涡旋-离心处理油样-毛细管GC-MS-SIM分析技术
首发时间:2009-07-02
摘要:建立了涡旋-离心处理油样-毛细管GC-MS-SIM分析技术方法,优化了影响涡旋离心处理油样-毛细管GC-MS-SIM分析的主要影响因素,如提取液的种类、油样浓度的大小、吸附剂硅胶的用量大小、毛细管柱的类型、升温速率等,结果表明,6mL 1:1正己烷-二氯甲烷混合液(v/v)、油样浓度为2.1mg/mL、1g硅胶的离心涡旋净化油样,采用6℃/min的程序升温、HP-5MS(30m×0.25 mm或0.32mm×0.25μm)毛细管柱可以很好地分离油样中的生物标志物。涡旋-离心处理油样与柱层析法处理油样相比,有很好的可靠性,用生物标志物的诊断比值可鉴别油种。
关键词: 硅胶 涡旋-离心 油样 生物标志物 诊断比值 GC-MS-SIM
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Cleaning of Spilled Oils with Silica Gel Swirl-Centrifugal Separation and Analyzing by GC-MS-SIM
Abstract:A technical method for cleaning of samples of spilled oils with silica gel swirl-centrifugal separation and analyzing by gas chromatography coupled with mass spectrometry selected ion monitoring (GC-MS-SIM) with capillary column has been established. Optimizing the kinds of extract solvent, the concentrations of samples of oils, the quantities of silica gel or alumina as sorbent, the types of capillary column and the ratios of increased temperatures in program. The conditions of cleaning of samples of spilled oils with silica gel swirl-centrifugal separation have been obtained. The optimized condition of cleaning for concentrations of 2.1 mg/mL of spilled oils adsorbed in 1g of silica gel or alumina with extraction of 6 mL mix solution of hexane and dichloromethane and (1:1, v/v) and analysis by GC-MS-SIM with capillary column in HP-5MS(30m of length, 0.25 mm or 0.32mm in diameter and 0.25μm of film thickness)in 6℃/min of ratios of increased temperatures in program could be obtained. It has been indicated that the method for silica gel swirl-centrifugal separation compared with the method for chromatographic column, it is feasible for cleaning of samples of spilled oils, and identifying for kinds of oils with diagnostic ratios of biomarkers in spilled oils by GC-MS-SIM.
Keywords: silica gel swirl-centrifugal separation samples of oils biomarkers diagnostic ratio GC-MS-SIM
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No.3359088404124652****
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