Battezzati A, Fiorillo G, Spadafranca A, Bertoli S, Testolin G
Dipartimento di Scienze e Tecnologie Alimentari e Microbiologiche, International Center for the Assessment of Nutritional Status, Università degli Studi di Milano, 20133 Milan, Italy.
Anal Biochem. 2006 Jul 15;354(2):274-8. doi: 10.1016/j.ab.2006.05.009.
A simple, highly selective, and sensitive method using stable isotope dilution and gas chromatography-mass spectrometry has been developed to quantify salicylic acid (SA) at concentrations naturally occurring in biological fluids, such as in the serum of subjects not taking aspirin. After extraction of liquid-liquid with diethyl ether and ethyl acetate and preparation of the tert-butyldimethylsilyl derivative, SA content was detected using deuterated SA as internal standard. The mean recovery of SA from serum was 85 +/- 6%. Intra- and interday precision and % relative error were <15% in all cases. With a detection limit of 0.6 ng and a quantification limit of 2 ng, the method is therefore also adequate for population studies because of the small amount of blood necessary to perform the analyses.
已开发出一种使用稳定同位素稀释和气相色谱-质谱联用的简单、高选择性且灵敏的方法,用于定量生物流体中天然存在浓度的水杨酸(SA),例如未服用阿司匹林受试者的血清中的水杨酸。用乙醚和乙酸乙酯进行液-液萃取并制备叔丁基二甲基甲硅烷基衍生物后,以氘代SA作为内标检测SA含量。血清中SA的平均回收率为85±6%。在所有情况下,日内和日间精密度以及相对误差百分比均<15%。该方法的检测限为0.6 ng,定量限为2 ng,由于进行分析所需的血量少,因此也适用于人群研究。