmaceutics including increasing drug solubility, promoting drug permeability and enhancing oral drug absorption, and meanwhile their future applications in pharmaceutics were also prospected.

Design of ionic liquid-based microwave-assisted extraction of flavonoids from Cyclea barbata Miers. and its lipoxygenase inhibitory activity

Green grass jelly (Cyclea barbata Miers.) is a plant from Indonesia that is believed to have anti-inflammatory activity.This study aims to find the optimum condition in grass jelly extraction using the ionic liquid-microwave assistedextraction toward total flavonoid content (TFC) and lipoxygenase activity (LIA). The experimental design wasperformed using the parameters variable including extraction time, liquid–solid ratio, and ionic liquids concentrationto obtain the optimum condition. The optimization analysis used response surface methodology (RSM) with Box–Behnken design (17 trials) to obtain a predictive model with TFC and LIA as a response surface value. In the presentstudy, the optimum condition was suggested by RSM analysis with parameter variables, including extraction time of17 minutes, 1-butyl-3-methylimidazolium bromide ([BMIM]Br) concentration of 1.76 mol/l, and the liquid–solid ratioof 38.21 ml/g. The equation of regression quadratic model was obtained to predict TFC and LIA as follows: TFC =2.43A + 2.43B + 1.42C + 0.33AB − 3.20AC − 0.46BC − 4.90A2 − 3.10B2 − 3.10C2 + 28.32 with R2 = 0.8336 and LIA= 0.066A + 8.22B + 0.97C + 2.47AB − 5.86AC + 1.96BC − 9.99A2 − 13.75B2 − 13.11C2 + 63.53 with R2 = 0.9207,respectively

Determination of Escitalopram in Biological Samples by Dispersive Liquid-Liquid Microextraction Combined with GC-MS/MS / 法医学杂志

Objective To establish a method for determination of escitalopram in biological samples by ultrasound-assisted ionic liquid-dispersive liquid-liquid microextraction combined with gas chromatography-tandem mass spectrometry （GC-MS/MS） and provide evidences for forensic determination of cases related to escitalopram. Methods The 1-hexyl-3-methylimidazolium hexafluorophosphate （[C6MIM][PF6]） was selected as an extract solvent to process biological samples. Ultrasound-assisted extraction was used on the samples. Then the samples were detected by GC-MS/MS. Results The linear range of escitalopram in blood and liver were 5.56-1 111.10 ng/mL and 0.025-5.00 mg/g, respectively. The correlation coefficient （r） were greater than 0.999, limit of detection （LOD） were 4.00 ng/mL and 2.00 μg/g, limit of quantitation （LOQ） were 14.00 ng/mL and 6.00 μg/g, respectively. The extraction recovery rates were all greater than 50%, the interday and intraday precision were less than 20%. Escitalopram was detected in blood and liver samples from the actual poisoning case by this method with a content of 1.26 μg/mL and 0.44 mg/g, respectively. Conclusion The ultrasound-assisted ionic liquid-dispersive liquid-liquid microextraction combined with GC-MS/MS is environment friendly, rapid, has good enriching effect and consumes less organic solvent and can be used for forensic determination of escitalopram related cases.

Utilization of [Bmim]BF4-MAE on enhancement of γ-oryzanol extraction from rice bran and its tyrosinase inhibitory activity

This study investigated the effect of ionic liquid (IL)-microwave assisted extraction (MAE) on γ-oryzanol extraction from rice bran (Oryza sativa L.). The conditions included the concentration of IL, liquid (IL)/solid (sample) ratio, extraction time, and microwave power. The use of 1-butyl-3-methylimidazolium ([Bmim]BF4) as a selected solvent in IL-MAE method was developed for extraction of γ-oryzanol from rice bran. The Box-Behnken design on four factors with response surface methodology (RSM) was used to optimize the experimental conditions. The optimum conditions for the MAE were a [Bmim]BF4 concentration of 0.7 M, liquid/solid ratio of 15 mL/g, extraction time of 10 minutes, and 30% microwave power with a γ-oryzanol value of 0.41 mg/g. The experimental values agreed with those predicted by the RSM models. A microplate reader method was used to determine the IC50 value in tyrosinase inhibitory activity of the extract. An IC50 value of the extract obtained from IL-MAE was 1240 µg/mL. This study suggests that IL-MAE is suitable for the extraction of γ-oryzanol from rice bran and that under the optimum conditions the extract has low activity as a tyrosinase inhibitor.

