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1.
A novel microporous membrane/solvent microextraction (MPMSME) approach was developed in which a piece of microporous filter membrane was used as not only extraction solvent holder but also solid phase extraction unit. Subsequently, high-performance liquid chromatography with an UV detector was conducted. The wide exchange surface and very little organic solvent consumption made this sample pretreatment technology very interesting. The cinnamic acid derivatives were used as model analytes to evaluate the procedure. Parameters that affect the MPMSME such as type of extraction solvent, membrane area (or volumes of extraction solvent), aqueous phase pH, ionic strength, extraction stirring rate, extraction time, and sample volume were investigated and optimized. The enrichment factor (EF) of analyte was defined in MPMSME. Under the optimized conditions, the EFs of cinnamic acid derivatives were 43–144. Good linearities were obtained from 4 to 4,000 ng mL?1 for all the analytes with regression coefficients of between 0.9956 and 0.9977; the limits of quantification were below 0.4 ng mL?1, and satisfactory recoveries (93–106 %) and precisions (0.37–13 %) were also achieved. The experimental results showed that the method was simple, rapid, practical, and effective for preconcentration and determination of the cinnamic acid derivatives in rhizoma typhonii.  相似文献   

2.
A novel graphene/dodecanol floating solidification microextraction followed by HPLC with diode‐array detection has been developed to extract trace levels of four cinnamic acid derivatives in traditional Chinese medicines. Several parameters affecting the performance were investigated and optimized. Also, possible microextraction mechanism was analyzed and discussed. Under the optimum conditions (amount of graphene in dodecanol: 0.25 mg/mL; volume of extraction phase: 70 μL; pH of sample phase: 3; extraction time: 30 min; stirring rate: 1000 rpm; salt amount: 26.5% NaCl; volume of sample phase: 10 mL, and without dispersant addition), the enrichment factors of four cinnamic acid derivatives ranged from 26 to 112, the linear ranges were 1.0 × 10−2–10.0 μg/mL for caffeic acid, 1.3 × 10−3–1.9 μg/mL for p‐hydroxycinnamic acid, 2.8 × 10−3–4.1 μg/mL for ferulic acid, and 2.7 × 10−3–4.1 μg/mL for cinnamic acid, with r 2 ≥ 0.9993. The detection limits were found to be in the range of 0.1–1.0 ng/mL, and satisfactory recoveries (92.5–111.2%) and precisions (RSDs 1.1–9.5%) were also achieved. The results showed that the approach is simple, effective and sensitive for the preconcentration and determination of trace levels of cinnamic acid derivatives in Chinese medicines. The proposed method was compared with conventional dodecanol floating solidification microextraction and other extraction methods.  相似文献   

3.
A novel three‐phase hollow fiber liquid‐phase microextraction was developed based on reverse micelle as extraction solvent and acceptor phase, and compared with conventional two‐phase hollow fiber liquid‐phase microextraction. Both procedures were used in the extraction and concentration of four cinnamic acids (caffeic acid, p‐hydroxycinnamic acid, ferulic acid, and cinnamic acid) in traditional Chinese medicines prior to high‐performance liquid chromatography analysis. Parameters affecting the two procedures were investigated and optimized to obtain the optimum enrichment factors. The mechanism of the developed procedure was explored and elucidated by comparison with conventional two‐phase hollow fiber liquid‐phase microextraction. Under the optimized conditions, the analytes’ enrichment factors were between 50 and 118 for the proposed procedure, and 31–96 for conventional two‐phase mode. Satisfactory linear ranges (r2 ≥ 0.99), detection limits (0.1–0.6 ng/mL), precisions (<9.2%), and accuracies (recoveries: 80–123.1%) were observed for the two procedures. The results showed that the enrichment capacity of the proposed procedure for the cinnamic acids is better than that of conventional two‐phase procedure, and both are eco‐friendly, simple, and effective for the enrichment and detection of cinnamic acids in traditional Chinese medicines.  相似文献   

