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作 者:华雯妍[1] 张全英[1] 宗顺麟 黄明[1] 王蒙[1]
机构地区:[1]苏州大学附属第二医院临床试验机构,江苏苏州215004
出 处:《中国临床药理学杂志》2015年第24期2430-2432,共3页The Chinese Journal of Clinical Pharmacology
摘 要:目的建立测定人血浆中左舒必利的高效液相色谱-质谱联用(HPLC-MS/MS)方法。方法以硫必利为内标,血浆样品经甲醇沉淀蛋白提取分离,色谱柱为Xterra~RP18(4.6 mm×150 mm,5μm),流动相为乙腈-10 mmol·L^(-1)醋酸铵(含0.2%甲酸)水溶液(10:90),流速为1.0mL·min^(-1),柱温为30℃,选用电喷雾离子源(ESI)在正离子电离模式下,采用多反应监测(MRM)的质谱扫描方式。结果左舒必利标准曲线方程y=1.75×10^(-2)x+2.93×10^(-3)(n=3,r=0.999 3),线性范围1.00~600.00μg·L^(-1),定量下限为1.00μg·L^(-1),提取回收率在92.12%~98.53%,批内、批间RSD均小于4.61%。结论本方法专属性强,灵敏度高,操作简便、快速、准确,适用于血浆中左舒必利浓度的测定。Objective To establish an HPLC- MS/MS method for determination of levosulpiride in human plasma.Methods After protein precipitation,the plasma was separated on Xterra R P18(4.6 mm ×150 mm,5 μm) column,with a mobile phase of acetonitrile- 10 mmoL·L^-1 ammonium acetate containing 0.2%formic acid(10:90).The flow rate was 1.0 mL · min^-1 and the column temperature was 30℃.Quantification was performed in the positive ion multiple reaction monitoring(MRM) mode.Results Determination of levosulpiride had good linearity in the concentration range of 1.00- 600.00 μg·L^-1.The standard curve was y = 2.93 ×10^-3x+1.75×10^-2(n=3,r =0.999 3).The lower limit of quantization was 1.00 μg·L^-1,extraction recovery rate was 92.12%- 98.53%,and intra- batch and inter- batch RSD were both less than 4.61%.Conclusion The method is specific,simple,sensitive,rapid,accurate and suitable for determination of levosulpiride in human plasma.
关 键 词:左舒必利 高效液相色谱-质谱联用 药代动力学
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