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1.
A novel aptamer‐modified magnetic mesoporous carbon was prepared to develop a specific and sensitive magnetic solid‐phase extraction method through combination with ultra‐high performance liquid chromatography‐tandem mass spectrometry for the analysis chloramphenicol in complex samples. More specifically, the chloramphenicol aptamer‐modified Mg/Al layered double hydroxide magnetic mesoporous carbon was employed as a novel magnetic solid‐phase extraction sorbent for analyte enrichment and sample clean‐up. The extraction solvent, extraction time, desorption solvent, and desorption time were investigated. It was found that the mesoporous structure and aptamer‐based affinity interactions resulted in acceptable selective recognition and a good chemical stability toward trace amounts of chloramphenicol. Upon combination with the ultra‐high performance liquid chromatography‐tandem mass spectrometry technique, a specific and sensitive recognition method was developed with a low limit of detection (0.94 pmol/L, S/N = 3) for chloramphenicol analysis. The developed method was successfully employed for the determination of chloramphenicol in complex serum, milk powders, fish and chicken samples, giving recoveries of 87.0‐107% with relative standard deviations of 3.1‐9.7%.  相似文献   

2.
The application of layered double hydroxide–Al2O3–polymer mixed‐matrix disks for solid‐phase extraction is reported for the first time. Al2O3 is embedded in a polymer matrix followed by an in situ metal‐exchange process to obtain a layered double hydroxide–Al2O3–polymer mixed‐matrix disk with excellent flow‐through properties. The extraction performance of the prepared disks is evaluated as a proof of concept for the automated extraction using sequential injection analysis of organic acids (p‐hydroxybenzoic acid, 3,4‐dihydroxybenzoic acid, gallic acid) following an anion‐exchange mechanism. After the solid‐phase extraction, phenolic acids were quantified by reversed‐phase high‐performance liquid chromatography with diode‐array detection using a core–shell silica–C18 stationary phase and isocratic elution (acetonitrile/0.5% acetic acid in pure water, 5:95, v/v). High sensitivity and reproducibility were obtained with limits of detection in the range of 0.12–0.25 μg/L (sample volume, 4 mL), and relative standard deviations between 2.9 and 3.4% (10 μg/L, = 6). Enrichment factors of 34–39 were obtained. Layered double hydroxide–Al2O3–polymer mixed‐matrix disks had an average lifetime of 50 extractions. Analyte recoveries ranged from 93 to 96% for grape juice and nonalcoholic beer samples.  相似文献   

3.
A hydroxyl‐functionalized ionic liquid, 1‐hydroxyethyl‐3‐methylimidazolium bis(trifluoromethanesulfonyl)imide, was employed in an improved dispersive liquid‐phase microextraction method coupled with ultra high performance liquid chromatography for the enrichment and determination of three estrogens and bisphenol A in environmental water samples. The introduced hydroxyl group acted as the H‐bond acceptor that dispersed the ionic liquid effectively in the aqueous phase without dispersive solvent or external force. Fourier transform infrared spectroscopy indicated that the hydroxyl group of the cation of the ionic liquid enhanced the combination of extractant and analytes through the formation of hydrogen bonds. The improvement of the extraction efficiency compared with that with the use of alkyl ionic liquid was proved by a comparison study. The main parameters including volume of extractant, temperature, pH, and extraction time were investigated. The calibration curves were linear in the range of 5.0–1000 μg/L for estrone, estradiol, and bisphenol A, and 10.0–1000 μg/L for estriol. The detection limits were in the range of 1.7–3.4 μg/L. The extraction efficiency was evaluated by enrichment factor that were between 85 and 129. The proposed method was proved to be simple, low cost, and environmentally friendly for the determination of the four endocrine disruptors in environmental water samples.  相似文献   

