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1.
ABSTRACT

In this work, a novel layered sorbent for microextraction by packed sorbent (MEPS) was introduced, which has been prepared by coating graphene oxide/polyamide (GO/PA) nanocomposite (NC) onto cellulose paper through solvent exchange method. Scanning electron microscopy (SEM) was applied to investigate the surface characteristic and morphology of PA and GO/PA NC coated on cellulose paper. The prepared MEPS device was used for extraction of organophosphorous pesticides (OPPs) including chlorpyrifos, fenthion, fenithrothion, ethion, edifenphos and phosalone in environmental aqueous samples followed by detection using gas chromatography-flame ionisation detector (GC-FID). Important parameters affecting the MEPS method including pH of sample solution, extraction draw-discard cycles, sorbent layers, desorption solvent volume and desorption draw-eject number were studied and optimised using central composite design (CCD). Based on the method validation, limits of detection (LODs) were in the range of 0.2–1 µg L?1. The calibration graphs for chlorpyrifos, fenthion and edifenphos are linear in the concentration range of 1 to 500 µg L?1; for ethion and phosalone are linear in the range of 1–1000 µg L?1 and for fenithrothion is linear in the range of 3–1000 µg L?1. The method precision (RSD %) with six replicates determinations was in the range of 3 to 9.4 % and 3.9 to 11.9% for distilled water and spiked river water sample, respectively, at the concentration level of 300 µg L?1 . The developed method was applied successfully to determine OPP compounds in river, dam and tap water samples; accordingly, the relative recoveries (RR%) were obtained in the range of 77.8 to 113.3%.  相似文献   

2.
建立了超声辅助基质分散液-液微萃取(UA-DLLME)/气相色谱-串联质谱(GC-MS)同时测定地下和地表水中15种硝基苯、19种苯胺和14种邻苯二甲酸酯类化合物的分析方法。采用Plackett-Burman设计从萃取剂、分散剂体积、萃取温度、萃取时间和离子强度等变量中筛选最显著的影响因素,并利用中心组合设计(CCD)结合响应曲面图优化显著因素,最终确定最佳的萃取条件：10mL水样在2g/LNaCl条件下迅速加入0.65mL乙腈(分散剂)和40μL四氯化碳(萃取剂),于40℃超声2min,混合液以3500r/min离心3min。结果显示,目标分析物在1~200μg/L质量浓度范围内线性良好,相关系数不低于0.9958,方法的检出限(MDL)为0.001~0.030μg/L,定量下限(LOQ)为0.004~0.120μg/L,在低、中、高3个加标浓度下的平均回收率为77.4%~113%,相对标准偏差(RSD)均不高于9.6%(n=6)。  相似文献   

3.
    
This study aimed to design an effective nanoparticle-based carrier for the oral delivery of fisetin (FST) with improved biopharmaceutical properties. FST-loaded nanoparticles were prepared with polyvinyl alcohol (PVA) and poly(lactic-co-glycolic acid) (PLGA) by the interfacial deposition method. A central composite design of two independent variables, the concentration of PVA and the amount of PLGA, was applied for the optimization of the preparative parameter. The responses, including average particle size, polydispersity index, encapsulation efficiency, and zeta potential, were assessed. The optimized formulation possessed a mean particle size of 187.9 nm, the polydispersity index of 0.121, encapsulation efficiency of 79.3%, and zeta potential of −29.2 mV. The morphological observation demonstrated a globular shape for particles. Differential scanning calorimetry and powder X-ray diffraction studies confirmed that the encapsulated FST was presented as the amorphous state. The dissolution test indicated a 3.06-fold increase for the accumulating concentrations, and the everted gut sac test showed a 4.9-fold gain for permeability at the duodenum region. In conclusion, the optimized FST-loaded nanoparticle formulation in this work can be developed as an efficient oral delivery system of FST to improve its biopharmaceutic properties.  相似文献   

4.
    
