Vortex-Assisted Dispersive Liquid–Liquid Microextraction Coupled with Deproteinization for Determination of Nateglinide in Human Plasma Using HPLC/UV

2020 ◽  
Author(s):  
Mohamed A Hammad ◽  
Amira H Kamal ◽  
Reham E Kannouma ◽  
Fotouh R Mansour
Keyword(s):  
Human Plasma ◽  
High Performance ◽  
Limit Of Detection ◽  
Signal To Noise Ratio ◽  
Cost Effective ◽  
Salt Addition ◽  
Relative Standard ◽  
Dispersive Liquid Liquid Microextraction ◽  
Liquid Microextraction

Abstract A validated method for preconcentration and determination of nateglinide in plasma was developed using vortex-assisted dispersive liquid–liquid microextraction. Different variables that affect extraction efficiency were studied and optimized, including type and volume of extractant, type and volume of disperser, pH of diluent, salt addition effect, centrifugation and vortex time. Nateglinide was extracted using 30 μL of 1-octanol as an extractant and 200 μL of methanol as a disperser. The enrichment factor reached 330 under the optimum conditions. High-performance liquid chromatography/ultraviolet was used for detection using phosphate buffer (pH 2.5, 10 mM): acetonitrile (45:55, v/v) as a mobile phase at a flow rate of 1 mL/min. The method was linear over the range of 50–20,000 ng/mL with a limit of detection of 15 ng/mL (signal-to-noise ratio = 3). Intra- and inter-day precision had %relative standard deviation <6% (n = 3) and the %recoveries were found to be between 102.5 and 105.9%. The proposed method is simple, sensitive, eco-friendly, cost-effective and powerful for microextraction of nateglinide from human plasma samples.

Simultaneous Determination of Four Plant Hormones in Soil by Ultrasound-Assisted Ionic Liquid Based Dispersive Liquid-Liquid Microextraction

2014 ◽  
Vol 675-677 ◽  
pp. 181-184 ◽  
Author(s):  
Gui Qi Huang ◽  
She Ying Dong ◽  
Zhen Yang ◽  
Ting Lin Huang
Keyword(s):  
Ionic Liquid ◽  
Plant Hormones ◽  
High Performance ◽  
Extraction Solvent ◽  
Target Analytes ◽  
Relative Standard ◽  
Ultrasound Assisted ◽  
Dispersive Liquid Liquid Microextraction ◽  
Liquid Microextraction

An ultrasound-assisted ionic liquid based dispersive liquid-liquid microextraction (UA-IL-DLLME) was developed for the determination of four plant hormones (6-benzyladenine (6-BA), kinetin (6-KT), 2, 4-dichlorophenoxy acetic acid (2, 4-D) and uniconazole (UN)) in soil, using high performance liquid chromatography (HPLC)-diode array detection (DAD). Several important parameters including the type and volume of extraction solvent, the volume of disperser solvent, ultrasound time, pH of the solution and salt effect were studied and optimized. Under optimum conditions, the limits of detections (LODs) for the target analytes were in the range of 0.002-0.01 μg g-1. And satisfactory recoveries of the target analytes in the soil samples were 79.3-96.7 %, with relative standard deviations (RSD, n=5) that ranged from 4.3 to 6.7%.

scholarly journals Use of Dispersive Liquid-Liquid Microextraction and UV-Vis Spectrophotometry for the Determination of Cadmium in Water Samples

2014 ◽  
Vol 2014 ◽  
pp. 1-4 ◽  
Author(s):  
J. Pérez-Outeiral ◽  
E. Millán ◽  
R. Garcia-Arrona
Keyword(s):  
Water Samples ◽  
Limit Of Detection ◽  
Experimental Conditions ◽  
Cadmium Determination ◽  
A Value ◽  
Relative Standard ◽  
Potential Applicability ◽  
Dispersive Liquid Liquid Microextraction ◽  
Liquid Microextraction

