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目的建立Beagle犬血浆中25-OCH3-PPD浓度的LC-MS/MS测定方法。方法血浆样品用乙腈提取,采用选择性反应监测方法测定其血药浓度。检测仪器为Thermo TAQ型液相色谱-质谱联用仪,离子源为APCI源,用于定量分析的离子反应为:m/z 493.4→425.5(25-OCH3-PPD)和m/z 180.2→110.2(非那西丁);色谱柱为:Agilent C18柱(4.6×150 mm,5μm);流动相为:水-甲醇(5:95,V/V)。结果 25-OCH3-PPD的线性范围为5～1000 ng/mL,方法的绝对提取回收率为87.7%～98.0%,批内和批间的精密度均小于11.2%,血浆介质对25-OCH3-PPD低、中、高3个浓度水平的测定影响程度均小于15%。结论该方法经考察符合血浆样品的测定要求,可以应用于临床前Beagle犬血浆中25-OCH3-PPD的测定及其药代/毒代动力学研究。
Objective To establish a method for the determination of 25-OCH3-PPD in Beagle dog’s plasma by LC-MS / MS. Methods Plasma samples were extracted with acetonitrile and their plasma concentrations were determined by selective reaction monitoring. The detector was a Thermo TAQ liquid chromatography-mass spectrometer with the ion source as the APCI source and the ion reaction used for quantitative analysis was: m / z 493.4 → 425.5 (25-OCH3-PPD) and m / z 180.2 → 110.2 (Phenacetin). The column was Agilent C18 column (4.6 × 150 mm, 5μm). The mobile phase was water-methanol (5:95, V / V). Results The linear range of 25-OCH3-PPD was 5-1000 ng / mL. The absolute recovery of the method was 87.7% -98.0%. The precision of intra-assay and inter-assay was less than 11.2% PPD low, medium and high levels of the three concentration levels were less than 15%. Conclusions This method is suitable for the determination of 25-OCH3-PPD in the plasma of pre-clinical Beagle dogs and its pharmacokinetic / toxicokinetic studies after its investigation meets the requirements of the determination of plasma samples.