A Simple Vortex-Assisted Magnetic Dispersive Solid Phase Microextraction System for Preconcentration and Separation of Triazine Herbicides from Environmental Water and Vegetable Samples Using Fe3O4@MIL-100(Fe) Sorbent

2018 ◽  
Vol 101 (5) ◽  
pp. 1639-1646 ◽  
Author(s):  
Atefe Nasrollahpour ◽  
Seyyed Ershad Moradi
Keyword(s):  
Solid Phase Microextraction ◽  
High Performance ◽  
Limit Of Detection ◽  
Solid Phase ◽  
Signal To Noise Ratio ◽  
Correlation Coefficients ◽  
Environmental Water ◽  
Triazine Herbicides ◽  
Vegetable Samples ◽  
Relative Standard

Abstract A vortex-assisted magnetic dispersive solid phase microextraction coupled with high-performance liquid chromatography has been developed for the extraction and determination of triazine herbicides by using magnetic metal organic frameworks [Fe3O4@MIL-100(Fe)] in environmental water and vegetable samples. The Fe3O4@MIL-100(Fe) composite has been characterized by using X-ray diffraction spectroscopy, tunneling electron microscopy, thermogravimetric measurement, and Brunauer-Emmett-Teller analysis. The method is based on the sorption of triazine herbicides on Fe3O4@MIL-100(Fe) because of the complex formation between iron oxide nanoparticles and triazine herbicides beside π-π interactions between organic parts of Fe3O4@MIL-100(Fe) and triazine herbicides. The experimental parameters for the preconcentration of triazine herbicides, such as the type and volume of the eluent, pH, time of the sorption and desorption, and the amount of the sorbent, were optimized. Under the optimized conditions, the method was linear over the concentration range of 0.0061 to 70 ng/mL for each triazine herbicide, and the correlation coefficients ranged from 0.9988 to 0.9997. The limit of detection of the method at a signal-to-noise ratio of 3 was 2.0 to 5.3 ng/mL. The relative standard deviations for inter- and intraday assays were in the range of 5.8 to 10.2% and 3.8 to 6.3%, respectively.

A Novel Electrochemiluminescence Sensor for Sensitive Determination of Carbaryl Based on Solid Phase Microextraction at NH2–Graphene–Nafion Modified Electrode

2015 ◽  
Vol 68 (5) ◽  
pp. 793 ◽  
Author(s):  
Sui Wang ◽  
Shasha Lv ◽  
Wenwen Wu ◽  
Zhiyong Guo
Keyword(s):  
Solid Phase Microextraction ◽  
Limit Of Detection ◽  
Solid Phase ◽  
Signal To Noise Ratio ◽  
Initial Response ◽  
X Ray Diffraction ◽  
Relative Standard ◽  
Sensitive Determination ◽  
Response Current

Sensitive electrochemiluminescence (ECL) detection and solid phase microextraction (SPME) using a NH2–graphene–Nafion modified glassy carbon electrode was developed for carbaryl. The NH2–graphene was synthesised and characterised by Fourier transform infrared spectroscopy, scanning electron microscopy, and X-ray diffraction. The main parameters that affect the extraction efficiencies, such as the buffer and sample pH, and extraction time were investigated and optimised. The introduction of NH2–graphene into Nafion improves the conductivity of the film because of its electrical conductivity. The electrode enables the determination of carbaryl in the range from 5 × 10–4 to 10 μg mL–1, and the limit of detection was 2 × 10–4 μg mL–1 at a signal-to-noise ratio of 3. The ECL intensity retained 97 % of its initial response current after storage for 10 days, indicating a good storage stability of the sensor. The relative standard deviations (RSDs) of intra-assay and inter-assay were found to be 3.5 and 5.3 %, respectively, indicating an acceptable reproducibility. Furthermore, the ECL sensor was successfully applied to the selective and sensitive quantitative determination of carbaryl in river samples, the recoveries of carbaryl ranged from 99.0 to 108.0 %, and the RSDs were less than 5.0 %, which shows good reproducibility and high precision of analysis.