4.
A sodium dodecyl sulfate sensitized switchable solvent liquid‐phase microextraction method was developed and applied to the preconcentration of active alkaloids in Rhizoma coptidis followed by high performance liquid chromatography determination. Before extraction, nonionic triethylamine was converted to its cationic form in the presence of carbon dioxide. Then, the ionic solvent carrying target analytes was once more reverted to its nonionic form by adding sodium hydroxide, as well as phase separation and analytes enrichment were realized simultaneously. Several parameters affecting the approach, such as concentration of sodium dodecyl sulfate, extraction solvent volume, sodium hydroxide concentration, sample phase pH, injection solvent type, and extraction time, were investigated and optimized. The possible microextraction mechanism of double micelle supramolecular inclusion was explored. Under the optimum conditions, the enrichment factors of four protoberberine alkaloids were from 101.8 to 152.0. The linear ranges (with r≥ 0.990) were 0.032–4.23, 0.031–4.33, 0.0026–10.04, and 0.0013–4.13 μg/mL for epiberberine, coptisine, palmatine, and berberine, respectively. The detection limits were in the range of 0.16–0.32 ng/mL. Satisfactory accuracies (recoveries 98.8–104.6%) and precisions (RSDs 1.9–10.9%) were also obtained. The results showed that the approach is rapid, effective, eco‐friendly, and easy‐to‐handle for the enrichment and detection of active alkaloids in Rhizoma coptidis.  相似文献   

5.
A novel stirrer‐liquid/solid microextraction method was developed for the separation and enrichment of trace levels of curcumin, bisdemethoxycurcumin, and demethoxycurcumin in Rhizoma Curcumae Longae, Radix Curcumae, and Rhizoma Curcumae before their analysis by high‐performance liquid chromatography with ultraviolet detection. In the proposed approach, a magnetic stirrer was immersed in decanol to coat its surface completely with decanol, which was used as an extraction platform. The stirrer coated with decanol is not only a power to agitate the sample solution to constantly update the sample on the stirrer surface but also it can adsorb and extract the target analytes. Some effective parameters, including suitable superficial area of stirrer, extraction solvent, sample phase pH, NaCl concentration, stirring rate, extraction time, sample phase volume, were analyzed and selected. Under the optimal conditions, the linearities are 0.0044–2.20 μg/mL, detection limits are 0.3–0.6 ng/mL, and the extraction content per unit length and enrichment factors of the target analytes are 6.24–9.71/mm and 589–917, respectively. Also, the stirrer‐liquid/solid microextraction mechanism for the extraction and enrichment of the target analytes was analyzed and expounded. The results showed that stirrer‐liquid/solid microextraction is a simple, rapid sample pretreatment approach with a high enrichment factor.  相似文献   

6.
A low‐cost and simple cooling‐assisted headspace liquid‐phase microextraction device for the extraction and determination of 2,6,6‐trimethyl‐1,3 cyclohexadiene‐1‐carboxaldehyde (safranal) in Saffron samples, using volatile organic solvents, was fabricated and evaluated. The main part of the cooling‐assisted headspace liquid‐phase microextraction system was a cooling capsule, with a Teflon microcup to hold the extracting organic solvent, which is able to directly cool down the extraction phase while the sample matrix is simultaneously heated. Different experimental factors such as type of organic extraction solvent, sample temperature, extraction solvent temperature, and extraction time were optimized. The optimal conditions were obtained as: extraction solvent, methanol (10 μL); extraction temperature, 60°C; extraction solvent temperature, 0°C; and extraction time, 20 min. Good linearity of the calibration curve (R2 = 0.995) was obtained in the concentration range of 0.01–50.0 μg/mL. The limit of detection was 0.001 μg/mL. The relative standard deviation for 1.0 μg/mL of safranal was 10.7% (n = 6). The proposed cooling‐assisted headspace liquid‐phase microextraction device was coupled (off‐line) to high‐performance liquid chromatography and used for the determination of safranal in Saffron samples. Reasonable agreement was observed between the results of the cooling‐assisted headspace liquid‐phase microextraction high‐performance liquid chromatography method and those obtained by a validated ultrasound‐assisted solvent extraction procedure.  相似文献   

7.
A new hollow‐fiber double‐solvent synergistic microextraction method was proposed for the extraction and concentration of trace active compounds in traditional Chinese medicine. The main variables affecting the method were investigated and optimized. Under the optimized conditions, linearities were 0.01–10 μg/mL, detection limits were lower than 0.8 ng/mL, and interday, and intraday relative standard deviations were <9.20%. Furthermore, average recoveries ranged from 102.8 to 104.1%, and enrichment factors were 6–70 for the four alkaloids tested. The antitumor alkaloid group in Coptis chinensis was screened and identified by hollow‐fiber cell fishing with high‐performance liquid chromatography. The four alkaloids were then enriched and quantified by hollow‐fiber double‐solvent synergistic microextraction with high‐performance liquid chromatography. The mechanism of the proposed microextraction method was described, and results demonstrated that the approach was a simple and reliable sample‐preparation procedure. This method, as well as hollow‐fiber cell fishing combined with high‐performance liquid chromatography can be adopted to study the different characteristic effects of the multiple components and multiple targets of traditional Chinese medicine. The approach can also be used to conduct tailored quality control of the active compounds associated with therapeutic efficacy.  相似文献   

