摘要
目的采用液相色谱-串联质谱法（LC-MS/MS）定量分析大鼠血浆中复方鹿角颗粒14种主要成分（补骨脂素、异补骨脂素、马钱苷、淫羊藿苷、柚皮苷、橙皮苷、朝藿定A、朝藿定B、朝藿定C、宝藿苷Ⅰ、红景天苷、特女贞苷、淫羊藿次苷Ⅱ、女贞苷）,比较四种不同前处理方法的基质效应对其影响,并结合成分提取回收率选择适合的前处理方法。方法在大鼠空白血浆中加入低、中、高三种不同质量浓度的对照品溶液作为模拟血浆样品,瑞格列奈和地塞米松对照品分别为正、负离子内标。采用蛋白沉淀、液-液萃取、固相萃取和微固相萃取四种前处理方法,对最终测定的基质效应和提取回收率进行评价。结果采用微固相萃取法对大鼠血浆中复方鹿角颗粒14种主要成分高、中、低三种质量浓度的样品处理分析后,除橙皮苷、特女贞苷和中浓度女贞苷外,其余水平浓度样品的基质效应均在80%~120%范围间;除宝藿苷I和朝藿定A外,样品提取回收率均在70%以上。结论四种前处理方法中,采用微固相萃取法,样品基质效应对测定方法影响小,提取回收率高,操作简便、快速、灵敏度高、稳定性好,可以作为复方鹿角颗粒中14种主要成分在大鼠体内血药浓度测定和药代动力学研究的样品前处理方法。
Objective To investigate the influence of four different pretreatment methods on the matrix effect for determination of fourteen compounds（ psoralen,isopsoralen,loganin,icariin,naringin,hesperidin,epimedin C,baohuoside Ⅰ,epimedin A,epimedin B,salidroside,specnuezhenide,icarisidⅡ,nuezhenide） in compound Lujiao granules with matrix of rat plasma and recovery by liquid chromatography- tandem mass spectrometry（ LC- MS / MS）. Methods Adding three different concentration standard solutions into blank rat plasma as simulated sample,repaglinide and dexamethasone were used as internal standard in both positive and negative ionization modes. Investigation of matrix effect and recovery result through the method of protein precipitation（ PPT）,liquid- liquid extraction（ LLE）,solid- phase extraction（ SPE） and micro- solid- phase extraction（ Oasis HLB μ Elution）. Results The results showed that,after the sample at low,medium and high concentration were pretreatmented by Oasis μ Elution method. The matrix effects of compound Lujiao granules fourteen compounds in rat plasma were in the 80%-120% range except compounds of hesperidin,specnuezhenide and medium concentration of nuezhenide. The recoveries were higher than 70% except compounds of baohuosideⅠ and epimedin A. Conclusion Comparison of four pretreatment methods,the micro- solid phase extraction is better than others. As a simple,rapid,high sensitivity,good stability method,this pretreatment method suitable for the pharmacokinetic study of compound Lujiao granules in rat as the plasma sample pretreatment.
出处
《时珍国医国药》
CAS
CSCD
北大核心
2016年第4期1017-1021,共5页
Lishizhen Medicine and Materia Medica Research
基金
国家"十一五"重大新药创制专项(No.2010ZX09102-208)
国家临床重点专科(中医专业)临床药学建设项目(财社[2013]239号)
