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本研究建立和验证了测定家兔血浆中舒尼替尼含量的液相色谱串联质谱法(LC-MS/MS)。含舒尼替尼的血浆样品经乙腈沉淀蛋白质后,用Zorbax Extended-C18色谱柱(150 mm×4.6 mm,5μm)分离,流动相为乙腈和0.05%甲酸水溶液(27:73,v/v),流速为0.8 mL/min,色谱柱柱温30 oC。液相流出液使用电喷雾离子源(ESI,正离子模式),质谱多反应监测模式检测,检测离子:舒尼替尼m/z 399.24→283.01;内标(盐酸地尔硫卓):m/z 415.19→178.00。舒尼替尼在2–600 ng/mL范围内,线性关系良好,最低定量限为2 ng/m L。该方法的专属性、准确度(相对误差范围为–5.0%~1.1%)、精密度(相对标准偏差范围为2.8%~9.5%)、基质效应以及提取回收率均符合要求。结果显示,该方法为检测家兔血浆中舒尼替尼的含量提供了一种可靠的手段。
In this study, LC-MS / MS was established and validated for the determination of sunitinib in rabbit plasma. Plasma samples containing sunitinib were precipitated with acetonitrile and separated on a Zorbax Extended-C18 column (150 mm × 4.6 mm, 5 μm) with acetonitrile and 0.05% formic acid (27:73, v / v) , The flow rate of 0.8 mL / min, the column temperature 30 oC. Iodine: Sunitinib m / z 399.24 → 283.01; internal standard (diltiazem hydrochloride): m / z 415.19 → 178.00. Sunitinib ranged from 2 to 600 ng / mL with good linearity with a minimum limit of quantitation of 2 ng / mL. The specificity, accuracy (relative error range -5.0% ~ 1.1%) and precision (relative standard deviation range 2.8% ~ 9.5%) of the method were satisfactory. Both matrix effect and extraction recovery were satisfactory. The results show that this method provides a reliable means of detecting sunitinib content in rabbit plasma.