8.
We developed a CE and ultrasound‐assisted temperature‐controlled ionic liquid emulsification microextraction method for the determination of four parabens (methyl paraben, ethyl paraben, propyl paraben, and butyl paraben) in personal care products including mouthwash and toning lotion. In the proposed extraction procedure, ionic liquid (IL, 1‐octyl‐3‐methylimidazolium hexafluorophosphate) was used as extraction solvent, moreover, no disperser solvent was needed. Parameters affecting the extraction efficiency including volume of IL, heating temperature, ultrasonic time, extraction time, sample pH, ionic strength, and centrifugation time were optimized. Under the optimized conditions, the method was found to be linear over the range of 3–500 ng/mL with coefficient of determination (R2) in the range of 0.9990–0.9998. The LODs and LOQs for the four parabens were 0.45–0.72 ng/mL and 1.50–2.40 ng/mL, respectively. Intraday and interday precisions (RSDs, n = 5) were in the range of 5.4–6.8% and 7.0–8.7%, respectively. The recoveries of parabens at different spiked levels ranged from 71.9 to 119.2% with RSDs less than 9.5%.  相似文献   

9.
A simple, rapid, and efficient method, dispersive liquid–liquid microextraction (DLLME) coupled with high‐performance liquid chromatography‐fluorescence detector, has been developed for the determination of guaifenesin (GUA) enantiomers in human urine samples after an oral dose administration of its syrup formulation. Urine samples were collected during the time intervals 0–2, 2–4, and 4–6 h and concentration and ratio of two enantiomers was determined. The ratio of R‐(?) to S‐(+) enantiomer concentrations in urine showed an increase with time, with R/S ratios of 0.66 at 2 h and 2.23 at 6 h. For microextraction process, a mixture of extraction solvent (dichloromethane, 100 μL) and dispersive solvent (THF, 1 mL) was rapidly injected into 5.0 mL diluted urine sample for the formation of cloudy solution and extraction of enantiomers into the fine droplets of CH2Cl2. After optimization of HPLC enantioselective conditions, some important parameters, such as the kind and volume of extraction and dispersive solvents, extraction time, temperature, pH, and salt effect were optimized for dispersive liquid–liquid microextraction process. Under the optimum extraction condition, the method yields a linear calibration curve in the concentration range from 10 to 2000 ng/mL for target analytes. LOD was 3.00 ng/mL for both of the enantiomers.  相似文献   

10.
A new robust method of electromembrane‐surrounded solid‐phase microextraction coupled to ion mobility mass spectrometry was applied for nonsteroidal anti‐inflammatory drugs determination in complex matrices. This is the first time that a graphene/polyaniline composite coating is applied in electromembrane‐surrounded solid‐phase microextraction method. The homemade graphene/polyaniline composite is characterized by a high electrical conductivity and thermal stability. The variables affecting electromembrane‐surrounded solid‐phase microextraction, including extraction time; applied voltage and pH were optimized through chemometric methods, central composite design, and response surface methodology. Under the optimized conditions, limits of detection of 0.04 and 0.05 ng/mL were obtained for mefenamic acid and ibuprofen, respectively. The feasibility of electromembrane‐surrounded solid‐phase microextraction followed by ion mobility mass spectrometry was successfully confirmed by the extraction and determination of low levels of ibuprofen and mefenamic acid in human urine and plasma samples and satisfactory results were obtained.  相似文献   

11.
A new and fast sample preparation technique based on three‐phase hollow fiber liquid‐phase microextraction with a magnetofluid was developed and successfully used to quantify the aristolochic acid I (AA‐I) and AA‐II in plasma after oral administration of Caulis akebiae extract. Analysis was accomplished by reversed‐phase high‐performance liquid chromatography with fluorescence detection. Parameters that affect the hollow fiber liquid‐phase microextraction processes, such as the solvent type, pH of donor and acceptor phases, content of magnetofluid, salt content, stirring speed, hollow fiber length, extraction temperature, and extraction time, were investigated and optimized. Under the optimized conditions, the preconcentration factors for AA‐I and AA‐II were >627. The calibration curve for two AAs was linear in the range of 0.1–10 ng/mL with the correlation coefficients >0.9997. The intraday and interday precision was <5.71% and the LODs were 11 pg/mL for AA‐I and 13 pg/mL for AA‐II (S/N = 3). The separation and determination of the two AAs in plasma after oral administration of C. akebiae extract were completed by the validated method.  相似文献   