4.
A high‐performance liquid chromatographic (HPLC) method with integrated solid‐phase extraction for the determination of 1‐hydroxypyrene and 1‐, 2‐, 3‐, 4‐ and 9‐hydroxyphenanthrene in urine was developed and validated. After enzymatic treatment and centrifugation of 500 μL urine, 100 μL of the sample was directly injected into the HPLC system. Integrated solid‐phase extraction was performed on a selective, copper phthalocyanine modified packing material. Subsequent chromatographic separation was achieved on a pentafluorophenyl core–shell column using a methanol gradient. For quantification, time‐programmed fluorescence detection was used. Matrix‐dependent recoveries were between 94.8 and 102.4%, repeatability and reproducibility ranged from 2.2 to 17.9% and detection limits lay between 2.6 and 13.6 ng/L urine. A set of 16 samples from normally exposed adults was analyzed using this HPLC‐fluorescence detection method. Results were comparable with those reported in other studies. The chromatographic separation of the method was transferred to an ultra‐high‐performance liquid chromatography pentafluorophenyl core–shell column and coupled to a high‐resolution time‐of‐flight mass spectrometer (HR‐TOF‐MS). The resulting method was used to demonstrate the applicability of LC‐HR‐TOF‐MS for simultaneous target and suspect screening of monohydroxylated polycyclic aromatic hydrocarbons in extracts of urine and particulate matter.  相似文献   

5.
A novel bis(indolyl)methane‐modified silica reinforced with multiwalled carbon nanotubes sorbent for solid‐phase extraction was designed and synthesized by chemical immobilization of nitro‐substituted 3,3′‐bis(indolyl)methane on silica modified with multiwalled carbon nanotubes. Coupled with high‐performance liquid chromatography analysis, the extraction properties of the sorbent were evaluated for flavonoids and aromatic organic acid compounds. Under optimum conditions, the sorbent can simultaneously extract five flavonoids and two aromatic organic acid preservatives in aqueous solutions in a single‐step solid‐phase extraction procedure. Wide linear ranges were obtained with correlation coefficients (R2) ranging from 0.9843 to 0.9976, and the limits of detection were in the range of 0.5–5 μg/L for the compounds tested. Compared with the silica modified with multiwalled carbon nanotubes sorbent and the nitro‐substituted 3,3′‐bis(indolyl)methane‐modified silica sorbent, the developed sorbent exhibited higher extraction efficiency toward the selected analytes. The synergistic effect of nitro‐substituted 3,3′‐bis(indolyl)methane and multiwalled carbon nanotubes not only improved the surface‐to‐volume ratio but also enhanced multiple intermolecular interactions, such as hydrogen bonds, π–π, and hydrophobic interactions, between the new sorbent and the selected analytes. The as‐established solid‐phase extraction with high‐performance liquid chromatography and diode array detection method was successfully applied to the simultaneous determination of flavonoids and aromatic organic acid preservatives in grape juices with recoveries ranging from 83.9 to 112% for all the selected analytes.  相似文献   

6.
A novel two‐step extraction technique combining ionic‐liquid‐based dispersive liquid–liquid microextraction with magnetic solid‐phase extraction was developed for the preconcentration and separation of aflatoxins in animal feedstuffs before high‐performance liquid chromatography coupled with fluorescence detection. In this work, ionic liquid 1‐octyl‐3‐methylimidazolium hexafluorophosphate was used as the extractant in dispersive liquid–liquid microextraction, and hydrophobic pelargonic acid modified Fe3O4 magnetic nanoparticles as an efficient adsorbent were applied to retrieve the aflatoxins‐containing ionic liquid. Notably, the target of magnetic nanoparticles was the ionic liquid rather than the aflatoxins. Because of the rapid mass transfer associated with the dispersive liquid–liquid microextraction and magnetic solid phase steps, fast extraction could be achieved. The main parameters affecting the extraction recoveries of aflatoxins were investigated and optimized. Under the optimum conditions, vortexing at 2500 rpm for 1 min in the dispersive liquid–liquid microextraction and magnetic solid‐phase extraction and then desorption by sonication for 2 min with acetonitrile as eluent. The recoveries were 90.3–103.7% with relative standard deviations of 3.2–6.4%. Good linearity was observed with correlation coefficients ranged from 0.9986 to 0.9995. The detection limits were 0.632, 0.087, 0.422 and 0.146 ng/mL for aflatoxins B1, B2, G1, and G2, respectively. The results were also compared with the pretreatment method carried out by conventional immunoaffinity columns.  相似文献   

