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1.
An aqueous extraction system containing an ionic liquid (IL) surfactant was developed for the extraction of echinacoside and acteoside from Cistanche deserticola Y. C. Ma. We synthesized 1-dodecyl-3-methylimidazolium tetrafluoroborate ([C12mim][BF4])and applied it as a sustainable extraction solvent for echinacoside and acteoside. Single-factor and response surface methods were used to establish the optimum conditions for the ultrasound-assisted extraction (UAE) using [C12mim][BF4]. With an extraction time of 16 min, a liquid–solid ratio of 10 mL/g, and a [C12mim][BF4] concentration of 16 mmol/L, the yield of echinacoside obtained by the UAE was 7.47 mg/g, which was 123.58%, 190.44%, and 276.73% that of UAE with sodium dodecyl sulfate (SDS), ethanol, and water, respectively, and 334.80% that of heating reflux extraction (HRE) with water. The acteoside yield obtained with the [C12mim][BF4] UAE was 3.56 mg/g, which was 150.17%, 224.66%, and 364.80% that of UAE with SDS, ethanol, and water, respectively, and 450.93% that of HRE with water. The IL-UAE had a much shorter extraction time than the traditional ethanol extraction. The surfactant could be recycled and reused, and the relative regenerability of the target compounds was above 90%. Therefore, UAE with [C12mim][BF4] is a green and efficient extraction method for isolating echinacoside and acteoside from C. deserticola Y. C. Ma. This method could be also applied to the extraction of phenylethanol glycosides from other plants.  相似文献   

2.
In this work, an efficient in situ solvent formation microextraction (ISFME) was combined with stopped-flow injection spectrofluorimetry (SFIS) for the determination of copper. In the proposed approach, thiamine was oxidized with copper(II) to form hydrophobic and highly fluorescent thiochrome (TC), which was subsequently extracted into ionic liquid as an extractant phase. A small amount of an ion-pairing agent (NaPF6) was added to the sample solution containing a water-miscible ionic liquid ([Hmim][BF4]) to obtain a hydrophobic ionic liquid ([Hmim][PF6]), which acted as the extraction phase. After centrifuging, phase separation was performed and the enriched analyte was determined by SFIS. ISFME is an efficient method for separation and preconcentration of metal ions from aqueous solutions with a high ionic strength. Variables affecting the analytical performance were studied and optimized. Under optimum experimental conditions, the proposed method provided a limit of detection (LOD) of 0.024 μg L−1 and a relative standard deviation (RSD) of 2.1%. The accuracy of the combined methodology was evaluated by recovery experiments and by analyzing certified reference material (GBW 07605 Tea). Finally, the proposed method was successfully applied to copper determination in water and food samples.  相似文献   

3.
《Toxin reviews》2013,32(3):91-94
Abstract

The mechanisms of the cytotoxic effect of ionic liquid (IL) 1-octyl-3-methylimidazolium chloride ([C8mim][Cl]) on bacterial cells were studied. Bacterial cells were exposed to 0, 0.1, 1 and 10?mmol???L?1 [C8mim][Cl] for 10?h. The results showed that [C8mim][Cl] inhibited bacterial cell proliferation in a dose-dependent manner. When IL concentrations reached 10?mmol?L?1, almost no cell division was observed. [C8mim][Cl] treatment significantly reduced succinate dehydrogenase activity. The amount of total protein significantly decreased with increasing [C8mim][Cl] concentrations of up to 10?mmol?L?1. [C8mim][Cl] increased protein and nucleic acid contents in the extracellular fluid and increased cell permeability. The results suggest that the increase in cell membrane permeability, which was induced by [C8mim][Cl], could inhibit cell proliferation and metabolic activity in bacteria.  相似文献   

4.

Background and the purpose of the study

Ofloxacin is a quinolone synthetic antibiotic, which acts against resistant mutants of bacteria by inhibiting DNA gyrase. This antibacterial agent is widely used in the treatment of respiratory tract, urinary tract and tissue-based infections, which are caused by Gram-positive and Gram-negative bacteria. In this work, an efficient modified ionic liquid cold-induced aggregation dispersive liquid-liquid microextraction (M-IL-CIA-DLLME) was combined with spectrofluorimetry for trace determination of ofloxacin in real samples.

Methods

In this microextraction method, hydrophobic 1-hexyl-3-methylimidazolium hexafluorophosphate ([Hmim] [PF6]) ionic liquid (IL) as a microextraction solvent was dispersed into a heated sample solution containing sodium hexafluorophosphate (NaPF6) (as a common ion) and the analyte of interest. Afterwards, the resultant solution was cooled in an ice-water bath and a cloudy condition was formed due to a considerable decrease of IL solubility. After centrifuging, the enriched phase was introduced to the spectrofluorimeter for the determination of ofloxacin.