A simple and inexpensive method for cadmium determination in water using dispersive liquid-liquid microextraction and ultraviolet-visible spectrophotometry was developed. In order to obtain the best experimental conditions, experimental design was applied. Calibration was made in the range of 10–100 μg/L, obtaining good linearity (R2 = 0.9947). The obtained limit of detection based on calibration curve was 8.5 μg/L. Intra- and interday repeatability were checked at two levels, obtaining relative standard deviation values from 9.0 to 13.3%. The enrichment factor had a value of 73. Metal interferences were also checked and tolerable limits were evaluated. Finally, the method was applied to cadmium determination in real spiked water samples. Therefore, the method showed potential applicability for cadmium determination in highly contaminated liquid samples.

scholarly journals Microextraction by Packed Molecularly Imprinted Polymer Combined Ultra-High-Performance Liquid Chromatography for the Determination of Levofloxacin in Human Plasma

2019 ◽  
Vol 2019 ◽  
pp. 1-9 ◽  
Author(s):  
Jia Meng ◽  
Xu Wang
Keyword(s):  
High Performance Liquid Chromatography ◽  
Liquid Chromatography ◽  
Human Plasma ◽  
Bacterial Infections ◽  
High Performance ◽  
Limit Of Detection ◽  
Binding Capacity ◽  
Molecularly Imprinted ◽  
Relative Standard

Fluoroquinolones are considered as gold standard for the prevention of bacterial infections. To improve assessment of antibacterial efficacy, a novel method for determination of levofloxacin was developed and validated. Deep eutectic solvents (DESs) as only green solvent were used as a porogen for preparation of water-compatible molecularly imprinted polymers (MIPs) with a pseudotemplate. The DESs-MIPs were characterized in detail, including scanning electron microscope, nitrogen sorption porosimetry, and Fourier transform-infrared spectra. Clearly, the maximum binding capacity of levofloxacin on DESs-MIPs in water and methanol was 0.216 and 0.077 μmol g−1, respectively. The DESs-MIPs as adsorbing materials were applied in microextraction by packed sorbent (MEPS), and the DESs-MIPs-MEPS conditions were optimized. The DESs-MIPs-MEPS coupled with ultra-high-performance liquid chromatography (UHPLC) was used to determine levofloxacin in human plasma. The method was found linear over 0.05–10 μg mL−1 with coefficient of correlation equal to 0.9988. The limit of detection and limit of quantification were 0.012 and 0.04 μg mL−1, respectively. At three spiked levels, the precision of proposed method was between 95.3% and 99.7% with intraday and interday relative standard deviations ≤8.9%. Finally, the developed method was used to examine levofloxacin from human plasma of 20 hospitalized patients after transrectal ultrasound-guided prostate biopsy, and the average concentration (±SD) of levofloxacin was 2.35 ± 0.99 μg mL−1 in plasma.

scholarly journals Low Density Solvent-Based Dispersive Liquid-Liquid Microextraction for the Determination of Synthetic Antioxidants in Beverages by High-Performance Liquid Chromatography

2013 ◽  
Vol 2013 ◽  
pp. 1-8 ◽  
Author(s):  
Hasan Çabuk ◽  
Mustafa Köktürk
Keyword(s):  
High Performance Liquid Chromatography ◽  
Liquid Chromatography ◽  
High Performance ◽  
Correlation Coefficients ◽  
Synthetic Antioxidants ◽  
Beverage Samples ◽  
Relative Standard ◽  
Dispersive Liquid Liquid Microextraction ◽  
Liquid Microextraction