7.
Ionic liquids have been functionalized for modern applications. The functional ionic liquids are also called task‐specific ionic liquids. Various task‐specific ionic liquids with certain groups have been constructed and exploited widely in the field of separation. To take advantage of their properties in separation science, task‐specific ionic liquids are generally used in techniques such as liquid–liquid extraction, solid‐phase extraction, gas chromatography, high‐performance liquid chromatography, and capillary electrophoresis. This review mainly covers original research papers published in the last five years, and we will focus on task‐specific ionic liquids as the chiral selectors in chiral resolution and as extractant or sensor for biological samples and metal ion purification.  相似文献   

8.
The determination of 15 pyrethroids in soil and water samples was carried out by gas chromatography with mass spectrometry. Compounds were extracted from the soil samples (4 g) using solid–liquid extraction and then salting‐out assisted liquid–liquid extraction. The acetonitrile phase obtained (0.8 mL) was used as a dispersant solvent, to which 75 μL of chloroform was added as an extractant solvent, submitting the mixture to dispersive liquid–liquid microextraction. For the analysis of water samples (40 mL), magnetic solid‐phase extraction was performed using nanocomposites of magnetic nanoparticles and multiwalled carbon nanotubes as sorbent material (10 mg). The mixture was shaken for 45 min at room temperature before separation with a magnet and desorption with 3 mL of acetone using ultrasounds for 5 min. The solvent was evaporated and reconstituted with 100 μL acetonitrile before injection. Matrix‐matched calibration is recommended for quantification of soil samples, while water samples can be quantified by standards calibration. The limits of detection were in the range of 0.03–0.5 ng/g (soil) and 0.09–0.24 ng/mL (water), depending on the analyte. The analyzed environmental samples did not contain the studied pyrethroids, at least above the corresponding limits of detection.  相似文献   

9.
A recent guideline recommends therapeutic drug monitoring for risperidone, paliperidone and olanzapine, which are frequently used second‐generation antipsychotics. We developed a simple high‐performance liquid chromatography–tandem mass spectrometry coupled with an online solid‐phase extraction method that can be used to measure risperidone, paliperidone and olanzapine using small (40 μL) samples. The analytes were extracted from serum samples automatically pre‐concentrated and purified by C8 (5 μm, 2.1 × 30 mm) solid‐phase extraction cartridges, then chromatographed on an Xbidge™ C18 column (3.5 μm, 100 × 2.1 mm) thermostatted at 30°C with a mobile phase consisting of 70% acetonitrile and 30% ammonium hydroxide 1% solution at an isocratic flow rate of 0.3 mL/min, and detected with tandem mass spectrometry. The assay was validated in the concentration range from 2.5 to 160 ng/mL. Intra‐ and inter‐day precision for all analytes was between 1.1 and 8.2%; method accuracy was between 6.6 and 7.6%. The risperidone and paliperidone assay was compared with a high‐performance liquid chromatography‐ultraviolet assay currently used in our hospital for risperidone and paliperidone therapeutic drug monitoring, and the results of weighted Deming regression analysis showed good agreement. For the olanzapine assay, we compared 20 samples in separate re‐assays on different days; all the relative errors were within the 20% recommended limit.  相似文献   