Results and major conclusion

In this technique, the performance of the microextraction method was not influenced by variations in the ionic strength of the sample solution (up to 30% w/v). Furthermore, [Hmim][PF6] IL was chosen as a green microextraction phase and an alternative to traditional toxic organic solvents. Different parameters affecting the analytical performance were studied and optimized. At optimum conditions, a relatively broad linear dynamic range of 0.15-125 µg l-1 and a limit of detection (LOD) of 0.029 µg l-1 were obtained. The relative standard deviation (R.S.D.) obtained for the determination of five replicates of the 10 ml solution containing 50 µg l-1 ofloxacin was 2.7%. Finally, the combined methodology was successfully applied to ofloxacin determination in actual pharmaceutical formulations and biological samples.  相似文献   

5.
Recently, the new concept of three-phase liquid microextraction was introduced based on applying two immiscible organic solvents in lumen and wall pores of hollow fiber. In the present work, this novel microextraction technique combined with gas chromatography-mass spectrometry has been developed for determination of tramadol, an analgesic agent, in plasma and urine samples. A systematic investigation of the proposed method was applied to find optimal extraction conditions and evaluate the interaction effects between the factors by designing experiments according to the methodology of Box-Behnken response surface design. Analysis of variance (ANOVA) revealed that the important factors contributing to extraction efficiency are extraction time, stirring rate and hollow fiber length. Under the optimum conditions, the developed method provided a preconcentration factor of 546, good repeatability (RSD % = 6.4), and good linearity (r2 = 0.995) for spiked plasma and urine real samples. The linear dynamic range from 0.1 to 400 μg L−1 and limit of detection (LOD) of 0.08 μg L−1 were obtained under selected ion monitoring mode. The results demonstrated that three-phase hollow fiber microextraction based on two immiscible solvents is a simple and accurate technique with very good preconcentration factor and clean-up for extraction of tramadol from biological samples.  相似文献   

6.
Ionic liquids have recently received considerable attention due to their negligible vapor pressure and substitute for conventional organic solvents. However, their solubility in water and a great deal of literature regarding their toxicity on aquatic organisms have caused much concern in recent years. This study aims to evaluate the cytotoxicity of 1-octyl-3-methylimidazolium chloride ([C8mim][Cl]) on the rat pheochromocytoma (PC12) cell line by cell viability assay and to determine the cytological alterations and damages in PC12 cells after 24 h of exposure at the concentrations of 0.07, 0.14, and 0.28 mM of [C8mim][Cl]. The results show that [C8mim][Cl] inhibits PC12 cell growth and decreases their viabilities in a remarkable dose-dependent manner, and the 24 h EC50 of [C8mim][Cl] for PC12 cells is calculated to be around 0.56 mM. Our results also reveal that [C8mim][Cl]-exposure induces DNA damage, sustained increase of intracellular Ca2+, overproduction of reactive oxygen species, gradually exhausted cellular ATP, mitochondrial permeability transition, and apoptosis in PC12 cells. We suppose that mitochondrial permeability transition and mitochondrial dysfunction maybe the major cytotoxicity mechanism of [C8mim]Cl for PC12 cells.  相似文献   

7.
In the present work, hollow fiber liquid phase microextraction (HF-LPME) in conjunction with reversed-phase HPLC/UV was developed for extraction and determination of trace amounts of chlorpromazine in biological fluids. The drug was extracted from an 11 ml aqueous sample (source phase; SP) into an organic phase impregnated in the pores of the hollow fiber (membrane phase; MP) followed by the back-extraction into a second aqueous solution (receiving phase; RP) located in the lumen of the hollow fiber. The effects of several factors such as the nature of organic solvent, compositions of SP and RP solutions, extraction time, ionic strength and stirring rate on the extraction efficiency of the drug were examined and optimized. Under the optimal conditions, enrichment factor of 250, dynamic linear range of 1–500 μg l−1, and limit of detection of 0.5 μg l−1 were obtained for the drug. The percent relative intra-day and inter-day standard deviation (R.S.D.%) based on three replicate determinations were 6.7 and 10.3%, respectively. The method was applied to drug level monitoring in the biological fluids and satisfactory results were obtained.  相似文献   