Calcium/Copper alginate framework doped with CuO nano-particles as a novel adsorbent for micro-extraction of benzodiazepines from human serum

2020 ◽  
Vol 16 ◽  
Author(s):  
Nadereh Rahbar ◽  
Fatemeh Ahmadi ◽  
Zahra Ramezani ◽  
Masoumeh Nourani
Keyword(s):  
Human Serum ◽  
High Performance ◽  
Limit Of Detection ◽  
Solid Phase ◽  
Nano Particles ◽  
Limit Of Quantification ◽  
Analytical Methodology ◽  
Fiber Fabrication ◽  
Relative Standard ◽  
Green Procedure

Background: Sample preparation is one of the most challenging phases in pharmaceutical analysis, especially in biological matrices, affecting the whole analytical methodology. Objective: In this study, a new Ca(II)/Cu(II)/alginate/CuO nanoparticles hydrogel fiber (CCACHF) was synthesized through a simple, green procedure and applied for fiber micro solid phase extraction (FMSPE) of diazepam (DIZ) and oxazepam (OXZ) as model drugs prior to high-performance liquid chromatography-UV detection (HPLC-UV). Methods: Composition and morphology of the prepared fiber were characterized and the effect of main parameters on the fiber fabrication and extraction efficiency have been studied and optimized. Results: In optimal conditions, calibration curves were linear ranging between 0.1–500 µg L−1 with regression coefficients of 0.9938 and 0.9968. Limit of detection (LOD) (S/N=3) and limit of quantification (LOQ) (S/N=10) of the technique for DIZ and OXZ were 0.03 to 0.1 µg L−1. Within-day and between-day relative standard deviations (RSDs) for DIZ and OXZ were 6.0–12.5% and 3.3–9.4%, respectively. Conclusion: The fabricated adsorbent has been substantially employed to extraction of selected benzo-diazepines (BZDs) from human serum real specimens and the obtained recoveries were also satisfactory (82.1-109.7%).

Development of a solid-phase extraction – spectrofluorimetric method for trace glutathione determination

2011 ◽  
Vol 89 (4) ◽  
pp. 517-523 ◽  
Author(s):  
Ke-Jing Huang ◽  
Cong-Hui Han ◽  
Ying-Ying Wu ◽  
Chao-Qun Han ◽  
De-Jun Niu ◽  
...  
Keyword(s):  
Solid Phase Extraction ◽  
Limit Of Detection ◽  
Solid Phase ◽  
Signal To Noise Ratio ◽  
Calibration Graph ◽  
Extraction Column ◽  
Phase Extraction ◽  
Selective Reaction ◽  
Spectrofluorimetric Method ◽  
Relative Standard

A simple and efficient solid-phase extraction – spectrofluorimetric method has been developed to determine glutathione (GSH). Fluorescent probe N-(4,4-difluoro-5,7-dimethyl-4-bora-3a,4a-diaza-s-indacene-3-yl)methyl)iodoacetamide (BODIPY Fl-C1-IA) was used as the derivatization reagent. The procedure was based on a BODIPY Fl-C1-IA selective reaction with GSH to form the highly fluorescent product BODIPY Fl-C1-IA–GSH, using a solid-phase extraction column and spectrofluorimetric determination. The variables affecting analytical performance were studied and optimized. The calibration graph using the preconcentration system for GSH was linear over the range of 1–200 nmol/L with a limit of detection of 0.05 nmol/L (signal-to-noise ratio = 3). The relative standard deviation for six replicate determinations of GSH at the 100 nmol/L concentration level was 3.9%. The method was applied to water samples and average recoveries between 87.5% and 111.5% were obtained for spiked samples.

scholarly journals Ionic Liquid-modified NiTi Composite Nanosheets Coating for Efficient Solid Phase Microextraction of Octadecylamine in Brine

2019 ◽  
pp. 1-8
Author(s):  
Huiju Wang
Keyword(s):  
Ionic Liquid ◽  
Solid Phase Microextraction ◽  
Extraction Efficiency ◽  
Solid Phase ◽  
Correlation Coefficients ◽  
Fiber Coating ◽  
Relative Standard ◽  
Optimized Conditions ◽  
As Solid Phase

Ionic     liquid (IL), 1-dodecyl-3-methylimidazolium-3-hydroxy-2-naphthoate (C12mimHNC) was synthesized and coated on the surface of NiTi as solid phase microextractiom fiber coating for determination the octadecylamine in brine. Prior to modification with IL, the NiTi was hydrothermally treated for in-situ growth of titanium and nickel oxide composite nanosheets (TiO2/NiOCNSs). The TiO2/NiOCNSs fibers coating was oriented  around the NiTi  substrate and  presented  double-faced  open  access  sites,  which provided a desired support framework for the further modification with IL. The extraction performance of C12mimHNC-TiO2/NiOCNSs fiber coating was evaluated for       detection of octadecylamine (ODA) coupled to HPLC with UV detection. As a result, the C12mimHNC-TiO2/NiOCNSs fiber coating illustrated excellent adsorption and extraction capability for ODA. The main factors affected extraction efficiency were optimized. Under the optimized  conditions,  good  linearity was  obtained  in  the  range of  1-150  µg/L with correlation  coefficients  (r2)  above  0.985.  Limits of detection (LODs) for  the  developed method was 0.280 µg/L. The proposed method was first applied to extract the ODA in brine samples. Relative recoveries varied from 78.3% to 96.5% at spiking level of 15µg/L and 30 µg/L with the relative standard deviations (RSDs) less than 8.7%.