10.
Iron nanoparticles were prepared by a green method following functionalization using 1‐butyl‐3‐methylimidazolium bromide. 1‐Butyl‐3‐methylimidazole iron nanoparticles were characterized using FTIR spectroscopy, energy dispersive X‐ray fluorescence, X‐ray diffraction, scanning electron microscopy and transmission electron microscopy. The nanoparticles were used in solid‐phase membrane micro‐tip extraction to separate vitamin B complex from plasma before high‐performance liquid chromatography. The optimum conditions obtained were sorbent (15 mg), agitation time (30 min), pH (9.0), desorbing solvent [water (5 mL) + methanol (5 mL) + sodium hydroxide (0.1 N) + acetic acid (d = 1.05 kg/L, pH 5.5), desorbing volume (10 mL) and desorption time (30 min). The percentage recoveries of all the eight vitamin B complex were from 60 to 83%. A high‐performance liquid chromatography method was developed using a PhE column (250 × 4.6 mm, 5.0 μm) and water/acetonitrile (95:5, v/v; pH 4.0 with 0.1% formic acid) mobile phase. The flow rate was 1.0 mL/min with detection at 270 and 210 nm. The values of the capacity, separation and resolution factor were 0.57–39.47, 1.12–6.00 and 1.84–26.26, respectively. The developed sample preparation and chromatographic methods were fast, selective, inexpensive, economic and reproducible. The developed method can be applied for analyzing these drugs in biological and environmental matrices.  相似文献   

11.
We describe a rapid and simple microextraction of atrazine from water samples. This method is based on the use of magnetic nanoparticles as sorbents and bioaggregates that are applied to the extraction and preconcentration of atrazine. The resulting magnetic nanoparticles possess a fast adsorption kinetics and high adsorption capacity. Bioaggregates made up of rhaminolipid biosurfactant were assessed as a new strategy for the sample treatment. The extractant was obtained from magnetic nanoparticles using the magnetic solid‐phase extraction method. Then the target analyte was rapidly transferred from the sorbent surface to bioaggregates, which have a low toxicity and are green and ecofriendly. Finally, the extract is centrifuged and transferred to micro‐syringe for analysis by high‐performance liquid chromatography. Experimental parameters affecting the extraction efficiency were studied and optimized. Under optimum conditions the enrichment factor was 268. The linear dynamic range and limit of detection were 0.1–50 and 0.033 μg/L, respectively. The relative standard deviation for six replicate measurements was 5.3%. The results demonstrate good applicability of biosorption‐assisted magnetic solid‐phase extraction method for the determination of atrazine from water samples.  相似文献   

12.
We describe a highly sensitive micro‐solid‐phase extraction method for the pre‐concentration of six phthalate esters utilizing a TiO2 nanotube array coupled to high‐performance liquid chromatography with a variable‐wavelength ultraviolet visible detector. The selected phthalate esters included dimethyl phthalate, diethyl phthalate, dibutyl phthalate, butyl benzyl phthalate, bis(2‐ethylhexyl)phthalate and dioctyl phthalate. The factors that would affect the enrichment, such as desorption solvent, sample pH, salting‐out effect, extraction time and desorption time, were optimized. Under the optimum conditions, the linear range of the proposed method was 0.3–200 μg/L. The limits of detection were 0.04–0.2 μg/L (S/N = 3). The proposed method was successfully applied to the determination of six phthalate esters in water samples and satisfied spiked recoveries were achieved. These results indicated that the proposed method was appropriate for the determination of trace phthalate esters in environmental water samples.  相似文献   

13.
An efficient on‐site extraction technique to determine carcinogenic heterocyclic aromatic amines in seawater has been reported. A micro‐solid‐phase extraction device placed inside a portable battery‐operated pump was used for the on‐site extraction of seawater samples. Before on‐site applications, parameters that influence the extraction efficiency (extraction time, type of sorbent materials, suitable desorption solvent, desorption time, and sample volume) were investigated and optimized in the laboratory. The developed method was then used for the on‐site sampling of heterocyclic aromatic amines determination in seawater samples close to distillation plant. Once the on‐site extraction completed, the small extraction device with the analytes was brought back to the laboratory for analysis using high‐performance liquid chromatography with fluorescence detection. Based on the optimized conditions, the calibration curves were linear over the concentration range of 0.05–20 μg/L with correlation coefficients up to 0.996. The limits of detection were 0.004–0.026 μg/L, and the reproducibility values were between 1.3 and 7.5%. To evaluate the extraction efficiency, a comparison was made with conventional solid‐phase extraction and it was applied to various fortified real seawater samples. The average relative recoveries obtained from the spiked seawater samples varied in the range 79.9–95.2%.  相似文献   

