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[摘要]
目的:建立测定人血浆中人参三醇二琥珀酸酯钠的液相色谱-质谱联用法。方法:色谱柱为Shimadzu VP-C18柱(150 mm×2.0 mm,5 μm); 乙腈-10 mmol/L乙酸铵水溶液(55∶45)为流动相,体积流量0.3 mL/min;柱温40 ℃;内标物吲达帕胺。质谱条件为电喷雾离子源(ESI),选择负离子提取方式检测,人参三醇二琥珀酸酯钠和吲达帕胺的选择检测离子分别为m/z 675.5([M-Na+H] +)、m/z 364.1([M+H] + )。结果:人参三醇二琥珀酸酯钠线性范围为0.030 4~101.3 μg/mL,定量下限为0.030 4 μg/mL。准确度、精密度以及稳定性均符合有关要求。结论:本方法专属性强,灵敏度高,适用于人血浆中人参三醇二琥珀酸酯钠的药代动力学研究。
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[Abstract]
Objective: To develop a sensitive and specific LC-MS method for the determination of sodium panaxatriol disuccinate in human plasma. Methods: Separation was carried out on a Shimadzu VP-ODS analytical column (150 mm × 2.0 mm, 5 μm) with a mobile phase of CH3CN-10 mmol/L ammonium acetate (55:45) at a flow rate of 0.3 mL/min. The internal standard was Indapamide. ESI was applied and operated in negative mode. The ion of monitor: m/z 675.5 (sodium panaxatriol disuccinate), m/z 364.1 (Indapamide). Results: The linear calibration curve was observed in the concentration range of 0.030 4 - 101.3 μg/mL. The lower limit quantification was 0.030 4 μg/mL. The accuracy, precision (intra-day and inter-day), sensitivity and stability (ambient temperature, freeze/thaw, freeze storage) of the method fulfilled the guideline of the analytical validation criteria. Conclusion: The method with specificity is sensitive, rapid and suitable for pharmacokinetics study on sodium panaxatriol disuccinate in human plasma.
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