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气相色谱-质谱联用法定量分析生物样品中1-羧基去甲骆驼蓬碱和去甲骆驼蓬碱

Identification and quantification of 1-carboxysalsolinol and salsolinol in biological samples by gas chromatography--mass spectrometry.

作者信息

Sjöquist B, Ljungquist C

出版信息

J Chromatogr. 1985 Sep 13;343(1):1-8. doi: 10.1016/s0378-4347(00)84562-4.

Abstract

1-Carboxysalsolinol was found to be present in rat striatum, human urine and caudate nucleus of post mortem human brain, according to capillary column gas chromatographic retention times and selected ion monitoring of the hexafluoropropionyl ester pentafluoropropyl derivative. Simultaneous quantification of 1-carboxysalsolinol and salsolinol was performed in biological samples using deuterium labelled internal standards. In human urine, the precision of the method was +/- 7.1% (coefficient of variation, n = 25) for 1-carboxysalsolinol at 15 pmol/ml and +/- 8.5% for salsolinol at 10 pmol/ml. According to enzymatic hydrolysis, 68% of 1-carboxysalsolinol was found as conjugates in urine, and the corresponding figure for salsolinol was 92%. In human caudate nucleus, the amounts of 1-carboxysalsolinol were found to be significantly greater in brains from alcoholics, who at autopsy had ethanol present in the blood, whereas alcoholics without blood ethanol levels at autopsy had significantly lower concentrations of salsolinol.

摘要

根据毛细管柱气相色谱保留时间以及对六氟丙酰酯五氟丙基衍生物的选择离子监测,发现1-羧基去甲猪毛菜酚存在于大鼠纹状体、人类尿液以及死后人类大脑的尾状核中。使用氘标记内标物对生物样品中的1-羧基去甲猪毛菜酚和去甲猪毛菜酚进行了同时定量分析。在人类尿液中,该方法对于浓度为15皮摩尔/毫升的1-羧基去甲猪毛菜酚的精密度为±7.1%(变异系数,n = 25),对于浓度为10皮摩尔/毫升的去甲猪毛菜酚的精密度为±8.5%。根据酶促水解分析,发现尿液中68%的1-羧基去甲猪毛菜酚以缀合物形式存在,而去甲猪毛菜酚的相应比例为92%。在人类尾状核中,发现死于酒精中毒且尸检时血液中存在乙醇的个体大脑中的1-羧基去甲猪毛菜酚含量显著更高,而尸检时血液中无乙醇的酒精中毒者的去甲猪毛菜酚浓度则显著更低。

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