14.
In this research, a carbon nanotube/layered double hydroxide nanocomposite was synthesized by an in situ growth route by electrostatic force. The prepared carbon nanotube/layered double hydroxide nanocomposite was successfully prepared and deposited on a stainless‐steel wire for the fabrication of the solid‐phase microextraction fiber. The fiber was evaluated for the extraction of phenolic compounds from water samples. Analytical merits of the method, under optimum conditions (extraction temperature: 75°C, extraction time: 30 min, desorption time: 2 min, desorption temperature 260°C, salt concentration: 10% w/v) are 0.01–300 ng/mL for the linear dynamic range and 0.005–0.08 for the limit of detection. In optimum conditions, the repeatability for one fiber (n = 3), expressed as relative standard deviation, was between 6.5 and 9.9% for the phenolic compounds.  相似文献   

15.
Most organotin compounds that have been widely used in food packaging materials and production process show serious toxicity effects to human health. In this study, a simple and low‐cost method based on high‐performance liquid chromatography with inductively coupled plasma mass spectrometry for the simultaneous determination of four organotins in edible vegetable oil samples was developed. Four organotins including dibutyltin dichloride, tributyltin chloride, diphenyltin dichloride, and triphenyltin chloride were simultaneously extracted with methanol using the low‐temperature precipitation process. After being concentrated, the extracts were purified by matrix solid‐phase dispersion using graphitized carbon black. The experimental parameters such as extraction solvent and clean‐up material were optimized. To evaluate the accuracy of the new method, the recoveries were investigated. In addition, a liquid chromatography with tandem mass spectrometry method was also proposed for comparison. The procedures of extracting and purifying samples for the analysis were simple and easy to perform batch operations, also showed good efficiency with lower relative standard deviation. The limits of detection of the four organotins were 0.28–0.59 μg/L, and the limits of quantification of the four organotins were 0.93–1.8 μg/L, respectively. The proposed method was successfully applied to the simultaneous analysis of the four organotins in edible vegetable oil. Some analytes were detected at the level of 2.5–28.8 μg/kg.  相似文献   

16.
In this study, a method coupling turbulent flow chromatography with online solid‐phase extraction and high‐performance liquid chromatography with tandem mass spectrometry was developed for analyzing the lignans in Magnoliae Flos. By the online pretreatment of turbulent flow chromatography solid‐phase extraction, the impurities removal and analytes concentration were automatically processed, and the lignans were separated rapidly and well. Seven lignans of Magnoliae Flos including epieudesmin, magnolin, 1‐irioresinol‐B‐dimethyl ether, epi‐magnolin, fargesin aschantin, and demethoxyaschantin were identified by comparing their retention behavior, UV spectra, and mass spectra with those of reference substances or literature data. The developed method was validated, and the good results showed that the method was not only automatic and rapid, but also accurate and reliable. The turbulent flow chromatography with online solid‐phase extraction and high‐performance liquid chromatography with tandem mass spectrometry method holds a high potential to become an effective method for the quality control of lignans in Magnoliae Flos and a useful tool for the analysis of other complex mixtures.  相似文献   