In vitro penetration activity of ionic liquid-Gnetum gnemon seed extract loaded solid lipid nanoparticles

Gnetum gnemon L. (Melinjo) seeds have high trans-resveratrol, which was known to have poor skin absorption ability.This study was performed to evaluate the skin absorption of ionic liquid-melinjo seed extract (IL-MSE) loaded solidlipid nanoparticles (SLN). The SLNs was formulated with glyceryl monostearate as the lipid ingredient, ceteareth-25,ceteareth-6, stearyl alcohol, an aqueous phase, and 10% melinjo seed extract. The SLNs were prepared by modificationof high-pressure homogenization. The polydispersity index (PDI), zeta potential, entrapment efficiency (EE), particlesize (PS), and morphological scanning electron microscopy (SEM) were evaluated. The in vitro penetration of IL-MSESLN was carried out by using the Franz cell diffusion method. The SLNs formulations showed an average of particlessize about 794 nm, and with high lipid and surfactant, the content could contributing to high entrapment efficiencyto almost 89%. Even though the polydispersity index of SLN was 1.229, and zeta potential measurement was 62.56mV. Up to 45% of the trans-resveratrol penetrated through the skin after 8 hours of the test run. The IL-MSE loadedto SLNs could improve the absorption of trans-resveratrol through the skin.

Assessment of wasteland derived biomass for bioethanol production

Background: The bioethanol produced from biomass is a promising alternative fuel. The lignocellulose from marginal areas or wasteland could be a promising raw material for bioethanol production because it is present in large quantities, is cheap, renewable and has favorable environmental properties. Despite these advantages, lignocellulosic biomass is much more difficult to process than cereal grains, due to the need for intensive pretreatment and relatively large amounts of cellulases for efficient hydrolysis. Therefore, there is a need to develop an efficient and cost-effective method for the degradation and fermentation of lignocellulosic biomass to ethanol. Results: The usefulness of lignocellulosic biomass from wasteland for the production of bioethanol using pretreatment with the aid of ionic liquids of 1-ethyl-3-methylimidazolium acetate and 1-ethyl-3-methylimidazolium chloride was evaluated in this study. The pretreatment process, enzymatic hydrolysis and alcoholic fermentation lasted a total of 10 d. The largest amounts of bioethanol were obtained from biomass originating from agricultural wasteland, in which the dominant plant was fireweed (Chamaenerion angustifolium) and from the field where the common broom (Cytisus scoparius) was the dominant. Conclusions: The plants such as fireweed, common broom, hay and goldenrod may be useful for the production of liquid biofuels and it would be necessary in the further stage of research to establish and optimize the conditions for the technology of ethyl alcohol producing from these plant species. Enzymatic hydrolysis of biomass from agricultural wastelands results in a large increase in fermentable sugars, comparable to the enzymatic hydrolysis of rye, wheat, rice or maize straw.

Improvement of ethanol production from birch and spruce pretreated with 1-H-3-methylmorpholinium chloride

Background: Pretreatment is the critically important step for the production of ethanol from lignocelluloses. In this study, hardwood birch (Betula pendula) and softwood spruce (Norway spruce) woods were pretreated with a newly synthesized morpholinium ionic liquid, 1-H-3-methylmorpholinium chloride ([HMMorph][Cl]), followed by enzymatic hydrolysis and fermentation to ethanol. Results: [HMMorph][Cl] was synthesized using inexpensive raw materials, i.e., hydrochloric acid and N-methyl morpholine, following a simple process. The influence of pretreatment time (2, 3, 5, and 8 h) and temperature (120 and 140°C) in terms of hydrolysis efficiency was investigated. Glucose yields from enzymatic hydrolysis were improved from 13.7% to 45.7% and 12.9% to 51.8% after pretreatment of birch and spruce woods, respectively, under optimum pretreatment conditions (i.e., at 140°C for 3 h) as compared to those from pristine woods. Moreover, the yields of ethanol production from birch and spruce were increased to 34.8% and 44.2%, respectively, while the yields were negligible for untreated woods. Conclusions: This study demonstrated the ability of [HMMorph][Cl] as an inexpensive agent to pretreat both softwood and hardwood.

