Quantitative analysis by thin-layer chromatography with secondary ion mass spectrometry |
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Authors: | K Banno M Matsuoka R Takahashi |
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Institution: | (1) Analytical Chemistry Research Laboratory, Tanabe Seiyaku Co., Ltd., 16-89, Kashima 3-chome, 532 Yodogawa, Osaka, Japan;(2) Department of Chemistry, Ritsumeikan University, 56, Toujiinkita, Kita, 603 Kyoto, Japan |
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Abstract: | Summary 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 aluminium 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. |
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Keywords: | Thin-layer chromatography Secondary ion mass spectrometry Nicergoline Semisynthetic alkaloid |
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