8.
In the study, a fast and green natural deep eutectic solvent based ultrasound-assisted liquid liquid microextraction (NDES-UALLME) were proposed for the determination and extraction of deltamethrin in food samples using UV/Vis spectrophotometry. The extraction step was based on ion-pair formation between deltamethrin and levulinic acid-tetraethylammonium bromide (as extraction solvent) at pH 5.5, and then extraction of deltamethrin into micro-drops of extraction solvent by using tetrahydrofuran. Levulinic acid-based natural deep eutectic solvents composed of natural, green compounds, i.e., choline acetyl chloride, tetrabutylammonium bromide, tetraethylammonium chloride and tetraethylammonium bromide were used for the first time as extraction solvents for extraction of deltamethrin. The NDES-UALLME procedure allowed to exclude matrixes effects and increase enrichment factor (283) of deltamethrin. Several key factors, including the type and the volume of extraction solvent, the pH of sample solution, ultrasound time, extraction temperature, ionic strength and sample volume were optimized in detail. At optimized conditions, the NDES-UALLME procedure was characterized by low limit of detection (2.4 ng mL?1), a wide linear dynamic range (8–950 ng mL?1), quantitative recoveries (93 ± 4%-103 ± 2%) and acceptable relative standard deviations (2.9%≤). The validation of NDES-UALLME procedure was carried out using recovery tests, intraday and intraday studies. The applicability of NDES-UALLME procedure was confirmed by the assay of deltamethrin in real food samples.  相似文献   

9.
The recent developments in hollow fiber liquid phase microextraction and dispersive liquid –liquid microextraction are reviewed. Applications of these newly emerging developments in extraction and preconcentration of a vast category of compounds including heavy metals, pesticides, pharmaceuticals and abused drugs in complex matrices (environmental and biological matrices) are reviewed and discussed. The new developments in these techniques including the use of solvents lighter than water, ionic liquids and supramolecular solvents are also considered. Applications of these new solvents reduce the use of toxic solvents and eliminate the centrifugation step, which reduces the extraction time.  相似文献   

10.
The modification of clinoptilolite as a natural zeolite via a simple route was carried out for CO2 adsorption. Cation exchange with Li+, Mg2+, and Ca2+, amine modification using monoethanolamine (MEA), triethanolamine (TEA) and hexyl amine, and ionic liquid modification using [bmim]X (X = PF6?, NO3?, Br?, Cl?, and bmim = 1-Butyl-3-methylimidazolium) were performed in a different amount of the modifiers. The samples were characterized by several methods (XRD, FT-IR, BET, and SEM), and adsorbed CO2 was evaluated utilizing adsorption isotherm at a wide range of pressure. The results showed enhancement in CO2 adsorption capacity for all the samples and 4.18, 3.58, and 4.35 times increase in CO2 adsorption were obtained where clinoptilolite/Li+, clinoptilolite/2% MEA and clinoptilolite/5% [bmim]PF6 were used as adsorbent at 4 bar pressure of CO2, respectively.  相似文献   

11.
A simple, inexpensive, and efficient nanomagnetic powder three-phase hollow fibre-based liquid-phase microextraction (HF-LPME) technique combined with ultrahigh performance liquid chromatography–mass spectrometry (UPLC–MS) was developed for the simultaneous analysis of nine flavonoids in Polygonum hydropiper L. samples. The final, optimised extraction conditions were as follows: an organic solvent of ethyl acetate, a donor phase of aqueous KH2PO4 at pH 3.0, an acceptor phase of aqueous NaHCO3 at pH 8.5, a stirring rate of 1000 rpm, and an extraction time of 50 min. Under these conditions, analyte calibration curves were all linear, with correlation coefficients ≥0.9994. The relative standard deviation for all analytes in intra-day (0.8–2.2%) and inter-day (1.7–3.5%) precision tests was well within the acceptable ranges, as were the limits of quantitation (LOQ < 0.054 μg/L) and detection (LOD < 0.170 μg/L). Recoveries for all standard compounds were between 95.17% and 99.82%, with a RSD of no more than 2.3%. Correlative analyses demonstrated that the physicochemical parameters of the compounds themselves also influenced the extraction efficiency. This technology proved to be rapid, sensitive, and reliable for the quality control of P. hydropiper L. samples.  相似文献   

12.
Substrate solubility remains a major limitation in Ir(I)‐catalyzed isotopic hydrogen exchange labelling. In the search for an alternative to the solvent dichloromethane, which is critical to the success of the reaction, we examined a series of ionic liquids for their suitability. Commercially available 1‐butyl‐3‐methylimidazolium hexafluorophosphate (abbreviated to [BMI][PF6]) was found to support efficient deuterium and tritium exchange labelling of N‐(4‐methoxyphenyl)‐N‐methyl benzamide 1 under standard conditions. The solvent dissolves both polar hydroxyl and carboxylic acid substituted acetanilides, providing isotopomers in unprecedentedly high deuterium incorporation as compared to dichloromethane. We report the application of [BMI][PF6] and its potential for extending the scope of Ir(I)‐catalyzed H/T exchange to more polar compounds. Copyright © 2003 John Wiley & Sons, Ltd.  相似文献   

