QUANTITATIVE-ANALYSIS BY THIN-LAYER CHROMATOGRAPHY WITH SECONDARY ION MASS-SPECTROMETRY

被引:15
作者
BANNO, K [1 ]
MATSUOKA, M [1 ]
TAKAHASHI, R [1 ]
机构
[1] RITSUMEIKAN UNIV,DEPT CHEM,KITA KU,KYOTO 603,JAPAN
关键词
THIN-LAYER CHROMATOGRAPHY; SECONDARY ION MASS SPECTROMETRY; NICERGOLINE; SEMISYNTHETIC ALKALOID;
D O I
10.1007/BF02325023
中图分类号
Q5 [生物化学];
学科分类号
071010 ; 081704 ;
摘要
A direct combination of thin-layer chromatography with secondary ion mass spectrometry (TLC/SIMS) provides a method for the quantitative analysis of thermally unstable compounds or compounds of low volatility such as nicergoline. The method is very simple and has excellent precision. The analysis was performed by using an aluminum TLC plate and a mixture of methylene chloride, acetone, and distilled water as a developing solvent. After development the portion of the plate with the nicergoline and the internal standard spots was cut off the TLC plate, and was attached to the SIMS holder directly. The amount of nicergoline was determined from the ratio of the fragment ion intensity of the nicergoline to the internal standard. The calibration curve was linear, and the detection limit was 10 ng at a signal-to-noise ratio of 5. This method should be considered for application to the determination of drugs in biological samples and also for the determination of possible impurities and decomposition products in drugs.
引用
收藏
页码:179 / 181
页数:3
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