METHOD FOR DETERMINATION OF ACETYLCHOLINE BY SLOW PYROLYSIS COMBINED WITH MASS FRAGMENTOGRAPHY ON A PACKED CAPILLARY COLUMN

被引:33
作者
POLAK, RL [1 ]
MOLENAAR, PC [1 ]
机构
[1] LEIDEN UNIV,MED CTR,DEPT PHARMACOL,SYLVIUS LABS,NL-2333 AL LEIDEN,NETHERLANDS
关键词
D O I
10.1111/j.1471-4159.1979.tb00364.x
中图分类号
Q5 [生物化学]; Q7 [分子生物学];
学科分类号
071010 ; 081704 ;
摘要
A new procedure is described for the estimation of ACh by pyrolysis‐gas chromatography/ mass spectrometry. ACh iodide and the iodides of ACh‐d16 or propionylcholine are slowly demethylated at 250°C by pyrolysis on the tip of a glass probe after insertion into the heated entrance of a glass tube leading to a packed capillary column. The volatile tertiary amines are then carried by helium to the column and trapped in its initial part which is kept at about 60°C. After 2–3 min the chromatography is started when the amines are released by heating this part to the ambient temperature in the oven (165°C). Peaks due to demethylated ACh and propionylcholine are well separated. The limit of detection is about 0.3pmol. After pyrolysis of mixtures of ACh and either ACh‐d16 or propionylcholine the peak amplitudes are linearly related to the doses. Copyright © 1979, Wiley Blackwell. All rights reserved
引用
收藏
页码:407 / 412
页数:6
相关论文
共 9 条
[1]   GAS CHROMATOGRAPHIC MICROESTIMATION OF ACETYLCHOLINE AND RELATED COMPOUNDS [J].
JENDEN, DJ ;
HANIN, I ;
LAMB, SI .
ANALYTICAL CHEMISTRY, 1968, 40 (01) :125-&
[2]   SIMULTANEOUS MEASUREMENT OF ENDOGENOUS AND DEUTERIUM-LABELED TRACER VARIANTS OF CHOLINE AND ACETYLCHOLINE IN SUBPICOMOLE QUANTITIES BY GAS CHROMATOGRAPHY MASS SPECTROMETRY [J].
JENDEN, DJ ;
ROCH, M ;
BOOTH, RA .
ANALYTICAL BIOCHEMISTRY, 1973, 55 (02) :438-448
[3]  
JENDEN DJ, 1970, DRUGS CHOLINERGIC ME, P7
[4]   IDENTIFICATION AND ESTIMATION OF CHOLINE DERIVAVITES BY MASS SPECTROMETRY [J].
JOHNSTON, GA ;
TRIFFETT, AC ;
WUNDERLICH, JA .
ANALYTICAL CHEMISTRY, 1968, 40 (12) :1837-+
[5]  
KOELLE GB, 1949, P SOC EXP BIOL MED, V70, P617
[6]   ANALYSIS OF ACETYLCHOLINE IN FROG MUSCLE BY MASS FRAGMENTOGRAPHY [J].
MILEDI, R ;
MOLENAAR, PC ;
POLAK, RL .
PROCEEDINGS OF THE ROYAL SOCIETY SERIES B-BIOLOGICAL SCIENCES, 1977, 197 (1128) :285-297
[7]  
POLAK RL, 1974, J NEUROCHEM, V23, P1295
[8]   MICROANALYTICAL DETERMINATION OF ACETYLCHOLINE OTHER CHOLINE ESTERS AND CHOLINE BY PYROLYSIS-GAS CHROMATOGRAPHY [J].
SZILAGYI, PI ;
SCHMIDT, DE ;
GREEN, JP .
ANALYTICAL CHEMISTRY, 1968, 40 (13) :2009-&
[9]   ACETYLCHOLINE, CHOLINE ACETYLTRANSFERASE AND CHOLINESTERASES IN MOTOR AND SENSORY NERVES OF BULL FROG [J].
WELSCH, F ;
SCHMIDT, DE ;
DETTBARN, WD .
BIOCHEMICAL PHARMACOLOGY, 1972, 21 (06) :847-&