13.
In this study, a novel method for extraction saponins from Xanthoceras sorbifolium Bunge leaves (XLs) was developed using ultrasonic-assisted ionic liquid combined with in situ alkaline aqueous biphasic systems (UAE-IL-AABS). UAE-IL was firstly used to extract saponins from XLs, followed by removal of the phenolic impurities using in situ IL-AABS. A Box-Behnken Design (BBD) was used to analyze the [C4MIM]BF4 concentration, time, liquid/solid ratio, and power on the saponins yield. Under the optimal conditions with [C4MIM]BF4 concentration 2.3 M, time 19.9 min, liquid/solid ratio 24.9:1 (mL/g), and power 165 W, the saponins yield was 8.17%, which was 11.01% higher than ultrasonic assisted ethanol extraction method. The major compounds in UAE-IL were also identified using UPLC-MS/MS. Moreover, the optimized conditions of IL-AABS with recovery rate of saponins was 96.70%. Finally, a low extraction time, and favorable impurities removal efficiency and recyclability suggested UAE-IL-AABS is greener for production in the food, medicine, and chemical industry.  相似文献   

14.
Switchable-hydrophilicity solvent-liquid-liquid microextraction (SHS-LLME), as an efficient sample cleanup method, was combined with dispersive solid-phase microextraction (DSPME) for preconcentration of quercetin prior to its spectrophotometric determination. Optimum SHS-LLME were found as 1000 μL of N,N-dimethylcyclohexylamine as the extraction solvent and 750 μL of 10.0 M sodium hydroxide as the phase separation trigger. Optimum DSPME were sample pH at 6.0, 1000 μL of acetone as the eluent, 30.0 mL of sample, 12.5 mg of Fe3O4@XAD-16 as the adsorbent, 4.0 and 1.5 min as the adsorption and elution times, respectively. Calibration graphs with coefficient of determination (R2) higher than 0.9956, limits of detection (LOD) of 9.0–11.9 ng mL?1 and limits of quantitation (LOQ) of 29.9–39.6 ng mL?1 were obtained. Repeatability, expressed as percentage relative standard deviation (%RSD), was better than 3.2 and 8.9% for intra- and inter-day precision, respectively. The proposed SHS-LLME-DSPME-UV/Vis method was applied for the determination of quercetin in four food samples (i.e., apple, pepper, red and white onion) with percentage recoveries in the range of 92.1–107.4%. The proposed method is superior to others in terms of greenness, rapidness, simplicity, good repeatability and low capital cost.  相似文献   

15.
The aim of this study was to investigate cytotoxicity, acute and subchronic oral toxicity of an ionic liquid didecyldimethylammonium saccharinate [DDA][Sac] in rat.IC50 values tested on six human cell lines varied from 1.44 μM to 5.47 μM. The compound tested was classified to the 4th toxicity class with a fixed LD50 cut-off value 500 mg/kg. Organ pathology induced by [DDA][Sac] in an acute experiment included exfoliation of the surface layer of the colon and alveolar septa in lung parenchyma. In a subchronic experiment rats were administered 10, 30 and 100 mg/kg/day [DDA][Sac] for 28 days. Reduced body weight gain and slightly reduced food consumption was observed particularly in high-dose rats. Slight hematology changes were found only in mid-dose females. Statistically significant changes in clinical chemistry parameters included: increases in the ALT, SDH, ALP and GGT activities, and in glucose, blood urea nitrogen and creatinine concentrations. However, these changes did not occur in both sexes and were not dose-related with the exception of ALP in females. No treatment-related microscopic changes were observed in a subchronic experiment. Under the condition of this study the lowest-observed-adverse-effect level of [DDA][Sac] was considered to be 10 mg/kg/day.  相似文献   

16.
This study evaluated the toxicity of 1-methyl-3-octylimidazolium chloride ([C8mim]Cl) on Paramisgurnus dabryanus by enzyme analysis, comet assay, and apoptosis analysis. The study showed that [C8mim]Cl had an obvious toxic effect inducing oxidative stress, genotoxicity, and cytotoxicity to fish liver cells. [C8mim]Cl also induced changes in the activities of superoxide dismutase and catalase, and the glutathione content and malondialdehyde level in fish exposed at 20–80 mg L−1. With increased exposure concentration and time, the four antioxidant enzyme activities, three different comet parameters and apoptosis rates of tested cells were significantly increased, with significant differences (P < 0.05 or P < 0.01) observed between control group and each treatment group. This study shows that [C8mim]Cl could be a threat to aquatic organism health when accidentally released into aquatic ecosystems.  相似文献   

