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目的:建立LC-MS测定人血浆中双氯芬酸浓度的方法。方法:待测血浆样品经乙酸乙酯萃取后,用HPLC-MS法进行检测,以格列吡嗪为内标。色谱柱为Agilent ZORBAX SB-C18(150 mm×4.6 mm,5μm),流动相为10 mmol.L-1醋酸铵溶液-甲醇(35∶65),流速为0.5 mL.min-1;质谱采用电喷雾离子化(ESI)方式和选择性离子检测(SIM)模式,检测离子为负离子。结果:本方法线性范围为3.936 0~492.000 0 ng.mL-1,最低定量浓度3.936 0 ng.mL-1,准确度、精密度以及稳定性均符合有关要求。结论:该方法简便、准确,灵敏度高,专属性强,适用于人血浆中双氯芬酸浓度的测定。
Objective: To establish a method for the determination of diclofenac in human plasma by LC-MS. Methods: Plasma samples were extracted with ethyl acetate and detected by HPLC-MS. Glipizide was used as internal standard. The column was Agilent ZORBAX SB-C18 (150 mm × 4.6 mm, 5 μm) and the mobile phase was 10 mmol·L-1 ammonium acetate-methanol (35:65) at a flow rate of 0.5 mL.min-1. Spray ionization (ESI) mode and selective ion detection (SIM) mode, the detection of ions is negative ions. Results: The linear range of this method was 3.936 0 ~ 492.000 0 ng.mL-1 with the lowest concentration of 3.936 0 ng.mL-1. The accuracy, precision and stability of the method met the relevant requirements. Conclusion: The method is simple, accurate, sensitive and specific. It is suitable for the determination of Diclofenac in human plasma.