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气相色谱-质谱碎片分析法同时测定生物样品和天然产物中的泛酸和羟泛酸

Simultaneous determination of pantothenic acid and hopantenic acid in biological samples and natural products by gas chromatography-mass fragmentography.

作者信息

Banno K, Matsuoka M, Horimoto S, Kato J

机构信息

Analytical Chemistry Research Laboratory, Tanabe Seiyaku Co., Ltd., Osaka, Japan.

出版信息

J Chromatogr. 1990 Feb 23;525(2):255-64. doi: 10.1016/s0378-4347(00)83402-7.

Abstract

A method for the simultaneous determination of pantothenic acid and hopantenic acid in plasma samples was developed using gas chromatography-mass spectrometry with multiple ion detection. Plasma samples were directly purified without deproteinization on an ion-exchange resin, and the eluate was extracted with ethyl acetate under acidic conditions. The organic layer was evaporated to dryness under a stream of nitrogen, and the residue was dissolved in an internal standard solution. Pantothenic and hopantenic acids were converted into their trimethylsilyl derivatives by treating with bis(trimethylsilyl)trifluoroacetamide. Aliquots of this solution were injected into the gas chromatograph-mass spectrometer, which was equipped with a wide-bore fused-silica column (DB-17) and analysed by the multiple ion detection method. The detection limits for pantothenic acid and hopantenic acid in plasma were 1 ng/ml each at a signal-to-noise ratio of 5. This method was applied to a study of the assay of pantothenic acid and hopantenic acid in biological samples and natural products.

摘要

建立了一种采用气相色谱 - 质谱联用多离子检测法同时测定血浆样品中泛酸和羟基泛酸的方法。血浆样品直接在离子交换树脂上进行纯化,无需脱蛋白,洗脱液在酸性条件下用乙酸乙酯萃取。有机层在氮气流下蒸发至干,残渣溶于内标溶液。通过用双(三甲基硅基)三氟乙酰胺处理,将泛酸和羟基泛酸转化为它们的三甲基硅基衍生物。取该溶液的等分试样注入配备有宽口径熔融石英柱(DB - 17)的气相色谱 - 质谱仪中,并采用多离子检测法进行分析。在信噪比为5时,血浆中泛酸和羟基泛酸的检测限均为1 ng/ml。该方法应用于生物样品和天然产物中泛酸和羟基泛酸的测定研究。

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