1992Journal of Liquid ChromatographyRequires access

Solid-Phase Extraction (SPE) and HPLC Analysis of Toxic Compounds and Comparison of SPE and Liquid-Liquid Extraction. I. Analysis of 4, 4′-Methyl-Enedianiline in Serum. II. Analysis of the Components of Dental Materials

Hideharu Shintani

Open publisher page 18 citations

Abstract

In this paper, we discuss two subjects concerned with solid phase extraction (SPE) and HPLC analysis of toxic compounds eluted to serum from materials used for medical devices. SPE and liquid-liquid extraction for serum toxic compounds were compared. Firstly, an analysis of a toxic and carcinogenic compound, 4,4′-methylenedianiline (MDA), from polyurethane sterilized by gamma-ray irradiation was studied. Serum MDA was analyzed to assess the potential MDA risk to patients exposed to PU medical devices. MDA was determined by reverse-phase HPLC using an eluent of a mixed solution of ammonium acetate and acetonitrile. An ODS column was used. Detection was carried out by an electrochemical detector (ECD). As liquid-liquid extraction was complex due to deproteinization followed by centrifuge separation and concentration, we substituted SPE. Serum MDA was satisfactorily recovered using Bond Elut C-18, Phenyl and Cyclohexyl columns. The recovery of serum MDA from Bond ElutR C-1, C-2, C-8 and Silica was unsatisfactory. Elution was carried out using methanol containing lM NH4.OH. SPE was superior to a liquid-liquid extraction due to an unnecessary of denroteinization, centrifuge separation and concentration. Secondly, we analyzed the toxic compounds, methyl methacrylate (MMA), N, N-dimethyl p-toluidine (DMPT), and benzoylperoxide (BPO), all of which are components of the dental material of polymethyl methacrylate (PMMA). PMMA is widely used as the composite resin. for the dental plate. BPO was converted to benzoic acid (BA) when in contact with DMPT or serum, therefore BA analysis is necessary for BPO determination. As these compounds exhibit a potential for residue as well as toxicity, determination method and safety evaluation are required. Analysis was by HPLC combined with SPE using a C-18 column in both methods.

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In this paper, we discuss two subjects concerned with solid phase extraction (SPE) and HPLC analysis of toxic compounds eluted to serum from materials used for medical devices. SPE and liquid-liquid extraction for serum toxic compounds were compared. Firstly, an analysis of a toxic and carcinogenic compound, 4,4′-methylenedianiline (MDA), from polyurethane sterilized by gamma-ray irradiation was studied. Serum MDA was analyzed to assess the potential MDA risk to patients exposed to PU medical devices. MDA was determined by reverse-phase HPLC using an eluent of a mixed solution of ammonium acetate and acetonitrile. An ODS column was used. Detection was carried out by an electrochemical detector (ECD). As liquid-liquid extraction was complex due to deproteinization followed by centrifuge separation and concentration, we substituted SPE. Serum MDA was satisfactorily recovered using Bond Elut C-18, Phenyl and Cyclohexyl columns. The recovery of serum MDA from Bond ElutR C-1, C-2, C-8 and Silica was unsatisfactory. Elution was carried out using methanol containing lM NH4.OH. SPE was superior to a liquid-liquid extraction due to an unnecessary of denroteinization, centrifuge separation and concentration. Secondly, we analyzed the toxic compounds, methyl methacrylate (MMA), N, N-dimethyl p-toluidine (DMPT), and benzoylperoxide (BPO), all of which are components of the dental material of polymethyl methacrylate (PMMA). PMMA is widely used as the composite resin. for the dental plate. BPO was converted to benzoic acid (BA) when in contact with DMPT or serum, therefore BA analysis is necessary for BPO determination. As these compounds exhibit a potential for residue as well as toxicity, determination method and safety evaluation are required. Analysis was by HPLC combined with SPE using a C-18 column in both methods.

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Available abstract

In this paper, we discuss two subjects concerned with solid phase extraction (SPE) and HPLC analysis of toxic compounds eluted to serum from materials used for medical devices. SPE and liquid-liquid extraction for serum toxic compounds were compared. Firstly, an analysis of a toxic and carcinogenic compound, 4,4′-methylenedianiline (MDA), from polyurethane sterilized by gamma-ray irradiation was studied. Serum MDA was analyzed to assess the potential MDA risk to patients exposed to PU medical devices. MDA was determined by reverse-phase HPLC using an eluent of a mixed solution of ammonium acetate and acetonitrile. An ODS column was used. Detection was carried out by an electrochemical detector (ECD). As liquid-liquid extraction was complex due to deproteinization followed by centrifuge separation and concentration, we substituted SPE. Serum MDA was satisfactorily recovered using Bond Elut C-18, Phenyl and Cyclohexyl columns. The recovery of serum MDA from Bond ElutR C-1, C-2, C-8 and Silica was unsatisfactory. Elution was carried out using methanol containing lM NH4.OH. SPE was superior to a liquid-liquid extraction due to an unnecessary of denroteinization, centrifuge separation and concentration. Secondly, we analyzed the toxic compounds, methyl methacrylate (MMA), N, N-dimethyl p-toluidine (DMPT), and benzoylperoxide (BPO), all of which are components of the dental material of polymethyl methacrylate (PMMA). PMMA is widely used as the composite resin. for the dental plate. BPO was converted to benzoic acid (BA) when in contact with DMPT or serum, therefore BA analysis is necessary for BPO determination. As these compounds exhibit a potential for residue as well as toxicity, determination method and safety evaluation are required. Analysis was by HPLC combined with SPE using a C-18 column in both methods.

Key concepts: Solid phase extraction, Extraction (chemistry), Chromatography, High-performance liquid chromatography, Elution, Ammonium acetate, Chemistry, Methacrylate

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Solid-Phase Extraction (SPE) and HPLC Analysis of Toxic Compounds and Comparison of SPE and Liquid-Liquid Extraction. I. Analysis of 4, 4′-Methyl-Enedianiline in Serum. II. Analysis of the Components of Dental Materials — Research Paper | ScholarLens