Abbott F S, Burton R, Orr J, Wladichuk D, Ferguson S, Sun T H
J Chromatogr. 1982 Feb 12;227(2):433-44. doi: 10.1016/s0378-4347(00)80396-5.
A highly sensitive ion monitoring method for the determination of valproic acid in saliva and in serum has been developed based on the gas chromatographic--mass spectrometric analysis of the tert.-butyldimethylsilyl derivatives. Extraction methods are simple and the techniques for derivatization are rapid and convenient. Selected ion monitoring was carried out using electron ionization conditions and a common ion m/z 201 (M+--57) present in valproic acid and the internal standard octanoic acid. The lower limit of sensitivity that has acceptable precision for assay purposes is 0.1 mg/l based on a 200-microliter sample size. The ion monitoring method (derivatized) was compared to a gas chromatographic method (underivatized) for serum valproate assays and found to be essentially identical. The assay methodology was used in a kinetic study of valproic acid in two normal subjects. Saliva levels of drug were found to give reasonably good correlations with serum total and with serum free concentrations of drug in both individuals.U
基于叔丁基二甲基甲硅烷基衍生物的气相色谱 - 质谱分析，开发了一种用于测定唾液和血清中丙戊酸的高灵敏度离子监测方法。提取方法简单，衍生化技术快速便捷。使用电子电离条件和丙戊酸及内标辛酸中存在的常见离子m/z 201（M⁺ - 57）进行选择离子监测。基于200微升的样本量，用于分析目的且具有可接受精密度的灵敏度下限为0.1毫克/升。将离子监测方法（衍生化）与用于血清丙戊酸盐测定的气相色谱方法（未衍生化）进行比较，发现基本相同。该分析方法用于两名正常受试者的丙戊酸动力学研究。发现两名受试者的唾液药物水平与血清总药物浓度以及血清游离药物浓度均具有合理的良好相关性。
