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目的:建立测定大鼠全血4-二甲氨基苯酚(4-dimethylaminophenol,4-DMAP)的液相色谱/质谱联用法(LC-MS)。方法:全血样品经乙腈蛋白沉淀后,用丹磺酰氯衍生化,LC-MS法测定其血药浓度。以乙腈-0.1%甲酸水溶液(70/30,V/V)为流动相,用Venusil XBP-C18柱(50 mm×2.1 mm,5μm)分离,通过电喷雾电离源(ESI)选择性离子检测。检测离子为m/z:370.8(4-DMAP衍生物),m/z:373(内标衍生物)。对Wistar大鼠(n=5),于肌注4-DMAP(15 mg/kg)后进行了血药浓度测定。结果:4-DMAP在0.02~5μg/ml范围内呈良好线性关系(r=0.9987),批内和批间精密度RSD均小于10%。结论:本法操作简单、灵敏、准确,可用于4-DMAP的临床血药浓度测定和药代动力学研究。
Objective: To establish a liquid chromatography / mass spectrometry (LC-MS) method for the determination of 4-dimethylaminophenol (4-DMAP) in rat whole blood. Methods: Whole blood samples were precipitated with acetonitrile and derivatized with dansyl chloride. The plasma concentration of the sample was determined by LC-MS. Separation was performed on a Venusil XBP-C18 column (50 mm × 2.1 mm, 5 μm) using acetonitrile-0.1% formic acid in water (70/30, V / V) as mobile phase and selective ion detection by electrospray ionization (ESI). The detected ion was m / z: 370.8 (4-DMAP derivative), m / z: 373 (internal standard derivative). Blood plasma concentrations were determined in Wistar rats (n = 5) after intramuscular injection of 4-DMAP (15 mg / kg). Results: The linearity of 4-DMAP was in the range of 0.02-5 μg / ml (r = 0.9987). The intra-assay and inter-assay RSDs were less than 10%. Conclusion: This method is simple, sensitive and accurate and can be used for the determination of 4-DMAP in clinical plasma concentration and pharmacokinetics.