In this research, sponge-activated carbon was applied as an effective adsorbent for simultaneous dispersive solid ultrasound-assisted microextraction followed by high-performance liquid chromatography for the preconcentration and determination of losartan (LOS) and chlordiazepoxide (CDP) drugs from urine and plasma samples. The synthesized adsorbent was characterized using scanning electron microscopy and Brunauer–Emmett–Teller techniques. To investigate the effects of different parameters, such as adsorbent dosage, pH, adsorption time, and volume of extraction solvent on the extraction process of LOS and CDP, a central composite design (CCD)-based response surface methodology was applied. Using a CCD, the optimized factors achieved an adsorption time of 13 min, an adsorbent dosage of 14 mg, an extraction solvent (methanol) of 1.3 mL, and pH = 4.7 under the desirability function. Under the optimized conditions, the presented method showed a wide linear range of 0.005–10.0 μg/mL with a limit of detections of 0.0011 and 0.0018 μg/mL for LOS and CDP, respectively. Moreover, the applied method had relative standard deviations of 4.7% and 5.3% for LOS and CDP, respectively.  相似文献   

5.
    
A brand-new nano-crystal (NC) version of the hydrophobic drug Paclitaxel (PT) were formulated for cancer treatment. A stable NC formulation for the administration of PT was created using the triblock co-polymer Pluronic F127. To achieve maximum entrapment effectiveness and minimal particle size, the formulation was improved using the central composite design by considering agitation speed and vacuum pressure at five levels (coded as +1.414, +1, 0, −1, and −1.414). According to the Design Expert software’s predictions, 13 runs were created and evaluated for the chosen responses. The formulation prepared with an agitation speed of 1260 RPM and a vacuum pressure of 77.53 mbar can meet the requirements of the ideal formulation in order to achieve 142.56 nm of PS and 75.18% EE, according to the level of desirability (D = 0.959). Folic acid was conjugated to Pluronic F127 to create folate receptor-targeted NC. The drug release profile of the nano-crystals in vitro demonstrated sustained release over an extended period. Folate receptor (FR)-targeted NC (O-PT-NC-Folate) has also been prepared by conjugating folic acid to Pluronic F127. MTT test is used to validate the targeting efficacy on the FR-positive human oral cancer cell line (KB). At pharmacologically relevant concentrations, the PT nano-crystal formulation did not cause hemolysis. Compared to non-targeted NC of PT, the O-PT-NC-Folate showed a comparable but more sustained anti-cancer effect, according to an in vivo anti-tumor investigation in NCI/ADR-RES cell lines. The remarkable anti-tumor effectiveness, minimal toxicity, and simplicity of scale-up manufacturing of the NC formulations indicate their potential for clinical development. Other hydrophobic medications that are formulated into nano-systems for improved therapy may benefit from the formulation approach.  相似文献   

6.
    
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7.
The fluorescence properties of piroxicam in various micellar media were investigated. It was found that the presence of 0.05M sodium dodecyl sulfate (SDS) surfactant (pH 1.5–2, nitric acid) causes an approximately 5-fold enhancement in the fluorescence of this drug. An experimental design approach based on central composite design was used to investigate the influence of the main variables (pH, SDS concentration and temperature) on the fluorescence signal. Based on the obtained results, a micelle-enhanced fluorescence method was developed for the determination of piroxicam in pharmaceuticals and also in spiked human serum (after extraction with diethyl ether). The linear calibration ranges of the methods were 0.05–1.5 and 0.2–10µgmL–1 for aqueous solution and serum samples, respectively. The detection limits were 0.015 and 0.10µgmL–1 in aqueous and serum samples, respectively.Received November 24, 2002; accepted April 13, 2003 Published online August 8, 2003  相似文献   

8.
    
Vitamin B12, only found naturally in animal-based foods, is essential for brain functions and various chemical reactions in the human body. Insufficient vitamin B12 leads to vitamin B12 deficiency, common among strict vegetarians due to their limited intake of animal-based foods. Nevertheless, extensive studies have demonstrated that macroalgae, specifically the Ulva lactuca species, are rich in vitamin B12 and could be further exploited in future dietary applications. In the current study, the ideal extraction method of vitamin B12 from dried U. lactuca was developed and optimised to achieve the maximum vitamin B12 yield. The effects of several extraction parameters, including the solvent-to-solvent, methanol:water (MeOH:H2O), and solute-to-solvent ratios, and pH on the total vitamin B12 content were analysed through a two-level factorial and central composite design. The highest vitamin B12 content, particularly cyanocobalamin (CN-Cbl), was recovered through the ultrasonic-assisted extraction (UAE) of oven-dried U. lactuca at 3 g:60 mL of solute-to-solvent and 25:75% of MeOH to H2O ratios at pH 4. The extraction of CN-Cbl from oven-dried U. lactuca that employed the UAE method has elevated CN-Cbl content recovery compared to other extraction methods.  相似文献   

9.
    
