TY - JOUR
T1 - Determination and quantification of clonidine in human blood serum
AU - Wenzl, Thomas
AU - Lankmayr, Ernst
AU - Wintersteiger, Reinhold
AU - Sadjak, Anton
AU - Likar, Rudolf
AU - Zakel, Dieter
PY - 2002
Y1 - 2002
N2 - Clonidine ((2-[2,6-dichlorophenyl]amino)-2-imidazoline) preferentially stimulates central alpha(2)-adrenoceptors, which leads to inhibition of sympathetic tone, resulting in a lowering of arterial pressure and of heart rate. Additionally, many other desirable and undesirable effects are described, including analgesia, sedation and withdrawal reactions, which consist of a sudden rise in arterial pressure, nervousness, agitation and increased heart rate. The present study has the goal to develop a simple and effective method for the analysis of trace amounts of clonidine in human blood serum. Special emphasis is necessary to make application of electron impact ionization and separation of the analyte fragments in a quadruple mass analyzer suitable. The procedure comprises solid phase extraction followed by formation of the pentafluorobenzyl derivative. Further purification is achieved by phase transfer extraction into an acidic aqueous solution succeeded by re-extraction into dichloromethane. After solvent exchange, an aliquot is injected into the gas chromatograph equipped with a DB5 MS capillary column and a mass spectrometric detector. Chromatograms are recorded in single ion monitoring mode. Quantification is accomplished by internal standardization with moxonidine [4-chloro-5-(2-imidazolin-2-yl-amino)-6-methoxy-2-methylpyridine].
AB - Clonidine ((2-[2,6-dichlorophenyl]amino)-2-imidazoline) preferentially stimulates central alpha(2)-adrenoceptors, which leads to inhibition of sympathetic tone, resulting in a lowering of arterial pressure and of heart rate. Additionally, many other desirable and undesirable effects are described, including analgesia, sedation and withdrawal reactions, which consist of a sudden rise in arterial pressure, nervousness, agitation and increased heart rate. The present study has the goal to develop a simple and effective method for the analysis of trace amounts of clonidine in human blood serum. Special emphasis is necessary to make application of electron impact ionization and separation of the analyte fragments in a quadruple mass analyzer suitable. The procedure comprises solid phase extraction followed by formation of the pentafluorobenzyl derivative. Further purification is achieved by phase transfer extraction into an acidic aqueous solution succeeded by re-extraction into dichloromethane. After solvent exchange, an aliquot is injected into the gas chromatograph equipped with a DB5 MS capillary column and a mass spectrometric detector. Chromatograms are recorded in single ion monitoring mode. Quantification is accomplished by internal standardization with moxonidine [4-chloro-5-(2-imidazolin-2-yl-amino)-6-methoxy-2-methylpyridine].
U2 - 10.1016/S0165-022X(02)00101-X
DO - 10.1016/S0165-022X(02)00101-X
M3 - Article
SN - 1872-857X
VL - 53
SP - 131
EP - 139
JO - Journal of Biochemical and Biophysical Methods
JF - Journal of Biochemical and Biophysical Methods
IS - 1-3
ER -