采用稳定同位素稀释质谱法同时测定人血浆中稳定同位素标记的L-组氨酸和尿刊酸。
Simultaneous determination of stable isotopically labelled L-histidine and urocanic acid in human plasma by stable isotope dilution mass spectrometry.
作者信息
Furuta T, Katayama M, Shibasaki H, Kasuya Y
机构信息
Department of Medicinal Chemistry and Clinical Pharmacy, Tokyo College of Pharmacy, Japan.
出版信息
J Chromatogr. 1992 May 8;576(2):213-9. doi: 10.1016/0378-4347(92)80195-v.
A capillary gas chromatographic-mass spectrometric method for the simultaneous determination of stable isotopically labelled L-histidine (L-[3,3-2H2,1',3'-15N2]histidine, L-His-[M + 4]) and urocanic acid ([3-2H,1',3'-15N2]urocanic acid, UA-[M + 3]) in human plasma was developed using DL-[2,3,3,5'-2H4,2'-13C,1',3'-15N2]histidine (DL-His-[M + 7]) and [2,3,5'-2H3,2'-13C,1',3'-15N2]urocanic acid (UA-[M + 6]) as internal standards. L-Histidine and urocanic acid were derivatized to alpha N-(trifluoroacetyl)-imN-(ethoxycarbonyl)-L-histidine n-butyl ester and imN-(ethoxycarbonyl)urocanic acid n-butyl ester. Quantification was carried out by selected ion monitoring of the molecular ions of the respective derivatives of L-His-[M + 4], DL-His-[M + 7], UA-[M + 3] and UA-[M + 6]. The sensitivity, specificity, precision and accuracy of the method were demonstrated to be satisfactory for measuring plasma concentrations of L-His-[M + 4] and UA-[M + 3] following administration of trace amounts of L-His-[M + 4] to humans.
建立了一种毛细管气相色谱 - 质谱法，用于同时测定人血浆中稳定同位素标记的L-组氨酸（L-[3,3-2H₂,1',3'-¹⁵N₂]组氨酸，L-His-[M + 4]）和尿刊酸（[3-²H,1',3'-¹⁵N₂]尿刊酸，UA-[M + 3]），使用DL-[2,3,3,5'-²H₄,2'-¹³C,1',3'-¹⁵N₂]组氨酸（DL-His-[M + 7]）和[2,3,5'-²H₃,2'-¹³C,1',3'-¹⁵N₂]尿刊酸（UA-[M + 6]）作为内标。L-组氨酸和尿刊酸被衍生化为α N-(三氟乙酰基)-imN-(乙氧羰基)-L-组氨酸正丁酯和imN-(乙氧羰基)尿刊酸正丁酯。通过对L-His-[M + 4]、DL-His-[M + 7]、UA-[M + 3]和UA-[M + 6]各自衍生物的分子离子进行选择离子监测来进行定量。该方法的灵敏度、特异性、精密度和准确度对于在向人体施用痕量L-His-[M + 4]后测量血浆中L-His-[M + 4]和UA-[M + 3]的浓度而言表现令人满意。
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