Drug products used for treating tuberculosis are one of the most widely reported medicines to be classified as falsified or substandard in low- and middle-income countries, representing a major hazard to health. The aim of this study was, firstly, to develop an ultra-performance liquid chromatography (UPLC) method which is able to analyze fixed combination tablets with up to four active pharmaceutical ingredients, including isoniazid, pyrazinamide, rifampicin, and ethambutol. Secondly, we aimed to optimize it through the design of experiments and multi-linear regression based on a central composite design and to validate it according to the guidelines of the International Conference on Harmonization. The application of this tools enabled the identification of the influential factors (flow rate, formic acid, and temperature) and their effects on the studied responses (retention factor and percentage for each drug) as part of the quality by design approach. The method proved to be to be linear in the range from 5.0 to 15 µg/mL for isoniazid, pyrazinamide, and rifampicin, being precise (<1%) and accurate (97–101%). In addition, the method validated for ethambutol proved to be linear from 1.4 to 4.2 µg/mL, as well as precise (0.54%) and accurate (97.3%). The method was stability indicated for all the active pharmaceutical ingredients studied and was able to detect two substandard formulations sampled on the African market.  相似文献   

10.
    
This is for the first time that application of complex nanostructure is reported as pH indicator in PVC matrix. This new optical pH sensor was constructed based on incorporation of ZnLI2 complex nanostructure in PVC matrix. The synthesized nanostructure ZnLI2 complex was characterized by SEM and XRD technique. The membrane solution was speared on the glass plate to provide thin film and the membrane surface morphology was investigated via field emission scanning microscope (FE‐SEM) technique. Central composite design (CCD) combined with desirability function (DF) was applied to find the best experimental composition of membrane providing the highest absorbance. These conditions were found in correspondence with 3 mg of pH indicator, 3 mg of ionic additive and 1.5 mg/mg of DBP/PVC weight ratio. Under optimum conditions, the proposed pH sensor has two linear working ranges of 4 ‐ 8 at 393 nm (R2 = 0.9897) and 5 ‐ 8 (R2 = 0.9982) at 570 nm with response time of 4 min. The pKa of proposed pH optical sensor was calculated through three methods that found to be 5.63. The present optical sensor shows stability after 2 months without any significant divergence in response properties (less than 5% RSD). Furthermore, current pH optode was exhibited good repeatability (RSD = 1.14%) as well as reproducibility (RSD = 4.06%). No significant variation was observed on sensor response with increasing the ionic strength in the range of 0.0–0.5 M of sodium chloride. All above features indicated that the proposed sensor can be successfully used for detection of pH in solutions with different ionic strength.  相似文献   

11.
高玉荣  黄培  孙佩佩  吴敏  黄勇 《化学进展》2016,28(5):647-656
近年来,石墨烯/纤维素复合材料引起了研究者的广泛关注。该材料在透明导电柔性薄膜、电容器、载药、紫外线防护、传感器、吸附等领域有重要的应用价值。本文在收集、归类研究国内外研究者在石墨烯/纤维素复合材料制备方法、性能以及应用工作的基础上,对石墨烯和纤维素复合材料的混合技术、制备方法及应用进行了综述。  相似文献   

12.

Elaboration of β-tricalcium Phosphate (β-TCP) was studied using a two-block central composite design including 4 factors. Analysis of the response allowed the definition of one set of experimental conditions in which β-TCP was obtained after powder calcination at 900°C.  相似文献   