A simple and efficient method was established for the determination of synthetic antioxidants in beverages by using dispersive liquid-liquid microextraction combined with high-performance liquid chromatography with ultraviolet detection. Butylated hydroxy toluene, butylated hydroxy anisole, and tert-butylhydroquinone were the antioxidants evaluated. Experimental parameters including extraction solvent, dispersive solvent, pH of sample solution, salt concentration, and extraction time were optimized. Under optimal conditions, the extraction recoveries ranged from 53 to 96%. Good linearity was observed by the square of correlation coefficients ranging from 0.9975 to 0.9997. The relative standard deviations ranged from 1.0 to 5.2% for all of the analytes. Limits of detection ranged from 0.85 to 2.73 ng mL−1. The method was successfully applied for determination of synthetic antioxidants in undiluted beverage samples with satisfactory recoveries.

scholarly journals Extraction and Determination of Oxymatrine Pesticide in Environmental Sample and in its Formulation using High-Performance Liquid Chromatography

2020 ◽  
Vol 8 (2) ◽  
pp. 1-7
Author(s):  
Ihsan M. Shaheed ◽  
Saadiyah A. Dhahir
Keyword(s):  
High Performance Liquid Chromatography ◽  
Liquid Chromatography ◽  
Water Samples ◽  
High Performance ◽  
Limit Of Detection ◽  
Limit Of Quantification ◽  
Chromatography Method ◽  
Relative Standard ◽  
Dispersive Liquid Liquid Microextraction

The quinolizindine alkaloid compound, oxymatrine pesticide, was analysis in the river water samples collected from different agriculture areas in the Iraqi city of Kerbala and also in its formulation using developed reverse-phase high-performance liquid chromatography method. Acetonitrile:methanol (60:40 v/v) was chosen as mobile phase at pH (7.0), flow rate 0.5 mL/min, and 20 µL as volume injection. Modified ecological-friendly method, dispersive liquid-liquid microextraction, was used for the extraction of oxymatrine from water samples. Linearity study was constructed from 0.1 to 70 μg/mL at λmax 205 nm. The limit of detection and limit of quantification were 0.025 and 0.082 μg/mL, respectively, and the relative standard deviation (RSD) % was 0.518%. Three spiked levels of concentration (20.0, 40.0, and 70.0 μg/mL) were used for the validation method. The percentage recovery for the three spiked samples was ranged between 98.743 and 99.432 and the RSD% was between 0.051 and 0.202%, the formulation studies of oxymatrine between 99.487 and 99.798, and the RSD% was ranged from 0.045 to 0.057%. The developed method can be used accurately and selectively for the determination of oxymatrine in environmental samples and in the formulation.

Dispersive Liquid-Liquid Microextraction Coupled with Gas Chromatography for the Determination of Orthochlorophenol in Environmental Water Samples

2012 ◽  
Vol 518-523 ◽  
pp. 1379-1382
Author(s):  
Ying Chun Yang ◽  
Qian Sun ◽  
Chong Shu Yi ◽  
Zhi Xiang Ye ◽  
Li Mo
Keyword(s):  
Gas Chromatography ◽  
Water Samples ◽  
Environmental Water ◽  
Environmental Water Samples ◽  
Extraction Solvent ◽  
Salt Addition ◽  
Relative Standard ◽  
Dispersive Liquid Liquid Microextraction ◽  
Liquid Microextraction

A rapid and effective method, the dispersive liquid-liquid microextraction(DLLME) with gas chromatography, has been developed for the extraction and determination of OCP in environmental water samples. The factors relevant to the efficiency of DLLME were investigated and optimized. Under the optimum conditions, such as 150μL of dichloromethane as extraction solvent, 1.2 mL acetone as dispersive agent, 8 minutes extraction time, and without salt addition, the linear response of this method was in the range of 0.5～5000μg L−1 (r = 0.9981), the relative standard deviation (RSD) for 500μg L−1 and 1000μg L−1 of OCP was 5.2% and 12.6% (n = 6), respectively. The detection limit (3σ) was 0.08 μg L−1. The developed method was successfully applied to the determination of trace amount of OCP in three kinds of real environmental water samples, the spiked recoveries were in the range of 87.4%～108.0%.

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