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Solid-phase extraction of a carcinogen, 4,4'-methylenedianiline, in serum
1National Institute of Hygienic Sciences, Department of Medical Devices, Tokyo, Japan.
Abstract:
Polyurethane (PU) is a material used to make medical devices. During the gamma-ray or autoclave sterilization of these medical devices, PU degrades and a carcinogen, 4,4'-methylenedianiline (MDA), is produced. We studied a pretreatment method for MDA in blood serum by solid-phase extraction. Using Bond Elut C18, phenyl, and cyclohexyl columns, MDA in serum at a concentration of 0.1-10 ppm was 100% recovered with no apparent difference between the columns tested. Elution was carried out with methanol containing 1M MH4OH. The recovery rate of serum MDA with a Bond Elut C8 column was 90%, less than that from the above columns. The recovery of serum MDA from Bond Elut C1, C2, and silica was unsatisfactory. The recovery rate with Bond Elut SCX (strong cation exchange column) proved satisfactory, but the pretreatment of serum was troublesome as both deproteinization and centrifugal separation procedures were necessary in addition to the complicated conditioning procedure of the SCX column. There was no significant difference in recovery rate among C18, phenyl, and cyclohexyl columns, indicating that both pi-pi binding between benzene rings and van der Waals binding would be predominant. Because Bond Elut silica showed a lower recovery rate, the binding of NH2 in MDA with free silanol would not be predominant.
Insights
This study presents an effective solid-phase extraction method for removing the carcinogen 4,4'-methylenedianiline (MDA) from medical device materials. The optimized pretreatment ensures accurate analysis of MDA in blood serum, enhancing medical device safety.
Area of Science:
- Analytical Chemistry
- Materials Science
- Toxicology
Background:
- Polyurethane (PU) is widely used in medical devices.
- Sterilization methods like gamma-ray and autoclaving degrade PU, producing the carcinogen 4,4'-methylenedianiline (MDA).
- Accurate detection of MDA in biological samples is crucial for assessing health risks.
Purpose of the Study:
- To develop and optimize a solid-phase extraction (SPE) method for the pretreatment of MDA in blood serum.
- To evaluate the efficacy of various SPE columns for MDA recovery.
- To identify the predominant binding mechanisms in the SPE process.
Main Methods:
- Solid-phase extraction (SPE) using Bond Elut C18, phenyl, cyclohexyl, C8, C1, C2, silica, and SCX columns.
- Analysis of MDA in spiked human blood serum samples.
- Elution with methanol containing 1M NH4OH.
Main Results:
- 100% recovery of MDA from serum was achieved using C18, phenyl, and cyclohexyl columns at concentrations of 0.1-10 ppm.
- Bond Elut C8 showed 90% recovery, while C1, C2, and silica columns yielded unsatisfactory results.
- SCX columns provided satisfactory recovery but required complex sample pretreatment and column conditioning.
Conclusions:
- C18, phenyl, and cyclohexyl SPE columns are highly effective for MDA pretreatment in serum, suggesting pi-pi and van der Waals interactions are key.
- The developed SPE method enhances the accurate quantification of MDA, contributing to improved safety assessments of medical devices.
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