Determination of trace amounts of polydimethylsiloxane in extracts of chemicals by proton nuclear magnetic resonance spectroscopy

Fux, Pierre

doi:10.1039/an9901500179

Cited by 9 publications

(3 citation statements)

References 7 publications

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“…Examples of application of 1 H-NMR in silicone analyses are the following [69]: identification of structural groups such as ethyl, trifluoropropyl, and isopropyl by characteristic splitting patterns; determination of chain length of low molecular weight (dp = 100 to 1000) PDMS by end group analysis; distinguishing stereoisomers and optical isomers; analysis of silanols [78]. Determination of silicones in environmental samples at 0.05 ppm has been reported [79]. The advantage of NMR analysis is the absence of interference from inorganic silicates.…”

Section: Spectroscopic Methodsmentioning

confidence: 99%

A Primer on the Analytical Aspects of Silicones at Trace Levels-Challenges and Artifacts – A Review

2006

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Silicones (polydimethylsiloxanes) find use in a wide variety of industrial and consumer product applications because of their outstanding properties. Potential human exposure to silicones occurs in the work place during manufacturing and product formulation, as well as through the normal use of consumer products containing them.The entry of silicones into various environmental compartments raised health and safety concerns from potential exposure and mandated numerous environmental and toxicological studies. Such studies require qualitative and quantitative determination of silicone species at trace levels. However, the ubiquitous presence of silicones coupled with their unique chemistry renders their analysis at trace levels challenging.This paper provides a consolidated account of various aspects of silicones that must be borne in mind to obtain reliable data. The following topics are discussed: differences in the chemistry of silicones vs carbon; precautions in sample handling to avoid losses and inadvertent chemical transformation; potential sources for artifacts and interferences that could lead to systematic errors and data misinterpretation; sources for background and the need for matrix matched blank experiments; distinguishing silicones from silicates to avoid overestimation; potential for incorrect structural assignments; preventing inadvertent contamination; and questionable claims on the presence of silicones in biological matrices including that of silicone implants.

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Section: Spectroscopic Methodsmentioning

confidence: 99%

A Primer on the Analytical Aspects of Silicones at Trace Levels-Challenges and Artifacts – A Review

2006

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“…A quantification limit of 0.1 mg kg À1 for PDMS was obtained by 1 H-NMR. 135 Other works by 1 H-NMR and 29 Si-NMR for determination of PDMS degradation products in animal models and human tissues have been related. [136][137][138] Indeed, Garrido et al have shown that silicon migrates from the implant to local and distant sites, and were located in tissues 136 and blood.…”

Section: Nmr Methodsmentioning

confidence: 99%

Silicon speciation by hyphenated techniques for environmental, biological and industrial issues: A review

Chainet

Lienemann

Courtiade

et al. 2011

J. Anal. At. Spectrom.

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Silicon speciation in environmental, biological and industrial matrices is of considerable importance due to its wide use in many consumer and personal care products and industry. In addition, the entry of silicones in various compartments like wastes, soils, air and water highlights the need to perform exposure studies, toxicological surveys and to measure negative effects. Due to possible contamination and trace level presence of silicon compounds, challenges to determination, identification and quantification are presented. The principal species of concern include siloxanes, silanols, silanediols and silanes. State of the art of analytical methods for total silicon determination and silicon speciation are established. Atomic spectroscopic methods are mainly used to measure total Si at trace concentration levels. On the opposite, hyphenated techniques are performed for Si speciation. Particular attention is paid to chromatographic methods coupled to sensitive and selective detectors (MS, AED and ICP) allowing structural information. Liquid and gas chromatography emerge as the most widespread separation techniques. However, other procedures such as MS, NMR, IR and XRF enable a better knowledge of these species. The potential and limitations of hyphenated techniques are highlighted, particularly concerning sensitivity and selectivity. Furthermore, potential sources of contamination and analytical artifacts in silicon determination are reviewed.

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“…In spectrum 3A corresponding to the brand-named formulation Prozac ® , the characteristic signals of FLX are detected and an average self-diffusion coefficient D = 1276 ± 9 m 2 s −1 is measured. The sole excipient partially soluble in CD 3 CN/D 2 O (80/20) is dimethicone, a polydimethylsiloxane, which presents 1 H NMR signals typical of di-and tri-methysilyl moiety at ≈0 ppm [29] and a self-diffusion coefficient of 913 m 2 s −1 .…”

Section: D Dosy 1 H Nmr Of Solutions Of Solid Commercial Formulationsmentioning

confidence: 99%

Quality assessment of fluoxetine and fluvoxamine pharmaceutical formulations purchased in different countries or via the Internet by 19F and 2D DOSY 1H NMR

Trefi

Gilard

Balayssac

et al. 2008

Journal of Pharmaceutical and Biomedical Analysis

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Determination of trace amounts of polydimethylsiloxane in extracts of chemicals by proton nuclear magnetic resonance spectroscopy

Cited by 9 publications

References 7 publications

A Primer on the Analytical Aspects of Silicones at Trace Levels-Challenges and Artifacts – A Review

A Primer on the Analytical Aspects of Silicones at Trace Levels-Challenges and Artifacts – A Review

Silicon speciation by hyphenated techniques for environmental, biological and industrial issues: A review

Quality assessment of fluoxetine and fluvoxamine pharmaceutical formulations purchased in different countries or via the Internet by 19F and 2D DOSY 1H NMR

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