CI Mass spectrometric analysis of physiologically active compoun

Details CI Mass spectrometric analysis of physiologically active compoun CI Mass spectrometric analysis of physiologically active compoun

1977-11-15

1980-09-23

Turk, Arnold

Chemistry: physical processes

Physical processes

Crystallization

G01N 3316

Patent

active

042240310

ABSTRACT:
A method for determining an analyte is provided, wherein a sample is prepared in a form useful for chemical inonization mass spectrometry and analyzed. Included in the sample is an analog of the compound which differs in having an unnatural isotopic distribution. The combined analyte and analog are derivatized as appropriate and then subjected to chemical protonation in the gaseous phase to provide charged species. The resulting charged species are then analyzed mass spectrometrically and the amount of analyte is determined by determining the ratio of one or more of the major peaks of the analyte and its analog.
The method finds particular use in the determination of physiologically active compounds as found in physiological fluids, particularly blood. With blood, the analyte is extracted with an appropriate extraction solvent freed of protein, combined with its isotopically different analog, and the mixture then derivatized, if necessary. The analyte and analog or derivatives thereof are then subjected to chemical protonation in the vapor phase and the resulting charged species analyzed by mass spectrometry. By comparing the ratio of one or more major peaks of the analyte and analog, the amount of analyte may be determined.

REFERENCES:
Mee et al.-I, Analytical Letters, 9(12), 1075-1083 (1976).
Mee et al.-II, Analytical Letters, 9(6), 605-610 (1976.
Mee et al.-III, Biomed. Mass Spectrometry, 4:178 (1977).
Milne et al., Anal. Chem. 43, 1815 (1971).
Lundeen et al., Anal. Chem. 45, 1288 (1973).
Milne et al., Anal. Chem. 45, 1952 (1973).
Chas et al., Anal. Chem. 46, 296 (1974).

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