13.
A two-step response surface methodology (RSM) study was conducted for the optimization of keratinase production and enzyme activity from poultry feather byStreptomyces sp7. Initially different combinations of salts were screened for maximal production of keratinase at a constant pH of 6.5 and feather meal concentration of 5 g/L. A combination of K2HPO4, KH2PO4, and NaCl gave a maximum yield of keratinase (70.9 U/mL) production. In the first step of the RSM study, the selected five variables (feather meal, K2HPO4, KH2PO4, NaCl, and pH) were optimized by a 25 full-factorial rotatable central composite design (CCD) that resulted in 95 U/mL of keratinase production. The results of analysis of variance and regression of a second-order model showed that the linear effects of feather meal concentration (p<0.005) and NaCl (p<0.029) and the interactive effects of all variables were more significant and that values of the quadratic effects of feather meal (p<1.72e-5), K2HPO4 (p<4.731e-6), KH2PO4 (p<1.01e-10), and pH (p 7.63e-7) were more significant than the linear and interactive effects of the process variables. In the second step, a 23 rotatable full-factorial CCD and response surface analysis were used for the selection of optimal process parameters (pH, temperature, and rpm) for keratinase enzyme activity. These optima were pH 11.0, 45°C, and 300 rpm.  相似文献   

14.
    
Tramadol is a centrally acting analgesic‐anodyne agent of high oral bioavailability. The tramadol contains a weakly absorbing chromophore in its molecule and it was determined by kinetic spectrophotometric method in pharmaceutical, urine, and blood plasma. Response surface methodology and the central composite design was applied to study the influence of maximum sensitivity, reagents concentration, temperature, and time on the UV–Vis spectrophotometry analysis of tramadol. Analysis of variance showed a high coefficient of determination (R2) value for responses, confirming adjustment of the models with experimental data. The change in absorbance was followed spectrophotometrically at 478 nm. Under optimum experimental conditions, calibration curve was linear over the range 0.45–100.0 μg/L of tramadol. The limit of detection was 0.12 μg/L of tramadol. The developed method was successfully applied for the determination of tramadol in real samples.  相似文献   

15.
An ultrasound-assisted emulsification microextraction (USAEME) based on low-density solvents was successfully applied for the extraction and pre-concentration of four toxic nitrophenols in water samples. The extracted analytes were analyzed by high-performance liquid chromatography-UV detection. The important parameters influencing the extraction efficiency were studied and optimized utilizing two different optimization methods: one variable at a time (OVAT) and central composite design (CCD). The results showed that the emulsification process can be completed in a few seconds using low-density solvents, but almost 10–20?min is necessary for high-density solvents. Under the optimum conditions (extraction solvent, 1-octanol; extraction solvent volume, 40?µL; sample pH, 3.0; salt concentration, 20% (w/v) NaCl; extraction temperature, 40 (±3)°C), limits of detection of the method were in the range of 0.25 to 1?µg?L?1 and the repeatability and reproducibility of the proposed method, expressed as relative deviation, varied in the range of 2.2–4.2% and 4.7–6.9%, respectively. Linearity was found to be in the range of 1 to 200?µg?L?1 and the preconcentration factors (PFs) were between 77 and 175. The relative recoveries of the four nitrophenols from water samples at spiking level of 10.0?µg?L?1 were in the range of 92.0 to 115.0%.  相似文献   

16.
    
This paper demonstrates a chemometric-assisted RP-HPLC method for the simultaneous determination of azithromycin, secnidazole, and fluconazole using water:methanol (63:37% v/v) as mobile phase at a flow rate of 1.2 mL · min−1. The separation of the three drugs was achieved on an Xterra RP-18 column (250 × 4.6 mm ID, 5 µM) and the detection of the eluents was realized on a diode array detector at 210 nm wavelength. The combined effects of % methanol (organic phase) and flow rate, each at three levels influencing the chromatographic efficiency were investigated and optimized employing central composite design. Under the optimal condition, the percent relative standard deviations for precision study were in the range of 0.2–0.7% and 0.5–1.2% for standard and formulation, respectively. The limits of detection were 12.5, 0.62, and 1.7 µg · mL−1 and limits of quantification were found 37.5, 1.86, and 5.1 µg · mL−1 for azithromycin, secnidazole, and fluconazole, respectively. Consequently, the method has been effectively applied to their direct determination in the commercial formulation (combi-kit).  相似文献   

17.
    