12.
An efficient, inexpensive and environmentally benign ultrasound‐assisted supramolecular‐solvent‐based microextraction technique combined with high‐performance liquid chromatography was used for the determination of chlorophenols in environmental water samples. Different factors such as amount of decanoic acid, volume of tetrahydrofuran, pH of the sample, ultrasound time and ionic strength were investigated and optimized. The optimized extraction conditions were 60 mg decanoic acid, 1.5 mL tetrahydrofuran, 3 min ultrasound time, without salt addition. Under this condition, the extraction recoveries were 83.0–89.3 with preconcentration factors of 94–102. The calibration curves were linear from 5.0–400.0 ng/mL with square of the correlation coefficient higher than 0.9998 and the limits of detection were between 1.5–2.0 ng/mL. The values of intra‐ and inter‐day relative standard deviations were 3.2–6.0 and 7.3–8.0%, respectively. Analysis of different samples showed that the concentration of 2,5‐dichlorophenol in Babolrood river water was 80.6 ng/mL.  相似文献   

13.
The simultaneous determination of amphetamine and methadone was carried out by magnetic graphene oxide nanoparticles, a magnetic solid‐phase extraction adsorbent, as a new sample treatment technique. The main factors (the amounts of sample volume, amount of adsorbent, type and amount of extraction organic solvent, time of extraction and desorption, pH, the ionic strength of extraction medium, and agitation rate) influencing the extraction efficiency were investigated and optimized. Under the optimized conditions, good linearity was observed in the range of 100–1500 ng/mL for amphetamine and 100–1000 ng/mL for methadone. The method was evaluated for determination of AM and methadone in positive urine samples, satisfactory results were obtained, therefore magnetic solid‐phase extraction can be applied as a novel method for the determination of drugs of abuse in forensic laboratories.  相似文献   

14.
For the first time, the high‐density solvent‐based solvent de‐emulsification dispersive liquid–liquid microextraction (HSD‐DLLME) was developed for the fast, simple, and efficient determination of chlorophenols in water samples followed by field‐enhanced sample injection with reverse migrating micelles in CE. The extraction of chlorophenols in the aqueous sample solution was performed in the presence of extraction solvent (chloroform) and dispersive solvent (acetone). A de‐emulsification solvent (ACN) was then injected into the aqueous solution to break up the emulsion, the obtained emulsion cleared into two phases quickly. The lower layer (chloroform) was collected and analyzed by field‐enhanced sample injection with reverse migrating micelles in CE. Several important parameters influencing the extraction efficiency of HSD‐DLLME such as the type and volume of extraction solvent, disperser solvent and de‐emulsification solvent, sample pH, extraction time as well as salting‐out effects were optimized. Under the optimized conditions, the proposed method provided a good linearity in the range of 0.02–4 μg/mL, low LODs (4 ng/mL), and good repeatability of the extractions (RSDs below 9.3%, n = 5). And enrichment factors for three phenols were 684, 797, and 233, respectively. This method was then utilized to analyze two real environmental samples from wastewater and tap water and obtained satisfactory results. The obtained results indicated that the developed method is an excellent alternative for the routine analysis in the environmental field.  相似文献   

15.
A simple and rapid method using microextraction by packed sorbent coupled with gas chromatography and mass spectrometry has been developed for the analysis of five phthalates, namely, diethyl phthalate, benzyl‐n‐butyl phthalate, dicyclohexyl phthalate, di‐n‐butyl phthalate, and di‐n‐propyl phthalate, in cold drink and cosmetic samples. The various parameters that influence the microextraction by packed sorbent performance such as extraction cycle (extract–discard), type and amount of solvent, washing solvent, and pH have been studied. The optimal conditions of microextraction using C18 as the packed sorbent were 15 extraction cycles with water as washing solvent and 3 × 10 μL of ethyl acetate as the eluting solvent. Chromatographic separation was also optimized for injection temperature, flow rate, ion source, interface temperature, column temperature gradient and mass spectrometry was evaluated using the scan and selected ion monitoring data acquisition mode. Satisfactory results were obtained in terms of linearity with R2 >0.9992 within the established concentration range. The limit of detection was 0.003–0.015 ng/mL, and the limit of quantification was 0.009–0.049 ng/mL. The recoveries were in the range of 92.35–98.90% for cold drink, 88.23–169.20% for perfume, and 88.90–184.40% for cream. Analysis by microextraction by packed sorbent promises to be a rapid method for the determination of these phthalates in cold drink and cosmetic samples, reducing the amount of sample, solvent, time and cost.  相似文献   

