scholarly journals Determination of sulfamerazine in aquatic products by molecularly imprinted capillary electrochromatography

2019 ◽  
Vol 6 (6) ◽  
pp. 190119 ◽  
Author(s):  
Shili Qin ◽  
Fenglong Jin ◽  
Lidi Gao ◽  
Liqiang Su ◽  
Yingjie Li ◽  
...  

A molecularly imprinted monolith was prepared and evaluated for the special selective separation of sulfamerazine (SMR) by capillary electrochromatography (CEC). The single-step in situ polymerization method was applied through thermally immobilized vinyl groups of itaconic acid and a derivatization capillary column using SMR as the template. The monolith with optimal selectivity and permeability was performed at 45°C for 7 h according to the molar ratios of 1 : 4 : 10 (template/functional monomer/cross-linker). Under the optimized separation conditions of 75% acetonitrile in 20 mM phosphate buffer with pH 5.0, 15 kV applied voltage and 20°C column temperature, the imprinted monolith showed strong recognition ability for SMR and high column performance. Finally, the molecularly imprinted monolith coupled with the CEC method was successfully developed for the quantification of SMR in aquatic products, which was properly validated by a good linear relationship, recoveries and limit of detection. The coupling technique of the molecularly imprinted technology and CEC achieved pre-treatment enrichment and separation analysis in only one miniaturized chromatographic column.

2013 ◽  
Vol 67 (5) ◽  
Author(s):  
Katarína Hroboňová ◽  
Andrea Spevak ◽  
Ľubica Spišská ◽  
Jozef Lehotay ◽  
Jozef Čižmárik

AbstractThe molecularly imprinted polymers (MIPs) were synthesised and the influence of the type of porogen, the nature of sample solvent, and the binding capacity of material were tested by high-performance liquid chromatography (HPLC). Umbelliferone was used as the template for imprint formation. Methacrylic acid was used as the monomer and acetonitrile, ethanol, and chloroform as porogen. Non-imprinted polymers (NIPs) were prepared by the same procedure. The highest value of the specific binding capacity (269 μg of umbelliferone per 100 mg of polymer) was obtained for polymers prepared in chloroform as porogen and methanol/water (φ r = 1: 1) as the sample solvent. The group-selective MIP was used as sorbent for the SPE pre-treatment of umbelliferone from plant extracts prior to HPLC analysis. Analysis of the spiked samples showed good recoveries (> 77 %). The limit of detection, limit of determination, and repeatability of the method were also calculated.


2019 ◽  
Vol 15 (3) ◽  
pp. 251-257
Author(s):  
Bahareh Sadat Yousefsani ◽  
Seyed Ahmad Mohajeri ◽  
Mohammad Moshiri ◽  
Hossein Hosseinzadeh

Background:Molecularly imprinted polymers (MIPs) are synthetic polymers that have a selective site for a given analyte, or a group of structurally related compounds, that make them ideal polymers to be used in separation processes.Objective:An optimized molecularly imprinted polymer was selected and applied for selective extraction and analysis of clozapine in rat brain tissue.Methods:A molecularly imprinted solid-phase extraction (MISPE) method was developed for preconcentration and cleanup of clozapine in rat brain samples before HPLC-UV analysis. The extraction and analytical process was calibrated in the range of 0.025-100 ppm. Clozapine recovery in this MISPE process was calculated between 99.40 and 102.96%. The limit of detection (LOD) and the limit of quantification (LOQ) of the assay were 0.003 and 0.025 ppm, respectively. Intra-day precision values for clozapine concentrations of 0.125 and 0.025 ppm were 5.30 and 3.55%, whereas inter-day precision values of these concentrations were 9.23 and 6.15%, respectively. In this study, the effect of lipid emulsion infusion in reducing the brain concentration of drug was also evaluated.Results:The data indicated that calibrated method was successfully applied for the analysis of clozapine in the real rat brain samples after administration of a toxic dose to animal. Finally, the efficacy of lipid emulsion therapy in reducing the brain tissue concentration of clozapine after toxic administration of drug was determined.Conclusion:The proposed MISPE method could be applied in the extraction and preconcentration before HPLC-UV analysis of clozapine in rat brain tissue.


2021 ◽  
Vol 11 (4) ◽  
pp. 1577
Author(s):  
Marco Mora-Granados ◽  
David González-Gómez ◽  
Jin Su Jeong ◽  
Alejandrina Gallego-Picó

