研究目的
The aim of this work was to expand the applicability of the trace level and simple, high sample throughput analytical method based on TLS detection for determination of colloidal, ionic and total silver contents to the analysis of personal care products based on colloidal silver. We also aimed to validate the performance of the method in case of other samples rather than drinking water, e.g. personal care products, and the performance of the method as analytical tool for quality control in case of personal care products containing colloidal silver.
研究成果
The study demonstrated that TLS is a highly sensitive and accurate method for determining colloidal and total silver in personal care products. It revealed that the examined products contained significantly less colloidal silver than declared, with ionic silver being the predominant form. The findings underscore the need for stringent quality control in products marketed as containing colloidal silver.
研究不足
The study was limited by the nonlinearity of TLS calibration curves at higher concentrations of colloidal silver, attributed to changes in nanoparticle size distribution. Additionally, the spectrophotometric method was less sensitive compared to TLS, with higher LOD and LOQ values.
1:Experimental Design and Method Selection:
The study utilized thermal lens spectrometry (TLS) in both batch mode (BM) and flow injection analysis (FIA) configurations for the determination of colloidal silver in personal care products. The method selection was based on the need for high sensitivity and accuracy in detecting trace levels of colloidal silver.
2:Sample Selection and Data Sources:
Five commercially available personal care products declared to contain nanosilver were examined. Samples included nasal spray, wound disinfection water, nose drops, and water for internal intake.
3:List of Experimental Equipment and Materials:
Equipment included a dual-beam TLS spectrometer, UV-VIS spectrophotometer, ICP-OES spectrometer, and SEM for nanoparticle characterization. Materials included AgNO3, NaBH4, NaOH, and HNO3 for sample preparation and analysis.
4:Experimental Procedures and Operational Workflow:
Samples were analyzed directly for colloidal silver content and after chemical conversion of ionic silver to colloidal form for total silver determination. TLS measurements were performed in batch and FIA modes, with comparative analyses using spectrophotometry and ICP-OES.
5:Data Analysis Methods:
Data were analyzed using calibration curves constructed from standard solutions. Statistical analysis included calculation of LODs, LOQs, and confidence intervals to validate method performance.
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Photodiode
PDA 36A-EC
THORLABS
Detection of the thermal lens signal.
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Lock-in amplifier
SR830 DSP
STANFORD RESEARCH INSTRUMENTS
Signal processing for TLS measurements.
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UV-VIS spectrophotometer
Lambda 650
PERKIN ELMER
Recording plasmon resonance absorption spectra of silver nanoparticles.
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SEM
JSM-7100F
JEOL
Recording scanning electron micrographs of synthesized nanoparticles.
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Dual-beam TLS spectrometer
Innova 300C
COHERENT
Used for thermal lens spectrometry measurements in batch mode.
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He-Ne laser
1103P
UNIPHASE
Probe beam source for TLS measurements.
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Mechanical chopper
300C
SCIENTIC INSTRUMENTS
Modulation of the pump beam.
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ICP-OES spectrometer
715 ES
VARIAN
Quantitation of total ionic silver concentrations.
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DLS system
90 plus/Bi-mas
Brook Haven
Determination of AgNPs size in solution.
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