β-Cyclodextrin Derivative Grafted on Silica Gel Represents a New Polymeric Sorbent for Extracting Nitisinone from Model Physiological Fluids

Nitisinone (NTBC) is used in the treatment of disorders affecting the tyrosine pathway, including hereditary tyrosinemia type I, alkaptonuria, and neuroblastoma. An inappropriate dosage of this therapeutic drug causes side effects; therefore, it is necessary to develop a rapid and sensitive method to monitor the content of NTBC in patients’ blood. This study aimed to develop anew polymeric sorbent containing β-cyclodextrin (β-CD) derivatives grafted on silica gel to effectively extract NTBC from model physiological fluids. The inclusion complex formed between β-CD and NTBC was examined by proton nuclear magnetic resonance spectroscopy. The novel sorbents with derivatives of β-CD were prepared on modified silica gel using styrene as a comonomer, ethylene glycol dimethacrylate as a crosslinking agent, and 2,2′-azo-bis-isobutyronitrile as a polymerization initiator. The obtained products were characterized via Fourier transform infrared spectroscopy and then used as sorbents as part of a solid phase extraction technique. High NTBC recovery (70%indicated that the developed polymeric sorbent may be suitable for extracting this compound from patients’ blood samples.

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Quantification of Mineral Oil Aromatic Hydrocarbons (MOAH) in Anhydrous Cosmetics Using 1H NMR

Journal of Chemistry ◽

10.1155/2019/1680269 ◽

2019 ◽

Vol 2019 ◽

pp. 1-10 ◽

Cited By ~ 1

Author(s):

Sandra Weber ◽

Tamina Schmidt ◽

Paul Schumacher ◽

Thomas Kuballa ◽

Gerd Mildau ◽

...

Keyword(s):

Silica Gel ◽

Aromatic Hydrocarbons ◽

Solid Phase ◽

Complete Removal ◽

Mineral Oil ◽

Retail Trade ◽

Butylated Hydroxytoluene ◽

Proton Nuclear Magnetic Resonance ◽

Resonance Spectroscopy ◽

Branched Chains

In cosmetic products, hydrocarbons from mineral oil origin are used as ingredients in a wide variety of consistency, from liquid oil to solid wax. Refined mineral oil hydrocarbons consist of MOSH (mineral oil saturated hydrocarbons) and a low proportion of MOAH (mineral oil aromatic hydrocarbons). MOSH and MOAH comprise a variety of chemically similar single substances with straight or branched chains. In the context of precautionary consumer protection, it is crucial to determine hydrocarbons from mineral oil origin of inferior quality quickly and efficiently. This publication presents a rapid method for quantifying MOAH by proton nuclear magnetic resonance spectroscopy (1H qNMR) in anhydrous cosmetics such as lipstick, lip gloss, and lip balm. A sample clean-up using solid-phase extraction (SPE) was developed for the complete removal of interfering aromatic substances to improve the robustness of the method for analysing compounded cosmetics. In preliminary trials using silica gel thin-layer chromatography, the retention behaviour of 21 common aromatic compounds was tested in eluents with different solvent strength including EtOAc, MeOH, cyclohexane, and dichloromethane. Based on these results, the SPE sample cleanup with silica gel and cyclohexane as an eluent was suggested as best suitable for the purpose. The SPE cleanup was successfully achieved for all tested potentially interfering aromatic cosmetic ingredients except for butylated hydroxytoluene. The recovery for lipophilic cosmetics is more than 80% based on naphthalene as calculation equivalent. Furthermore, a specific sample preparation for the examination of lipsticks was implemented. The SPE cleanup was validated, and the robustness of the method was tested on 57 samples from the retail trade. The 1H qNMR method is a good complement to the LC-GC-FID method, which is predominantly used for the determination of MOSH and MOAH. Chromatographic problems such as migration of MOSH into the MOAH fraction during LC-GC-FID can be avoided.