17.
In this research paper, fatty acid-based deep eutectic solvents (FA-DESs) were prepared and investigated for the extraction of butylparaben (BP) from cosmetic products by air assisted liquid liquid microextraction (AA-DLLME). The amounts of BP were determined by UV/Vis spectrophotometry. By combining single factor optimization and Box-Behnken design based multivariate approach, key extraction parameters affecting the FA-DES AA-LLME procedure were systematically optimized. Under the optimized conditions, wide working range (5–800 μg L?1) was obtained with a good r2:0.9972 and high enrichment factor (205). For three replications run of 10 μg L?1 (low), 300 μg L?1 (medium) and 600 μg L?1 (high) of BP, the percent extraction recovery and relative standard deviation were in the range of 92 ± 4%-98 ± 2% and 1.8–2.6%, respectively. The limit of detection and the limit of quantification were 1.5 μg L?1 and 5 μg L?1, respectively. The study of the matrix effect showed that the proposed method has high selectivity for measuring BP in the selected samples. Therefore, it has great potential in sample pre-treatment and quantification of trace BP in cosmetic products.  相似文献   

18.
A magnetic ionic based dispersive liquid liquid microextraction (MIL-DLLME) procedure was optimized for the analysis and extraction of cadmium in water and food samples by flame atomic absorption spectrophotometry (FAAS). Contribution of experimental variables were optimized through central composite design combined with response surface analysis. Under optimized conditions, the limit of detection was found 0.6 ng mL?1 with the relative standard deviation of 1.7%. Dynamic range was obtained in the concentration range of 2–700 ng mL?1 with correlation coefficient of 0.9983. Relative recoveries were ranged from 94% to 99% with enrichment factor of 172. The validation of the optimized method was successfully confirmed by reference material analysis. The optimized method allows the analysis of cadmium in water and food samples with good reliability of the determination. Compared with the conventional procedures, the method enabled a fast, green and simple determination of cadmium in the real sample with minimal solvent consumption and a higher extraction capability.  相似文献   

19.
A simple and highly sensitive method that involves miniaturized hollow fibre assisted liquid‐phase microextraction with gas chromatography‐flame ionization detector was developed for the determination of trace concentration of sufentanil and alfentanil in biological samples. These drugs were extracted from 5 ml of aqueous solution with pH 10.0 into an organic extracting solvent (1‐octanol) impregnated in the pores and lumen of a hollow fibre. After extraction for a prescribed time, 2.0 µl of the extraction solvent was injected directly in to the GC injection port. Under the optimized conditions, (1‐octanol as extracting solvent, stirring rate of 700 rpm, 15% (w/v) salt addition, pH 10.0 and 25 min sampling time at 50 °C) large enrichment factors of 535 and 420 were achieved for sufentanil and alfentanil, respectively. Dynamic linear ranges were in the range of 0.05 to 500 ng/ml for sufentanil and 0.1 to 500 ng/ml for alfentanil. Limits of detection 0.01 and 0.02 ng/ml were obtained for sufentanil and alfentanil, respectively. The percent relative intra‐day and inter‐day standard deviations were found to be less than 8.4% (n = 5). Finally, this method was successfully applied for the separation, preconcentration and determination of trace concentration of sufentanil and alfentanil in plasma and urine samples. Copyright © 2012 John Wiley & Sons, Ltd.  相似文献   

20.
A simple and efficient ultra-miniaturized pipette-tip matrix solid-phase dispersion microextraction using molecular sieve as adsorbent has been developed to simultaneously determine honokiol, magnolol, costunlide and dehydrocostus lactone in a complex Chinese medicine. The types of adsorbent and elution solventswere optimized by single factor experiment. Adsorbent/sample ratio, grinding time and elution volume were optimized by Box-Behnken design (BBD). The optimum extraction is: using SBA-3 as an adsorbent, 200 μL of methanol as elution solvent, 2:1 of sample/adsorbent ratio and 130 s of grinding time. The proposed method applied in real samples provides good linearity (R2 > 0.9999), sufficient accuracy, high reproducibility (RSD<4.93%) and satisfactory recoveries (91.4%–101.4%). Compared with the conventional methods, it is featured with a tiny amount of sample and adsorbent consumption (3 mg of sample and 6 mg of SBA-3) which accompanied with the advantage of rapid, simple, cheap and environment-friendly. Moreover, it shows great potential on analyzing precious or rare amounts of complicated samples.  相似文献   

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