Digital Childhood: the Impact of Using Digital Technology on Children’s Health

Background and Objective: Digital media can be considered as an important element of life for today's children and adolescents since theyspend a lot of time using it. This increased use of digital media is associated with poor behavior and health status. Society in general andpractitioners in public health in particular should promote digital media use strategies through health education. This study is aimed atevaluating the impact of using digital technology on children physical, social and behavior health. Methodology: This is a descriptive studywhich was conducted at the primary health care centers of Tabuk. Through purposive sampling, 300 people were included in the study. Aquestionnaire and a checklist were used as the tools for data collection. Results: There was a significant relationship between theattachment to technology and both physical and psychological health of the studied children. There was also a significant differencebetween the awareness of mothers regarding both negative and positive effects of technology and total effects of technology at the pre andpost-intervention stages. Conclusion: Using technology had an impact on both physical and psychological health of children, and there wasan improvement in mothers’ awareness in this regard. This reflects the key role of health education on improving the awareness of mothersabout the effects of using technology on the health of their children.

Application on imidazolium ionic liquid in extraction of flavonoids from natural products / 中草药

Flavonoids have many physiological and pharmacological activities. Ionic liquids are increasingly used in the extraction of flavonoids from natural products due to their unique properties. In this paper, various extraction methods of natural flavonoids were reviewed and summarized. The effects of anion and cation type, length of carbon chain, and bond cooperation on the extraction of natural flavonoids in ionic liquids, especially imidazole type ionic liquids, were also reviewed. Suggestions on selection of extractant for ionic liquid extraction of flavonoids were given. The advice of the green recovery of ionic liquids and the development of edible ionic liquids for the future direction of development were suggested. This study will lay the foundation for the basic research and industrial application of ionic liquids in the extraction of natural flavonoids.

Investigation of ion liquid combined withultrasound-assisted extraction technology of total flavones from Microcos paniculata and study on its lipids regulation activity / 中草药

Objective: To explore the high-efficiency green environmental extraction method of total flavones from Microcos paniculata (MPTF), and investigate its lipid-lowering activity. Methods: The ionic liquid was used to assist the ultrasonic extraction of MPTF, and the extraction process was investigated by single factor experiment and orthogonal test. Wistar rats were randomly divided into normal control group and positive control group (Resuvastatin Calcium Tablets 5.2 mg/kg) by high fat diet, high-fat model group and MPTF low, medium and high dose groups (ig dose MPTF 300, 600, 900 mg/kg), with 10 rats in each group. The total cholesterol (TC), glycerol lipid (TG), high density lipoprotein (HDL-C), low density lipoprotein (LDL-C) levels were determinated. Results: The optimum process conditions for ultrasonic-assisted extraction of MPTF by ionic liquid were as follow: ionic liquid was [BMIM]Cl at concentration of 0.30 mol/L; ratio of material to liquid was 1:40, extraction solvent was 60% ethanol aqueous solution with extraction time of 30 min at 50 ℃. The verification test results showed that the extraction rate of total flavonoids obtained from the extraction process was high and the process was stable. The results of lipid-lowering test showed that the levels of TC, TG and LDL-C were decreased in all doses of MPTF groups, and the level of HDL-C was increased (P < 0.05). With the increase of MPTF dose, the indicators showed obvious trends in a dese-dependent manner. Conclusion: The ionic liquid combined with ultrasonic- assisted extraction of MPTF is stable and feasible, which provides reference for ionic liquid synergistic ultrasound-assisted extraction of poorly soluble active ingredients in Chinese materia medica. MPTF extract has better lipid-lowering effect.

Separation and Determination of Rhynchophylline and Isorhynchophylline in Uncaria rhynchophylla by HPLC with Ionic Liquid as Mobile Phase Additives / 中国药房