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The Solid Phase Extraction of Some Metal Ions Using Palladium Nanoparticles Attached to Silica Gel Chemically Bonded by Silica-Bonded N-Propylmorpholine as New Sorbent prior to Their Determination by Flame Atomic Absorption Spectroscopy

The Scientific World JOURNAL ◽

10.1100/2012/764195 ◽

2012 ◽

Vol 2012 ◽

pp. 1-9 ◽

Cited By ~ 8

Author(s):

M. Ghaedi ◽

M. Rezakhani ◽

S. Khodadoust ◽

K. Niknam ◽

M. Soylak

Keyword(s):

Electron Microscopy ◽

Metal Ions ◽

Silica Gel ◽

Solid Phase ◽

Food Samples ◽

Natural Food ◽

Modified Silica Gel ◽

Flame Atomic Absorption ◽

Relative Standard

In this research at first palladium nanoparticle attached to a new chemically bonded silica gel has been synthesized and has been characterized with different techniques such as X-ray diffraction (XRD), fourier transform infrared (FT-IR), transmission electron microscopy (TEM), and scanning electron microscopy (SEM). Then, this new sorbent (chemically modified silica gel with N-propylmorpholine (PNP-SBNPM)) was efficiently used for preconcentration of some metal ions in various food samples. The influence of effective variables including mass of sorbent, flow rate, pH of sample solutions and condition of eluent such as volume, type and concentration on the recoveries of understudy metal ions were investigated. Following the optimization of variables, the interfering effects of some foreign ions on the preconcentration and determination of the investigated metal ions described. At optimum values of variables, all investigated metal ions were efficiently recovered with efficiency more than 95%, relative standard deviation (RSD) between 2.4 and 2.8, and detection limit in the range of 1.4–2.7 ng mL−1. The present method is simple and rapidly applicable for the determination of the understudied metal ions (ng mL−1) in different natural food samples.

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Functionalization of silica gel with 5-hydroxymethylfurfural: preparation, characterization and preliminary verification

New Journal of Chemistry ◽

10.1039/c6nj03815h ◽

2017 ◽

Vol 41 (12) ◽

pp. 4738-4742 ◽

Cited By ~ 3

Author(s):

Cheng Wang ◽

Limin Huang ◽

Yuanyuan Lin ◽

Youjia Li ◽

Yajing Hou ◽

...

Keyword(s):

Liquid Chromatography ◽

Silica Gel ◽

Solid Phase ◽

Hybrid Composites ◽

Modified Silica ◽

Modified Silica Gel ◽

Inorganic Hybrid

Herein, we report the organic–inorganic hybrid composites comprising surficial-modified silica gel with 5-HMF as a solid phase for liquid chromatography.

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Determination of Gentamicins C1, C1a, and C2 in Plasma and Urine by HPLC

Clinical Chemistry ◽

10.1093/clinchem/46.6.837 ◽

2000 ◽

Vol 46 (6) ◽

pp. 837-842 ◽

Cited By ~ 34

Author(s):

Nina Isoherranen ◽

Stefan Soback

Keyword(s):

Solid Phase Extraction ◽

Solid Phase ◽

Preparative Chromatography ◽

Detector Response ◽

Therapeutic Drug ◽

Resonance Spectroscopy ◽

Pharmacokinetic Studies ◽

Phase Extraction ◽

Limit Of Quantification

Abstract Background: Gentamicin is an aminoglycoside antibiotic complex containing gentamicins C1, C1a, and C2. Few methods have been described for analysis of the three gentamicin components separately in biological fluids, and none has been used in pharmacokinetic studies. Determination of the three gentamicins separately may have pharmacokinetic and toxicological implications. The present study describes development of an HPLC method for the analysis of gentamicin C1, C1a, and C2 components in plasma and urine. Methods: The three components were isolated by preparative chromatography and their identities verified by thin-layer chromatography, HPLC, mass spectrometry, nuclear magnetic resonance spectroscopy, and melting point determination. The gentamicins were extracted from the biological matrix by use of Tris buffer and polymer phase solid-phase extraction. Derivatization was carried out in the solid-phase extraction cartridge with 1-fluoro-2,4-dinitrobenzene. The 2,4-dinitrophenyl derivatives were separated with reversed-phase HPLC and quantified by the ultraviolet absorbance at 365 nm. Results: The detector response was linear from the limit of quantification to 50 mg/L for the individual components. The limit of quantification was 0.07 mg/L for gentamicin C1 and 0.1 mg/L for gentamicins C2 and C1a. The recovery of the gentamicin components was 72% from plasma and 98% from urine. The method was validated for human and dog plasma and urine. Conclusions: The method was repeatable and enabled the analysis of gentamicins C1, C1a, and C2 in plasma and urine in concentrations covering the therapeutic range of the drug, thus being suitable for therapeutic drug monitoring and pharmacokinetic studies.

