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高效液相色谱法同时测定5-氨基水杨酸和5-乙酰氨基水杨酸

Simultaneous determination of 5-aminosalicylic acid and 5-acetylaminosalicylic acid by high-performance liquid chromatography.

作者信息

Brendel E, Meineke I, Witsch D, Zschunke M

出版信息

J Chromatogr. 1987 Jan 9;385:299-304. doi: 10.1016/s0021-9673(01)94644-8.

DOI:10.1016/s0021-9673(01)94644-8
PMID:3558586
Abstract

A high-performance liquid chromatographic method has been developed for the simultaneous determination of 5-aminosalicylic acid (5-ASA) and its main metabolite 5-acetylaminosalicylic acid (5-AcASA) in plasma, with 4-acetylaminosalicylic acid as an internal standard. Prior to extraction into ethyl acetate, 5-ASA is derivatized to 5-carbobenzyloxyaminosalicylic acid (5-CboASA). The calibration graphs for both 5-ASA and 5-CboASA are linear between 0.1 and 20.0 mumol/l. The limit of detection is 0.02 mumol/l for 5-ASA and 0.05 mumol/l for 5-AcASA. At 0.1 mumol/l, the coefficients of variation were 8.1 and 9.8% for 5-ASA and 5-AcASA, respectively. At 1.0 and 10.0 mumol/l, the coefficients of variation were 4.1% or less. The mean bias ranged from -6.2 to -2.0% for 5-ASA and from +6.0 to 0% for 5-AcASA.

摘要

已开发出一种高效液相色谱法,以4-乙酰氨基水杨酸为内标,同时测定血浆中的5-氨基水杨酸(5-ASA)及其主要代谢物5-乙酰氨基水杨酸(5-AcASA)。在萃取到乙酸乙酯之前,将5-ASA衍生化为5-苄氧羰基氨基水杨酸(5-CboASA)。5-ASA和5-CboASA的校准曲线在0.1至20.0μmol/L之间呈线性。5-ASA的检测限为0.02μmol/L,5-AcASA的检测限为0.05μmol/L。在0.1μmol/L时,5-ASA和5-AcASA的变异系数分别为8.1%和9.8%。在1.0和10.0μmol/L时,变异系数为4.1%或更低。5-ASA的平均偏差范围为-6.2%至-2.0%,5-AcASA的平均偏差范围为+6.0%至0%。

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