scholarly journals Carbon and Tin-Based Polyacrylonitrile Hybrid Architecture Solid Phase Microextraction Fiber for the Detection and Quantification of Antibiotic Compounds in Aqueous Environmental Systems

Molecules ◽  
2019 ◽  
Vol 24 (9) ◽  
pp. 1670 ◽  
Author(s):  
Sandip Mondal ◽  
Jialing Jiang ◽  
Yin Li ◽  
Gangfeng Ouyang
Keyword(s):  
Solid Phase Microextraction ◽  
Tin Dioxide ◽  
Limit Of Detection ◽  
Solid Phase ◽  
Tap Water ◽  
Coefficient Of Determination ◽  
Lower Amount ◽  
Custom Made ◽  
Relative Standard ◽  
Detection And Quantification

In this study, the detection and quantification of multiple classes of antibiotics in water matrices are proposed using a lab-made solid phase microextraction (SPME) fiber coupled with high-performance liquid chromatography-tandem mass spectrometry (LC-MS/MS). The lab-made fiber was prepared using a graphene oxide (G), carbon nanotubes (C), and tin dioxide (T) composite, namely GCT, with polyacrylonitrile (PAN) as supporting material. The detected antibiotics were enrofloxacin, sulfathiazole, erythromycin, and trimethoprim. The custom-made fiber was found to be superior compared with a commercial C18 fiber. The excellent reproducibility and lower intra-fiber relative standard deviations (RSDs 1.8% to 6.8%) and inter-fiber RSDs (4.5% to 8.8%) made it an ideal candidate for the detection of traces of antibiotics in real environmental samples. The proposed validated method provides a satisfactory limit of detection and good linear ranges with higher (>0.99) coefficient of determination in the aqueous system. Application of the method was made in different real water systems such as river, pond and tap water using the standard spiking method. Excellent sensitivity, reproducibility, lower amount of sample detection and higher recovery was found in a real water sample. Therefore, the extraction method was successfully applied to the detection and quantification of multiple classes of antibiotics in different aqueous systems with satisfactory results.

scholarly journals In Situ Synthesis of a Magnetic Graphene Platform for the Extraction of Benzimidazoles from Food Samples and Analysis by High-Performance Liquid Chromatography

2017 ◽  
Vol 2017 ◽  
pp. 1-11 ◽  
Author(s):  
Qianchun Zhang ◽  
Yulan Liu ◽  
Xingyi Wang ◽  
Huimin Li ◽  
Junyu Chen
Keyword(s):  
High Performance Liquid Chromatography ◽  
Liquid Chromatography ◽  
High Performance ◽  
Solid Phase ◽  
Correlation Coefficients ◽  
Magnetic Solid Phase Extraction ◽  
Food Samples ◽  
Magnetic Graphene ◽  
Relative Standard

A novel method was proposed for the determination of five benzimidazoles (oxfendazole, mebendazole, flubendazole, albendazole, and fenbendazole) using magnetic graphene (G-Fe3O4). G-Fe3O4 was synthesized via in situ chemical coprecipitation. The properties of G-Fe3O4 were characterized by various instrumental methods. G-Fe3O4 exhibited a great adsorption ability and good stability towards analytes. Various experimental parameters that might affect the extraction efficiency such as the amount of G-Fe3O4, extraction solvent, extraction time, and desorption conditions were evaluated. Under the optimized conditions, a method based on G-Fe3O4 magnetic solid-phase extraction coupled with high-performance liquid chromatography was developed. A good linear response was observed in the concentration range of 0.100–100 μg/L for the five benzimidazoles, with correlation coefficients ranging from 0.9966 to 0.9998. The limits of detection (S/N=3) of the method were between 17.2 and 32.3 ng/L. Trace benzimidazoles in chicken, chicken blood, and chicken liver samples were determined and the concentrations of oxfendazole, mebendazole, flubendazole, and fenbendazole in these samples were 13.0–20.2, 1.62–4.64, 1.94–6.42, and 0.292–1.04 ng/g, respectively. The recovery ranged from 83.0% to 115%, and the relative standard deviations were less than 7.9%. The proposed method was sensitive, reliable, and convenient for the analysis of trace benzimidazoles in food samples.