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Effective phospholipid removal from plasma samples by solid phase extraction with the use of copper (II) modified silica gel cartridges

Journal of Chromatography B ◽

10.1016/j.jchromb.2017.10.021 ◽

2017 ◽

Vol 1070 ◽

pp. 1-6 ◽

Cited By ~ 1

Author(s):

Jolanta Flieger ◽

Małgorzata Tatarczak-Michalewska ◽

Anna Kowalska ◽

Anna Madejska ◽

Tomasz Śniegocki ◽

...

Keyword(s):

Solid Phase Extraction ◽

Silica Gel ◽

Solid Phase ◽

Phase Extraction ◽

Plasma Samples ◽

Modified Silica ◽

Modified Silica Gel

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Preparation of Imprinted Polymer with D-Phenylalanin on Silica Surface

Key Engineering Materials ◽

10.4028/www.scientific.net/kem.419-420.541 ◽

2009 ◽

Vol 419-420 ◽

pp. 541-544

Author(s):

Hong Xing Dong ◽

Qiu Li Jiang ◽

Fei Tong ◽

Zhen Xing Wang ◽

Jin Yong Tang

Keyword(s):

Silica Gel ◽

High Performance ◽

Silica Surface ◽

Solid Phase ◽

Adsorption Property ◽

Research Field ◽

Imprinted Polymer ◽

Modified Silica ◽

Modified Silica Gel ◽

Functional Monomers

Silica gel was modified with polymerizable double bonds on the surface. Then the molecular imprinting polymer imprinted with D-Phenylalanin was grafted on the surface of modified silica gel. The molecularly imprinted polymer (MIP) based on the surface of silica gel was characterized by IR and scanning electron microscopy (SEM). The adsorption property of D-Phenylalanin by MIP was mearsured. The MIP with the combined functional monomers exhibited better adsorption properties and selectivity compared with the corresponding non-imprinted polymers or MIP with the single functional monomer. The material could be used in separation research field, such as packing material of high performance liquid chromatography, solid-phase extraction and so on.

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Solid-phase extraction with injection of modified silica gel slurries into ETAAS for determination of Cu(II), Hg(II), Pd(II)

International Journal of Environmental Science and Technology ◽

10.1007/s13762-018-1917-2 ◽

2018 ◽

Vol 16 (7) ◽

pp. 2885-2894 ◽

Cited By ~ 1

Author(s):

D. N. Konshina ◽

M. Yu. Burylin ◽

R. Anashkin ◽

V. V. Konshin

Keyword(s):

Solid Phase Extraction ◽

Silica Gel ◽

Solid Phase ◽

Phase Extraction ◽

Modified Silica ◽

Modified Silica Gel

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Use of proton nuclear magnetic resonance spectroscopy in detection and study of organic acidurias.

Clinical Chemistry ◽

10.1093/clinchem/31.11.1795 ◽

1985 ◽

Vol 31 (11) ◽

pp. 1795-1801 ◽

Cited By ~ 81

Author(s):

R A Iles ◽

A J Hind ◽

R A Chalmers

Keyword(s):

Nuclear Magnetic Resonance ◽

Magnetic Resonance ◽

Magnetic Resonance Spectroscopy ◽

Nuclear Magnetic Resonance Spectroscopy ◽

Clinical Care ◽

Proton Nuclear Magnetic Resonance ◽

Resonance Spectroscopy ◽

Type I ◽

Organic Acidurias ◽

Nuclear Magnetic

Abstract We used high-resolution proton nuclear magnetic resonance spectroscopy to detect, identify, and study the major normal and abnormal organic acid metabolites in urine from patients with propionic acidemia, methylmalonic aciduria, branched-chain ketoaciduria, isovaleric acidemia, and glutaric aciduria type I. Characteristic and diagnostic spectra were obtained at 400 MHz for each disorder in all the patients studied and neutral and basic compounds, including amino acids and acylcarnitines, were also detected. The technique is rapid (10 min) and requires small samples (0.5 mL) and no preliminary extraction or derivative preparation. We believe that it is particularly suitable for the rapid and acute diagnosis of inborn errors of metabolism, especially the organic acidurias, and for acute pediatric clinical care, when rapid monitoring of major metabolic alterations is required in a time scale suitable to influence directly and immediately the therapy of the patients concerned.

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