In this study, the capillary electrophoresis-photodiode array detector was employed for the analysis of four iridoid compounds in Gentiana macrophylla Radix (RGM), and the method was optimized based on the concept of analytical quality by design (AQbD). The peak areas relative standard deviation (n = 3) and resolution of the four analytes were selected as critical method attributes. Fractional factorial design test combined with Pareto analysis were employed to screen critical method parameters (buffer concentration, pH, sodium dodecyl sulfate [SDS] micelle concentration, temperature, and voltage). Subsequently, three main factors (buffer concentration, buffer pH, and SDS concentration) were selected by central composite design test for constructing the design space. The optimal separation conditions as follows: capillary column (50.2 cm × 50 µm, detection length 40 cm). Working background electrolyte consisted of 51 mmol/L borax solution (pH = 9.47) and 40 mmol/L SDS. The samples were injected by pressure (5 s at 0.5 psi) and the detection was performed at 254 nm. Applied voltage was 20 kV and column temperature was 23°C. The developed method is rapid and reliable for the quantitative analysis of four iridoid compounds in RGM, providing a reference for the application of AQbD concept in the analysis of natural products.  相似文献   

18.
    
The inclusion of a polyamidoamine dendrimer in a silica sol–gel yielded a solid nanosorbent that was used for the preconcentration, extraction, and determination of citalopram in hospital waste water, hemodialysis solution, and some drinking water. The method was developed by applying a novel nanosorbent for the solid‐phase microextraction of citalopram, containing a silica sol–gel reinforced by polyamidoamine second‐generation dendrimer, which was protected by a polypropylene hollow fiber. Plackett–Burman design and central composite design were utilized to evaluate the significance of several factors on the extraction efficiency. The adsorption mechanism and thermodynamic and kinetic aspects were studied. The adsorption process was exothermic and well fitted to the Bangham equation kinetic model. Under optimal conditions, the presented method was liner in the range of 0.05–100 μg/mL. The limits of detection of quantification of citalopram were 0.0095 and 0.031 μg m/L, respectively.  相似文献   

19.
    
Treatment of herpes simplex infection requires high and frequent doses of oral acyclovir to attain its maximum therapeutic effect. The current therapeutic regimen of acyclovir is known to cause unwarranted dose-related adverse effects, including acute kidney injury. For this reason, a suitable delivery system for acyclovir was developed to improve the pharmacokinetic limitations and ultimately administer the drug at a lower dose and/or less frequently. In this study, solid lipid nanoparticles were designed to improve the oral bioavailability of acyclovir. The central composite design was applied to investigate the influence of the materials on the physicochemical properties of the solid lipid nanoparticles, and the optimized formulation was further characterized. Solid lipid nanoparticles formulated from Compritol 888 ATO resulted in a particle size of 108.67 ± 1.03 nm with an entrapment efficiency of 91.05 ± 0.75%. The analyses showed that the optimum combination of surfactant and solid lipid produced solid lipid nanoparticles of good quality with controlled release property and was stable at refrigerated and room temperature for at least 3 months. A five-fold increase in oral bioavailability of acyclovir-loaded solid lipid nanoparticles was observed in rats compared to commercial acyclovir suspension. This study has presented promising results that solid lipid nanoparticles could potentially be used as an oral drug delivery vehicle for acyclovir due to their excellent properties.  相似文献   

20.
    
Multimode chromatographic separations are highly desirable in pharmaceutical and environmental sciences. Current study deals with the application of newly developed mixed-mode end capped-immobilized humic acid onto an aminopropyl silica based chromatographic column for separation and identification of six drugs belonging to different therapeutic groups for its applicability in pharmaceutical industries. For this, central composite design was used to evaluate the separation and resolution by optimization of three most effective parameters (acetonitrile%, flow rate, and pH of mobile phase). Second-order quadratic model was used to evaluate their effect on resolution of peaks; the probability value (<0.05) obtained from analysis of variance suggested the best applicability of the model. Desirability function was applied to calculate optimum conditions (44.8% acetonitrile, 1.75 mL/min of flow rate, and 7.5 pH) required to achieve maximum separation with good resolution within 11 min. The method was validated for linearity, precision accuracy, selectivity, and sensitivity. The results revealed a highly precise (coefficient of variance > 1%), linear (R2 = 0.99), and highly selective method. Moreover, the limit of detection/quantification values revealed acceptable sensitivity of the method. The developed column was compared for its efficiency with a commercially available column and found to be highly applicable for industrial applications.  相似文献   

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