The use of a new silylating agent for analysis of catecholamines by gas chromatography-mass spectrometry.

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3-Methoxytyramine, dopamine, norepinephrine, epinephrine and 6-hydroxydopamine were derivatized to their N-trifluoroacetyl-O-dimethyl-n-propylsilyl ether or 2'-O-methyl-N-trifluoroacetyl-O-dimethyl-n-propylsilyl ether derivatives by treatment with trifluoroacetic anhydride, methanol and then dimethyl-n-propylsilyl imidazole. These derivatives could be separated completely by gas chromatography (GC) on a non-polar liquid stationary phase such as OV-101. In addition, these derivatives were very stable in benzene and ethyl acetate, and showed excellent stability during silica gel column chromatography in comparison with the corresponding trimethylsilyl ether derivatives. In GC-mass spectrometry (MS) of these derivatives, ammonia chemical ionization (CI)-MS provided the ion [M+NH4]+ as the base peak or an intense peak. The detection limit of the dopamine derivative in the CI mode with ammonia was 2 pg with S/N at 2 : 1.

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