17.
In the present study, a novel configuration of liquid‐phase microextraction was proposed, in which a magnetic stirrer with a groove was used as the extractant phase holder. It was termed as magnetic stirrer liquid‐phase microextraction. In this way, the stability of the organic solvent was much improved under high stirring speed; the extraction efficiency was enhanced due to the enormously enlarged contact area between the organic solvent and aqueous phase. The extraction performance of the magnetic stirrer liquid‐phase microextraction was studied using chlorobenzenes as the probe analytes. A wide linearity range (20 pg/mL to 200 ng/mL) with a satisfactory linearity coefficient (r2 > 0.998) was obtained. Limits of detection ranged from 9.0 to 12.0 pg/mL. Good reproducibility was achieved with intra‐ and inter‐day relative standard deviations <4.8%. The proposed magnetic stirrer liquid‐phase microextraction was simple, environmentally friendly and efficient; compared to single‐drop microextraction, it had obvious advantages in terms of reproducibility and extraction efficiency. It is a promising miniaturized liquid‐phase technology for real applications.  相似文献   

18.
The feasibility of developing a quick, easy, efficient procedure for the simultaneous determination of organochlorinated pesticides and polychlorinated biphenyls in aquatic samples using gas chromatography with electron capture detection based on solid‐phase extraction was investigated. The extraction solvent (n‐hexane/acetone, cyclohexane/ethyl acetate, n‐hexane/dichloromethane, n‐hexane) for ultrasound‐assisted solid–liquid extraction and solid‐phase extraction columns (florisil, neutral alumina, acidic alumina, aminopropyl trimethoxy silane, propyl ethylenediamine, aminopropyl trimethoxy silane/propyl ethylenediamine, graphitized carbon black and silica) for cleanup procedure were optimized. The gas chromatography with electron capture detection method was validated in terms of linearity, sensitivity, reproducibility, and recovery. Mean recoveries ranged from 75 to 115% with relative standard deviations <13%. Quantification limits were 0.20–0.40 ng/g for organochlorinated pesticides and polychlorinated biphenyls. The satisfactory data demonstrated the good reproducibility of the method with relative standard deviations lower than 13%. In comparison to other related methods, this method requires less time and solvent and allows for rapid isolation of the target analytes with high selectivity. This method therefore allows for the screening of numerous samples and can also be used for routine analyses.  相似文献   

19.
Solid‐phase extraction coupled with dispersive liquid–liquid microextraction was developed as an ultra‐preconcentration method for the determination of four organophosphorus pesticides (isocarbophos, parathion‐methyl, triazophos and fenitrothion) in water samples. The analytes considered in this study were rapidly extracted and concentrated from large volumes of aqueous solutions (100 mL) by solid‐phase extraction coupled with dispersive liquid–liquid microextraction and then analyzed using high performance liquid chromatography. Experimental variables including type and volume of elution solvent, volume and flow rate of sample solution, salt concentration, type and volume of extraction solvent and sample solution pH were investigated for the solid‐phase extraction coupled with dispersive liquid–liquid microextraction with these analytes, and the best results were obtained using methanol as eluent and ethylene chloride as extraction solvent. Under the optimal conditions, an exhaustive extraction for four analytes (recoveries >86.9%) and high enrichment factors were attained. The limits of detection were between 0.021 and 0.15 μg/L. The relative standard deviations for 0.5 μg/L of the pesticides in water were in the range of 1.9–6.8% (n = 5). The proposed strategy offered the advantages of simple operation, high enrichment factor and sensitivity and was successfully applied to the determination of four organophosphorus pesticides in water samples.  相似文献   

20.
A rapid analytical method based on online solid‐phase extraction with high‐performance liquid chromatography and mass spectrometry has been established and applied to the determination of tannin compounds that may cause adverse effects in traditional Chinese medicine injections. Different solid‐phase extraction sorbents have been compared and the elution buffer was optimized. The performance of the method was verified by evaluation of recovery (≥40%), repeatability (RSD ≤ 6%), linearity (r2 ≥ 0.993), and limit of quantification (≤0.35 μg/mL). Five tannin compounds, gallic acid, cianidanol, gallocatechin gallate, ellagic acid, and penta‐O‐galloylglucose, were identified with concentrations ranging from 3.1–37.4 μg/mL in the analyzed traditional Chinese medicine injections.  相似文献   

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