Analysis of spectinomycin in fermentation broth by reversed-phase chromatography

2009 ◽  
Vol 63 (6) ◽  
Author(s):  
Hong Yan ◽  
Pei Xu ◽  
Hai Huang ◽  
Juan Qiu
Keyword(s):  
High Performance ◽  
Limit Of Detection ◽  
Fermentation Broth ◽  
Correlation Coefficients ◽  
High Performance Liquid Chromatographic ◽  
Reversed Phase ◽  
Hplc Method ◽  
Standard Curve ◽  
Relative Standard ◽  
Liquid Chromatographic

AbstractA pre-column derivatized high-performance liquid chromatographic (HPLC) method with ultraviolet-visible detection was developed to measure the concentrations of spectinomycin in fermentation broth. Derivatization reagents, 2,4-dinitrophenylhydrazine in acetonitrile (5 mg mL−1) and trifluoroacetic acid in acetonitrile (0.8 mol L−1), were added to an aliquot of the fermentation broth, and the mixture was incubated for 60 min at 70°C. The resulting derivative was separated from other compounds by isocratic elution in a reversed-phase column Zorbax SB-C18 (250 mm × 4.6 mm, 5 µm). Mobile phase consisted of acetonitrile, tetrahydrofuran, and water (φ r = 40: 35: 25) and the flow rate was 1.0 mL min−1. The detection wavelength was 415 nm. The standard curve for spectinomycin sulfate was linear with correlation coefficients of 0.9997 in the range of 25 µg mL−1 to 600 µg mL−1. The relative standard deviation values ranged from 0.43 % to 2.18 % depending on the concentration of samples. The average recovery was 101.5 %. The limit of detection was 50 ng mL−1.

Fabrication of a novel Ti–TiO2–ZrO2 fiber for solid-phase microextraction followed by high-performance liquid chromatography for sensitive determination of UV filters in environmental water samples

2014 ◽  
Vol 6 (21) ◽  
pp. 8519-8525 ◽  
Author(s):  
Yi Li ◽  
Yaoxia Yang ◽  
Haixia Liu ◽  
Xuemei Wang ◽  
Xinzhen Du
Keyword(s):  
High Performance Liquid Chromatography ◽  
Water Samples ◽  
Solid Phase Microextraction ◽  
High Performance ◽  
Solid Phase ◽  
Environmental Water ◽  
Environmental Water Samples ◽  
Uv Filters ◽  
Sensitive Determination

A novel ZrO2 nanoparticle coated TiO2-based fiber for solid-phase microextraction was fabricated for sensitive determination of ultraviolet filters in environmental water samples.

scholarly journals Application of Packed-nanofibers Solid-phase Extraction for Determination of Rhodamine B in Sausage

2019 ◽  
Vol 8 (1) ◽  
pp. 17-21
Author(s):  
Lanlan Wei ◽  
Jianjun Deng ◽  
Tao Kang ◽  
Xuejun Kang
Keyword(s):  
Rhodamine B ◽  
High Performance ◽  
Orthophosphoric Acid ◽  
Limit Of Detection ◽  
Solid Phase ◽  
Volume Ratio ◽  
Standard Curve ◽  
Relative Standard ◽  
Limit Of Quantitation

A method for the determination of Rhodamine B in sausage was developed and validated. After extraction of Rhodamine B with acetonitrile from foodstuffs, a novel electrospun polymer nanofibers packed micro-column was used for cleaning and concentrating of the analyte in the sample. High performance liquid chromatography with fluorescence detection (HPLC-Flu) was used for the determination of Rhodamine B in the sample. The mobile phase was composed of 3.0 g L-1 phosphate buffer and methanol (3:7, volume ratio), and the pH was adjusted to 7. 0 with orthophosphoric acid. The results showed that the standard curve was linear over the validated concentrations range of 2-500 ng g-1, and the limit of detection (LOD) and the limit of quantitation (LOQ) for Rhodamine B spiked samples was 0. 2 ng g-1 and 0. 7 ng g-1, respectively. The average recoveries of Rhodamine B were 90.4% -94.3% for sausage, and the relative standard deviation of the method was from 1.7% to 3.8%. This proposed method was applied to real sample, and there was no Rhodamine B found in sausage.

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