Sensitive high-performance liquid chromatographic determination of 2,2'-[(2-aminoethyl)imino]diethanol bis(butylcarbamate) and its metabolites in human serum following pre-column derivatization with o-phthalaldehyde and stabilization of the derivatives.
A high-performance liquid chromatographic method for the sensitive determination of 2,2'-[(2-aminoethyl)imino]diethanol bis(butylcarbamate) (I) and its metabolites in human serum has been developed. The method was based on a pre-column derivatization with o-phthalaldehyde. The derivatives were stabilized at least for 24 h at 4 degrees C by using N-acetyl-L-cysteine as a thiol and by eliminating the excess o-phthalaldehyde in the reaction mixture by solvent extraction and the addition of an ammonium salt after the reaction. The recoveries and reproducibilities in human serum spiked with I and its two metabolites were satisfactory, and the responses were linear over a wide range of analyte concentrations. The detection limits of I and its metabolites, II and III, in serum were 0.5, 4 and 2 ng/ml, respectively, at a signal-to-noise ratio of 5. The method was satisfactorily applied to the clinical study of I.
Okuda
T
T
Takeda Analytical Research Laboratories, Ltd., Osaka, Japan.
Aoki
I
I
Motohashi
M
M
Yashiki
T
T
D015097:3-Mercaptopropionic Acid; D000111:Acetylcysteine; D000889:Anti-Arrhythmia Agents / Q000097:blood*; D002219:Carbamates / Q000097:blood*; D002851:Chromatography, High Pressure Liquid; D005029:Ethylenediamines / Q000097:blood*; D006801:Humans; D007202:Indicators and Reagents; D009764:o-Phthalaldehyde
C080601:2,2'-((2-aminoethyl)imino)diethanol bis(butylcarbamate); D000889:Anti-Arrhythmia Agents; D002219:Carbamates; D005029:Ethylenediamines; D007202:Indicators and Reagents; D009764:o-Phthalaldehyde; D015097:3-Mercaptopropionic Acid; D000111:Acetylcysteine