OBJECTIVE： To establish a method to determine the contents of rhynchophylline and isorhynchophylline in Uncaria rhynchophylla. METHODS： The separation degree of ionic liquid 1-butyl-3-methylimidazolium chloride （C4mimCl） as mobile phase additive was compared with that of mobile phase without additives and with traditional additive triethylamine （which damaged the chromatographic column）. The optimum concentration of C4mimCl was screened and the contents of rhynchophylline and isorhynchophylline in U. rhynchophylla from 4 habitats in Jiangxi province were determined by the newly established method. The determination was performed on Dikmatech Diamonsil Plus C18 column， the mobil phase was acetonitrile-buffer （0.1％ phosphoric acid+3.0 mmol/L C4mimCl）， gradient elution. UV detection wavelength was set at 245 nm and the flow rate was 1    mL/min. Sample size was 10 μL. RESULTS： When mobile phase had no additives or 3.0 mmol/L triethylamine and 3.0 mmol/L C4mimCl were added as additives， the separation of rhynchophylline from the front peak was 1.02， 1.23 and 1.72， and the separation from the back peak was 1.06， 6.00 and 4.25， respectively. The symmetry factors were 0.81， 0.86 and 1.13， respectively. The separation of isorhynchophylline from the front peak was 0.96， 3.89 and 4.05， and the separation from the back peak was 1.02， 2.34 and 2.36， respectively. The symmetry factors were 0.88， 0.81 and 0.96， respectively. The linear range of rhynchophylline and isorhynchophylline were 4.93-157.76 （r＝0.999 9） and 4.98-159.50 μg/mL （r＝1.000）， respectively. The quantitative limits were 0.486 4， 0.793 6 μg/mL， respectively. RSDs of precision， repeatability， stability and durability tests were all less than 5％ （n＝6）. The recovery rates were 102.9％-107.8％ （RSD＝1.7％，n＝6） and 95.4％-106.3％ （RSD＝3.9％，n＝6）， respectively. The content of rhynchophylline and isorhynchophylline in U. rhynchophylla from 4 habitats were 0.758-1.343         and 1.511-1.823 mg/g， respectively. CONCLUSIONS： Addition of C4mimCl into mobile phase can enhance its separation. Established HPLC method is rapid， accurate and reproducible， which can be used for content determination of rhynchophylline and isorhynchophylline in U. rhynchophylla.

Applications of ionic liquids in drug research / 药学学报

Ionic liquids are not limited to the traditional use of solvents because of their high permeability and excellent physicochemical and unique biological properties. Nowadays, with the deep understanding of their toxicity and biocompatibility, ionic liquids have been tailored as novel solutions to address potential problems of marketed drugs. Based on the research and development of modified new drugs, ionic liquids have been incorporated into drug synthesis and emerged as attractive environmental-friendly reaction media with milder reaction conditions, higher yields and easier reaction workups and drug delivery systems. In addition, they have been designed for effective drug carriers removing undesirable properties of solid drugs. Further, ionic liquids forming active pharmaceutical ingredients dedicated to the liquefaction of drugs for promising clinical applications.

Ionic Liquid Ultrasonic-assisted Solid Phase Extraction of Four Kinds of Hosenkosides from Seeds of Impatiens balsamina L / 分析化学

A green, rapid and efficient method was developed for the extraction of 4 kinds of hosenkosides from the seeds of Impatiens balsamina L. The hosenkosides were extracted by ionic liquid, and then enriched by solid phase extraction. The effects of the kinds and volume of ionic liquid, pH value, ultrasonic time, solid phase extractant and eluent on the extraction fields were investigated and optimized. Under the optimum conditions, the recoveries of 4 kinds of hosenkosides were between 92. 1％ and 108. 2％ , the correlation coefficients were 0. 9945-0. 9975, and the detection limits were 1. 8-4. 5 μg / mL. The RSD values were all less than 3. 9％ . The experimental results showed that this method was fast, efficient, environmental protection. This study provided a reference for the extraction and enrichment of trace components in Chinese medicinal herbs.

Investigation of Single-stranded Deoxyribonucleic Acid Translocation Through α-Hemolysin Nanopore with Ionic Liquid Supporting Electrolytes / 分析化学

Due to the difference in spatial configuration and charge of the bases in a DNA molecule, characteristic translocation current pulses through a single nanopore could be obtained. This could become the basis of DNA sequencing method. However, due to the fast translocation speed (sub-micro seconds) and the small current change (about pA), it is still a challenge to obtain the accurate molecular substructure with present electronic techniques. In this work, in order to control the translocation behavior of ssDNA, two kinds of ionic liquids with high viscosity and conductivity were introduced to establish a viscosity gradient with the α-hemolysin single nanopore interface and the acidity of the solution was optimized. The trans chamber contained pure BmimPF6 and the cis chamber contained 1 mol/ L BmimCl and 10 mmol/ L Tris-HCl ( pH 5. 5 ). Preliminary experiment results under this electrolyte configuration showed that poly ( dC) 15 , poly ( dC) 15 , poly(dC) 30 and poly(dC) 50 exhibited obvious long duration pulses with high current suppression ratio. The blocking depth reached more than 95％ of long blocking events. The duration time of long blocking events prolonged to tens or hundreds of milliseconds. Meanwhile, the peak-peak of baseline noise was reduced by about 30％ .

