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在引入固相萃取(SPE)C4前处理技术的基础上,首次采用气相色谱质谱联用(GC-MS)和离子色谱(ICS)技术定性、定量化评估了SPE C4柱对常见文物保存环境中可溶盐离子的排除效果,进一步探讨了该技术对氨基酸分析结果的影响、保护色谱柱的效果及对文物样品测试的适用性。结果表明,SPE C4技术能有效排除Na~+,K~+,Mg~(2+),Ca~(2+),Cl~-,NO_3~-,SO_4~(2-)等常见可溶盐离子,平均洗脱率(脱盐率)达99.99%;添加30 g/L NaCl的猪皮胶经SPE C4处理后测得的色谱图出峰完整,未检测到Na~+和Cl~-,11种氨基酸含量测量结果的平均相对误差约5%。文物样品氨基酸色谱图基线平稳、分离良好。因此,SPE C4技术适用于中国古代蛋白胶料气相色谱分析的前处理中,对分析鉴定我国古代文物蛋白胶料具有极高的实用价值。
Based on the introduction of solid phase extraction (SPE) C4 pretreatment technology, GC-MS and ICS were used for the qualitative and quantitative assessment of the effects of SPE C4 column on the preservation of common cultural relics The effect of soluble salt ion exclusion is further explored. The effect of this technique on the amino acid analysis, the effect of protecting the column and the applicability of the sample to the cultural relics testing are discussed. The results show that SPE C4 can effectively eliminate common soluble salts such as Na ~ +, K ~ +, Mg ~ (2 +), Ca ~ (2 +), Cl ~ -, NO_3 ~ - and SO_4 ~ Ions, the average elution rate (desalination rate) was 99.99%. The chromatograms of pigskin supplemented with 30 g / L NaCl after SPE C4 treatment showed a complete peak without Na ~ + and Cl ~ -, 11 The average relative error of the amino acid content measurements is about 5%. Amino acid chromatograms of cultural relics samples were stable and well separated. Therefore, SPE C4 technology is suitable for the pre-treatment of gas chromatographic analysis of ancient Chinese protein compounds, and has very high practical value for the analysis and identification of ancient Chinese cultural protein compounds.