摘要
目的:建立 LC-MS/MS 法测定人血浆中地氯雷他定及其主要代谢产物3-羟基地氯雷他定的浓度。方法:血浆样品经碱化后用乙醚提取,采用液相色谱-质谱联用法检测。色谱条件为分析柱 CAPCELL PAK C_(18)(50 mm×2.0 mm,5 μm),预柱Octadecyl C_(18)(4.0 mm×3.0 mm);流动相:甲醇-乙腈-5 mmol·L^(-1)甲酸铵水溶液(30:20:50);流速0.2 mL·min^(-1);柱温40℃;进样量10 μL。质谱条件为电喷雾离子源(ESI),正离子扫描;选择性监测质荷比(m/z)为311.1/259.1(地氯雷他定),327.1/275.1(3-羟基地氯雷他定),315.1/263.1(D_4-地氯雷他定,内标),331.1/279.1(D_4-3-羟基地氯雷他定,内标)带正电荷的分子离子峰。结果:地氯雷他定、3-羟基地氯雷他定的线性范围均为0.05～10.0 ng·mL^(-1),定量下限均为0.05 ng·mL^(-1),批内、批间 RSD 均小于10%。结论:该方法简便,灵敏度高,专属性强,可用于地氯雷他定及其代谢产物的临床药动学和生物等效性研究。
Objective： To develop an LC - MS/MS method for determination of desloratadine and its metabolite 3 - hydroxy desloratadine in human plasma. Methods：Plasma samples were basified by NaOH and extracted by ether. The concentrations of desloratadine and its metabolite 3 -hydroxy desloratadine were determined by LC -MS/MS. LC ：Use CAPCELL PAK C 18 （50 mm × 2. 0 mm,5 μm） column with preliminary column Octadecyl C 18 （4. 0 mm × 3.0 m） , the mobile phase consisted of methanol - acetonitrile - 5 mmol · L^ - 1 ammonium formate （ 30： 20：50 ） , the flow rate was 0. 2 mL·min^- 1 ; column temperature was 40 ℃. MS ： Electrospray ionization source was applied and operated in positive ion mode. Selected ion mass （m/z） 311.1/259. 1 （desloratadine） ,327.1/275.1 （3 -hydroxy desloratadine） ,315. 1/263.1 （D4 -desloratadine ,internal standard） ,331.1/279. 1 （D4 -3 -hydroxy desloratadine, internal standard） were be monitored to quantify. Results：The linear calibration curve of desloratadine and 3 - hydroxy desloratadine were both obtained over the concentration range of 0. 05 - 10. 0 ng · mL^- 1, the lowest limit of quantitative were both 0. 05 ng · mL^-1 ;within -batch RSD and between -batch RSD were less than 10%. Conclusion：The method is proved to be simple, sensitive and specific. Therefore it can be used for clinical pharmacokinetic studies of desloratadine and its metabolite 3 -hydroxy desloratadine in human plasma.
出处
《药物分析杂志》
CAS
CSCD
北大核心
2007年第6期805-808,共4页
Chinese Journal of Pharmaceutical Analysis
