LC-MS/MS法测定Beagle犬血浆中人参果抗肿瘤活性成分25-OCH_3-PPD  

Determination of 25-OCH_3-PPD in Beagle Dog Plasma by LC-MS/MS Method

作　　者：高海燕[1] 辛艳飞[1] 李巍[2] 顾利强[1] 余健[1] 宣尧仙[1] 赵余庆[2] 

机构地区：[1]浙江省医学科学院安全性评价研究中心,杭州310013 [2]沈阳药科大学中药学院,沈阳110016

出　　处：《中药新药与临床药理》2012年第3期312-315,共4页Traditional Chinese Drug Research and Clinical Pharmacology

基　　金：国家"十一五"科技重大专项(20092X09102-114);国家"十二五"科技重大专项(2011ZX09301-003);浙江省科技计划项目(2010F10026)

摘　　要：目的建立Beagle犬血浆中25-OCH3-PPD浓度的LC-MS/MS测定方法。方法血浆样品用乙腈提取,采用选择性反应监测方法测定其血药浓度。检测仪器为Thermo TAQ型液相色谱-质谱联用仪,离子源为APCI源,用于定量分析的离子反应为:m/z 493.4→425.5(25-OCH3-PPD)和m/z 180.2→110.2(非那西丁);色谱柱为:Agilent C18柱(4.6×150 mm,5μm);流动相为:水-甲醇(5:95,V/V)。结果 25-OCH3-PPD的线性范围为5～1000 ng/mL,方法的绝对提取回收率为87.7%～98.0%,批内和批间的精密度均小于11.2%,血浆介质对25-OCH3-PPD低、中、高3个浓度水平的测定影响程度均小于15%。结论该方法经考察符合血浆样品的测定要求,可以应用于临床前Beagle犬血浆中25-OCH3-PPD的测定及其药代/毒代动力学研究。Objective To develop an LC-MS/MS method for the determination of 25-OCH3-PPD concentration, an extract from Herba Herminii Monorchidis, in Beagle dog plasma. Methods The plasma samples were extracted with 500 μL acetonitrile, and the blood drug level was examined with selective reaction method. The detection was per- formed on a triple quadrupole Thermo TAQ tandem mass spectrometer equipped with ion atomospheric pressure chemi- cal ionization source operating in positive ion selected reaction monitoring mode. The conditions for ionic reaction were as follows ： m/z 493.4→425.5 （25-OCH3-PPD） and m/z 180.2→110.2（phenacetin）. An Agilent Cls column （4.6 mm×150 nm, 5 μm） was used, the mobile phase consisted of water： methonal（5 ： 95, V/V） , and the flow rate was 1 mL/min. Results The method was linear in the concentration range of 5-1000 ng/mL. The recovery rate was 87.7 %-98.0 %, the deviations of both intra- and inter-precision（RSD） were less than 11.2 %. The influence of plasm medium in the determination of low-, moderate- and high-concentration 25-OCH3-PPD was less than 15 %. Conclusion This method has been proved to be effective for the determination of 25-OCH3-PPD concentration in Beagle dog plasma and for the research of its pharmacokinetics and toxicity.

关 键 词：25-OCH3-PPD LC-MS/MS法 血药浓度 

分 类 号：R284.1[医药卫生—中药学]