Rapid determination of silicone oil lubricant in elastomeric closures by ICP-OES
A rapid method for determination of silicone oil in elastomeric closures of injection syringes by inductively coupled plasma optical emission spectrometry (ICP-OES) is presented. The silicone oil was extracted from the intact closure using a mixture of methyl isobutyl ketone and 1-pentanol, no furth...
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Published in | Analytical methods Vol. 5; no. 16; pp. 4263 - 4267 |
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Main Authors | , , , , |
Format | Journal Article |
Language | English |
Published |
01.01.2013
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Subjects | |
Online Access | Get full text |
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Summary: | A rapid method for determination of silicone oil in elastomeric closures of injection syringes by inductively coupled plasma optical emission spectrometry (ICP-OES) is presented. The silicone oil was extracted from the intact closure using a mixture of methyl isobutyl ketone and 1-pentanol, no further sample treatment was necessary. Quantitation was based on response from Si(i) at 288.158 nm using external calibration with standard solutions of silicone oil dissolved in the same extraction mixture. A supplemental flow of oxygen was used to decrease background interference, providing a detection limit (3s, n= 10) of 0.05 mg of silicone per L. The LOQ (10s, n= 10) was 0.15 mg silicone per L, equivalent to 3.8 mu g silicone/sample of elastomeric closure, based on 25 mL of extraction solvent per closure. The same samples were also analyzed by high-resolution flame atomic absorption spectrometry (HR-CS F-AAS), providing results similar to those obtained by ICP-OES. Spike recoveries of 97-104% demonstrated the accuracy of the methodology. Precision, expressed as the relative standard deviation, was 0.7-3.0% under conditions of repeatability and 0.7-3.3% for reproducibility. This simple procedure has been adopted by the Institute of Technology of Parana - TECPAR (Curitiba, Brazil). |
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Bibliography: | ObjectType-Article-2 SourceType-Scholarly Journals-1 ObjectType-Feature-1 content type line 23 |
ISSN: | 1759-9660 1759-9679 |
DOI: | 10.1039/c3ay40754c |