Los líquidos iónicos como prometedores catalizadores en síntesis orgánica: una contribución a la química sostenible / Ionic liquids as promising catalysts in organic synthesis: a contribution to sustainable chemistry / Líquidos iónicos como catalisadores promissores na síntese orgânica: um contributo para a química sustentável

Resumen Introducción. En todos los procesos químicos se requiere de un medio de reacción o solvente, y dichos solventes orgánicos son altamente volátiles por lo que son contaminantes de la atmósfera, y se requieren nuevos métodos, procesos y otro tipo de solventes que minimice dicha contaminación, y los líquidos iónicos están resultando ser una gran alternativa a dicho problema. Objetivo. Sintetizar líquidos iónicos a base del imidazol con aniones tanto inorgánicos como orgánicos y evaluar su potencial aplicación como catalizadores en reacciones importantes de síntesis orgánicas, como la síntesis asimétrica, específicamente la condensación aldolica. Materiales y métodos. El metil imidazol (99%), 1-bromobutano (97%), prolina (98%), KOH (97%), acetato de etilo, etanol, grado reactivo, fueron suministrados por Sigma Chemical Co. Se utilizó el metil imidazol; para la síntesis de líquido iónico base el bromuro de butil-metil-imidazol, [Bmim][Br]; los demás líquidos iónicos se obtienen por reacción de metátesis, para obtener el hidroxi de butil-metil-imidazol, [Bmim][OH], y el prolinato de butil-metil-imidazol, [Bmim][Pro]; estos líquidos fueron utilizados como catalizadores en la reacción de síntesis asimétrica como la condensación aldolica. Resultados. Se realizó una condensación aldolica clásica, p-nitrobenzalhedido con ciclohexanona para probar los líquidos iónicos sintetizados como catalizadores, y al comparar los resultados obtenidos con métodos convencionales se observan ventajas, como altos rendimientos y alta selectividad en menor tiempo de reacción. Conclusiones. En condiciones muy suaves de reacción, se logró reutilizar hasta 6 veces el líquido iónico como catalizador de la reacción sin perder las ventajas mencionadas, lo que lo hace un sistema sostenible.

Abstract Introduction. In all chemical processes, a reaction medium or solvent is required, and such organic solvents are highly volatile so they are pollutants to the atmosphere, and new methods, processes and other solvents are required to minimize the contamination, and Ionic liquids are proving to be a great alternative to such problem. Objective. Synthesize imidazole based ionic liquids with both inorganic and organic anions and evaluate their potential application as catalysts in important reactions of organic synthesis, such as asymmetric synthesis, specifically in asymmetric aldol reaction. Materials and Methods. Methyl imidazole (99%), 1-bromobutane (97%), proline (98%), KOH (97%), Ethyl acetate, ethanol, reagent grade were supplied by Sigma Chemical Co. It was used the methyl imidazol for the synthesis of the ionic liquid butyl methyl imidazole bromide, [Bmim] [Br], and the other ionic liquids were obtained by metathesis reaction from such ionic liquid, to obtain the butyl methyl imidazole hydroxy [Bmim] [OH], and the butyl methyl imidazole prolinate, [Bmim] [Pro]. These ionic liquids were used as catalysts in the asymmetric aldol reaction. Results. A classical aldol reaction, p-nitrobenzaldehyde with cyclohexanone was performed to test the ionic liquids synthesized as catalysts, and when comparing the results obtained with conventional methods, advantages were observed, such as high yields and high selectivity in less time reaction. Conclusions. Under very mild reaction conditions, it was possible to reuse up to 6 times the ionic liquid as a reaction catalyst without losing the mentioned advantages, which makes it a sustainable system.

