摘要
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。
The soluble salts ions contributed to the great part of the impurities, which would exert obvious influence in the separation and analysis with Gas Chromatography （GC）. In this paper, Solid- Phase Extraction C4 （SPE C4） technology was introduced in the pre-treatments, and the ions elution effects were explored qualitatively and quantitatively for the first time. Moreover, the deviation for the amino acids contents, the safeguarding property for the chromatography column and the applicability on the artwork samples analysis were discussed respectively. Results illustrated that the SPE C4 could effectively absorb the common soluble ions such as Na ＋ , K ＋ , Mg2＋ , Ca2 ＋ , Cl- , NO3-and SO42- with the 99. 99% average elution ratio. The amino acids contents of the pig hide glue with 30 g/L NaC1 showed the mere 5 % average deviation after purification with the SPE C4, and the GC chromatograms of the artwork samples were excellent with stable baselines and perfect individual amino acids peaks. Therefore, the SPE C4 technology was applicable in the artwork proteinaceous binding medium analysis with GC, which was of high practicable values.
作者
马珍珍
王丽琴
杨璐
张亚旭
吴玥
MA Zhen-zhen WANG Li-qin ＊ YANG Lu ZHANG Ya-xu WU Yue(College of Cultural Heritage, Northwest University, Xi＇an 710069 Key Laboratory of Cultural Heritage Research and Conservation, Northwest University, Ministry of Education, Xi＇an 710069)
出处
《分析试验室》
CAS
CSCD
北大核心
2017年第10期1127-1131,共5页
Chinese Journal of Analysis Laboratory
基金
国家自然科学基金(21175104)
陕西省教育厅基金(13JZ045)资助
关键词
固相萃取C4技术
气相色谱
蛋白胶料
可溶盐
SPE C4
Gas Chromatography
Proteinaceous binding medium
Soluble salts ions