Studies for monitoring the bioavailability of dietary flavonoid compounds generate great interest. Among them, low-molecular-weight phenolic acids, secondary metabolites present in colonic catabolism and urinary excretion, have been proposed as biomarkers of polyphenol intake. Using 4-hydroxyphenylacetic acid as a template, a molecularly imprinted polymer (MIP) was synthesized for selective extraction of these hydroxylated metabolites from human urine samples and posterior analysis in an HPLC-DAD-MS system. Polymers were characterized by Scanning electron microscopy (SEM), Attenuated total reflection-Fourier transform infrared spectroscopy (ATR-FTIR), Brunauer-Emmett-Teller (BET) method, and binding experiments. MIP presents specific recognition ability for template and analogues molecules. This capacity of recognition and the pH dependence of the binding strength was also studied. The method was validated over a concentration range of 0.25–40 mg/L, r2 > 0.995. In the optimized conditions, the recovery value was 94% with RSD 1.2%. The Limit of Detection (LOD) and Limit of Quantification (LOQ) were 1.22 and 3.69 mg/L, respectively. In our knowledge, it is the first time that this methodology is applied to analyze urinary catabolites of the polyphenol compound and to provide a specific method and simple analysis alternative. The selective extraction of these metabolites improves the application and results obtained by other less sensitive analysis methods than the validation method. It also facilitates the development of new screening methods.


2021 ◽  
Author(s):  
Xiaohan Zhang ◽  
Le Gao ◽  
Liying Niu ◽  
Xiaodong Bi

Molecularly imprinted polymers (MIPs) possess target-customized and range-adjustable selectivity, and hence have been attracting increasing efforts to develop new synthetic methods and new forms of applications. By wisely choosing functional...


2021 ◽  
Author(s):  
Kankan Swargiary ◽  
Romuald Jolivot ◽  
Waleed Soliman Mohammed

AbstractA polymer based horizontal single step waveguide for the sensing of alcohol is developed and analyzed. The waveguide is fabricated by 3-dimensional (3D) printing digital light processing (DLP) technology using monocure 3D rapid ultraviolet (UV) clear resin with a refractive index of n = 1.50. The fabricated waveguide is a one-piece tower shaped ridge structure. It is designed to achieve the maximum light confinement at the core by reducing the effective refractive index around the cladding region. With the surface roughness generated from the 3D printing DLP technology, various waveguides with different gap sizes are printed. Comparison is done for the different gap waveguides to achieve the minimum feature gap size utilizing the light re-coupling principle and polymer swelling effect. This effect occurs due to the polymer-alcohol interaction that results in the diffusion of alcohol molecules inside the core of the waveguide, thus changing the waveguide from the leaky type (without alcohol) to the guided type (with alcohol). Using this principle, the analysis of alcohol concentration performing as a larger increase in the transmitted light intensity can be measured. In this work, the sensitivity of the system is also compared and analyzed for different waveguide gap sizes with different concentrations of isopropanol alcohol (IPA). A waveguide gap size of 300 µm gives the highest increase in the transmitted optical power of 65% when tested with 10 µL (500 ppm) concentration of IPA. Compared with all other gaps, it also displays faster response time (t = 5 seconds) for the optical power to change right after depositing IPA in the chamber. The measured limit of detection (LOD) achieved for 300 µm is 0.366 µL. In addition, the fabricated waveguide gap of 300 µm successfully demonstrates the sensing limit of IPA concentration below 400 ppm which is considered as an exposure limit by “National Institute for Occupational Safety and Health”. All the mechanical mount and the alignments are done by 3D printing fused deposition method (FDM).


2012 ◽  
Vol 441 ◽  
pp. 640-644
Author(s):  
Ke Jie Fu ◽  
Li Sheng Yang ◽  
Chang Sheng Feng ◽  
Liang Chen

A detecting method for toxic flame retardant finishing agent tris-(2,3-dibromopropyl) -phosphate (TRIS for short) in textiles was studied. In the method, an acetonitrile ultrasound-assisted extraction process was included in sample pre-treatment, and HPLC/DAD was used in the separation and identification of extractives. After that, the conditions of pre-treatment and chromatograph were optimized. The results showed that the limit of detection (LOD) by this method (S/N10) is 1.0 mg/kg, its recovery ranged from 78.1% to 98.4%, and RSD of the precision test is 3.2%, of which all met the requirements for routine testing.


Author(s):  
Sandip A Telavane ◽  
Seema Kothari ◽  
Manohar V. Lokhande

Validation is important technique for detection, progress and estimation of drugs for pharmaceutical analysis. Aim of this article was to check the progress and validation of the method employed for the Residual Solvents in Bisoprolol Fumarate by Gas Chromatographic technique. The objective of this protocol is to validate a GC method of analysis for detection and Quantification of Residual Solvents Methanol, Acetone and Methylene dichloride in Bisoprolol Fumarate. In the pharmaceutical industry, validation policy is more important for documented of validation, types of validation and validation policy. The method was developed accurately and validation parameters are explained. Chromatographic condition was GC- 2014, gas chromatograph equipped with FID detector, column: 30 m x 0.32 mm ID x 1.8 µm DB - 624 capillary column or equivalent and column temperature was 45°C (hold 7 minutes) to 250°C @ 40°C/minutes, hold at 250°C for 3 minutes. The parameters such as Accuracy, Specificity, Precision, Linearity and Range, Limit of detection (LOD), Limit of quantitation (LOQ), ruggedness, robustness and system suitability testing with residual solvent such as Methanol, Acetone and methylene dichloride. All validation parameters are used in the routine and stability analysis.


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