摘要
目的建立HPLC-MS/MS方法测定人血浆中的羧甲司坦体内浓度,用于人体生物等效性分析。方法以直接沉淀法处理血浆,色谱柱为XTerra MS C18柱(150mm×2.1mm,5μm);流动相为甲醇-20mmol.L-1甲酸铵(含0.5%甲酸)(75∶25,v/v);流速为0.3mL.min-1;柱温为40℃。采用电喷雾离子源(ESI)负离子模式,用多反应监测模式(MRM)进行定量分析。结果羧甲司坦线性范围为0.210 9～54μg.mL-1,定量下限为0.210 9μg.mL-1,绝对回收率>80%,日内和日间RSD均<15%。结论此方法能够简便、高效、快速和灵敏的检测健康志愿者血浆中的羧甲司坦,可用于羧甲司坦药物代谢动力学及生物等效性研究。
Objective To establish a liquid chromatography-electrospray ionization tandem mass spectrum（HPLC-ESI-MS/MS） method to determine the carbocisteine in human plasma.Methods The XTerra MS C18（150 mm×2.1 mm,5 μm） column was used.The mobile phase was composed of 20 mmol·L-1 ammonium formate with 0.5% formic acid-methanol（25∶75,v/v）,the flow rate was 0.3 mL·min-1,and the column temperature was 40 ℃.The ionization was optimized with ESI（-） and selectivity was enhanced with tandem mass spectrometric analysis via MRM functions,m/z 178.0→90.9 for carbocisteine and m/z 122→78.0 for the internal standard.Results The calibration curve was linear at 0.210 9-54 μg·mL-1（r= 0.998）for arbocisteine.The absolute recovery was more than 80%.The inter-day and intra-day RSDs were all less than 15%.Conclusion The method is simple,rapid,efficient,sensitive and suitable for the content determination of carbocisteine in the plasma of healthy volunteers,which can be used in the pharmacokinetics and bioequivalence research of carbocisteine.
出处
《中南药学》
CAS
2012年第2期114-117,共4页
Central South Pharmacy