16.
Graphene‐based pipette tip solid‐phase extraction was combined with ultra‐high performance liquid chromatography and tandem mass spectrometry for the determination of carbamate pesticide residues in fruit juice samples. Four milligrams of graphene was used as sorbent material to pack a 1000 μL pipette tip for the extraction of pirimicarb, propoxur, isoprocarb, fenobucarb, and diethofencarb from 3 mL of fruit juice sample. The whole extraction process was finished in 12 min, and the volume of eluent used was only 1.5 mL. Under the optimized conditions, good linear relationship (R > 0.999) and lower limits of detection (0.0022–0.033 ng/mL) were achieved. The recoveries at three spiked levels ranged from 80.90 to 124.60% with relative standard deviations less than 4.88%. Compared with commercially available sorbents including propylsulfonic acid silica, graphitized carbon black, and C18, graphene was superior in extraction efficiency. The proposed method is simple, rapid, sensitive, selective, and solvent saving.  相似文献   

17.
In the present study, graphene oxide reinforced two‐phase electromembrane extraction (EME) coupled with gas chromatography was applied for the determination of methamphetamine as a model analyte in biological samples. The presence of graphene oxide in the hollow fiber wall can increase the effective surface area, interactions with analyte and polarity of support liquid membrane that leads to an enhancement in the analyte migration. To investigate the influence of the presence of graphene oxide in the support liquid membrane on the extraction efficiency, a comparative study was performed between graphene oxide and graphene oxide/EME methods. The extraction parameters such as type of organic solvent, pH of the donor phase, stirring speed, time, voltage, salt addition and the concentration of graphene oxide were optimized. Under the optimum conditions, the proposed microextraction technique provided low limit of detection (2.4 ng/mL), high preconcentration factor (195–198) and high relative recovery (95–98.5%). Finally, the method was successfully employed for the determination of methamphetamine in urine and hair samples.  相似文献   

18.
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   

19.
A sensitive and rapid method based on alcohol‐assisted dispersive liquid–liquid microextraction followed by high‐performance liquid chromatography for the determination of fluoxetine in human plasma and urine samples was developed. The effects of six parameters on the extraction recovery were investigated and optimized utilizing Plackett–Burman design and Box–Benken design, respectively. According to the Plackett–Burman design results, the volume of disperser solvent, extraction time, and stirring speed had no effect on the recovery of fluoxetine. The optimized conditions included a mixture of 172 μL of 1‐octanol as extraction solvent and 400 μL of methanol as disperser solvent, pH of 11.3 and 0% w/v of salt in the sample solution. Replicating the experiment in optimized condition for five times, gave the average extraction recoveries equal to 90.15%. The detection limit of fluoxetine in human plasma was obtained 3 ng/mL, and the linearity was in the range of 10–1200 ng/mL. The corresponding values for human urine were 4.2 ng/mL with the linearity range from 10 to 2000 ng/mL. Relative standard deviations for intra and inter day extraction of fluoxetine were less than 7% in five measurements. The developed method was successfully applied for the determination of fluoxetine in human plasma and urine samples.  相似文献   

20.
研究了离子液体分散液相微萃取(ILDLPME)机理, 建立了简单、快速、灵敏的ILDLPME-HPLC(高效液相色谱)同时测定中药白附子中5种低丰度苯丙烯酸类化合物含量的方法, 对不同产地白附子的质量进行了比较和评价. 在最佳的ILDLPME-HPLC条件下, 测得咖啡酸的线性范围为1.28×10-3~2.60 μg/mL, 对羟基桂皮酸及阿魏酸的线性范围为1.28×10-4~2.60 μg/mL, 桂皮酸及对甲氧基桂皮酸的线性范围为1.28×10-3~4.00 μg/mL, 检出限分别为0.13, 0.01, 0.01, 0.13和0.13 ng/mL, 日内精密度RSD<7.9%, 日间精密度RSD<9.7%, 药材中分析物的回收率在86.9%~112.6%之间, ILDLPME 对5种分析物的富集倍数分别在56.0~159.3倍之间. 结合5种苯丙烯酸类化合物ILDLPME萃取前后紫外光谱的变化, 提出了ILDLPME萃取苯丙烯酸羧基-离子液体电荷转移超分子(CTSMCIL)机理. 本研究为建立中药白附子的质量控制方法提供了理论依据和实验基础.  相似文献   

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