Resumo Introdução. Todos os processos químicos requerem um meio de reação ou solvente, tais solventes orgânicos são altamente voláteis, é assim que são os poluentes principais da atmosfera, porem precisa-se de novos métodos, processos e outros solventes para minimizar a contaminação, por isso, os líquidos iónicos estão provando para ser uma ótima alternativa para esse problema. Objetivo. A sínteses dos líquidos iónicos com base em imidazol e usando ânions inorgânicos e orgânicos e avaliar sua potencial aplicação como catalisadores em reações importantes em síntese orgânica, tais como a síntese assimétrica, especificamente a condensação aldólica. Materiais e Métodos. O imidazol metil (99%), 1-bromobutano (97%), prolina (98%), KOH (97%), acetato de etila e etanol no grau de reagente, foram fornecidos pelo Sigma Chemical Co. O metila-imidazol foi utilizado para a síntese baseado no líquido iónico brometo de metil-butil-imidazo-, [BMIM] [Br], Os outros líquidos iónicos são obtidos por reação de metátese, para se obter o hidroxi de butil-metil-imidazol, [BMIM][OH], e prolinato de butil-metil-imidazol, [BMIM][Pro], estes líquidos foram usadas como catalisadores na reação de síntese assimétrica, como a condensação aldólica. Resultados. Foi realizada uma condensação aldólica clássica usando p-nitrobenzaldeído com a cicloexanona para testar os líquidos iónicos sintetizados como catalisador, ao comparar os resultados obtidos com os métodos convencionais darão vantagens, tais como rendimentos elevados e alta seletividade é observada no tempo de reação mais rápido. Conclusões. Nas condições muito suave de reação, foi possível reutilizar até 6 vezes o líquido iónico como catalisador da reação, sem perder as vantagens mencionadas, tornando-se um sistema sustentável.

Matrix-assisted Laser Desorption/Ionizaiton-Mass Spectrometry Imaging of Oligosaccharides in Soybean and Leaf Using Ionic Liquid as Matrix / 分析化学

The ionic liquid butylamine 2,5-dihydroxybenzoate (DHB-BuN) was chosen as the matrix for improving repeatability of oligosaccharides quantitation, and imaging oligosaccharides in soybean and leaf by matrix-assisted laser desorption/ionization-mass spectrometry (MALDI-MS).Using the ionic liquid matrix methanol solution (20%, V/V) to cover sample slice, and setting MS acquisition parameters including polarity as positive and laser power as 70%, the MS imaging experiment was performed to analyze oligosaccharides and their distribution in soyben and soybean leaf.As a result, the MALDI-MS analysis of 3 kinds of oligosaccharides including sucrose, raffinose and stachyose was performed using the ionic liquid matrix and the reproducibility RSDs were less than 3% for in-spot and less than 4% for spot-to-spot.The standard curves linear correlation coefficients (R2) were all no less than 0.996 between MS peak intensity and oligosaccharides concentraions in the concentration rage of 0.062-1.00 mg/mL, which showed quantitative power in MALDI-MS analysis.The matrix was used for MALDI-MS imaging analysis of soybean chips and soybean leaf surface disaccharide, trisaccharide and tetrasaccharide to obtain the soybean mass spectrum and spatial resolution of 150 μm of the three oligosaccharides imaging.Three kinds of oligosaccharides in the soybean roughly balanced distribution, and the oligosaccharides distribution in the leave was mostly at its tip part.The contents of the 3 kinds of oligosaccharides could be estimated by their MS peak intensity and above standard curve.The result suggested that the ionic liquid DHB-BuN matrix could be well applied in MALDI-MS imaging analysis of oligosaccharides in different sample.

Simultaneous Determination of Curcumin and Germacrone in Curcuma wenyujin by Ultrasound-Assisted Ionic Liquid-Reversed Phase Liquid Chromatography / 中国药学杂志

OBJECTIVE: To establish a method for the simultaneous determination of curcumin and germacrone in Curcuma wenyujin by ultrasound-assisted ionic liquid-reversed phase liquid chromatography. METHODS: An Agilent ZORBAX Eclipse Plus C18 column (4. 6 mm × 250 mm, 5 μm) was used. Gradient elution was conducted with the mobile phase consisting of acetonitrile and 0.1% phosphoric acid at the flow rate of 1.0 mL·min-1. The detection wavelength was set at 265 nm, the flow rate was set at 1.0 mL·min-1, and the column temperature was maintained at 30 ℃. RESULTS: The result showed that curcumin and germacrone had the highest extraction yield when the [BMIM]PF6 methanol solution concentration of 0.6 mol·L-1 was used as the extraction solvent and the solid-liquid ratio was 1:20. Under the optimized condition, good linearity of curcumin was shown for curcumin in the range of 0.041 2-2.06 μg (r=0.999 9)and the average recovery was 98.31%. The good linearity of germacrone was shown for germacrone in the range of 0.010 04-0.502 μg (r=0.999 8)and the average recovery was 97.62%. CONCLUSION: This method is convenient, environmentally friendlygreen and highly reproducible. It is beneficial important to study the extraction method of the active gradients of the traditional Chinese medicine Curcuma wenyujin active gradient and its quality control of Curcuma wenyujin.