摘要
建立LC-MS检测大鼠血清中白桦脂酸浓度的方法。取内标物齐墩果酸,加100μL血清,乙酸乙酯萃取,取上清液以氮气吹干,乙腈复溶,进样1μL,在电喷雾离子源下进行负离子检测(SIM)分析。色谱柱为BEHC18柱(2.1mm×50mm,1.7μm),流动相为乙腈-0.1%甲酸水溶液(62:38)。白桦脂酸和内标物的质荷比(m/z)均为455.4。白桦脂酸在3.328~832ng·mL^-1内线性良好,检出限为3.328ng·mL^-1,提取回收率均大于80%.日内、日间精密度RSD值均小于10%,日内、日间准确度为92%~96%,本法成功检测了白桦脂酸在大鼠体内的血药浓度。且本方法稳定、灵敏度较好,适用于白桦脂酸在大鼠体内血药浓度测定。
The HPLC-MS was developed for the determination of Betulinic acid in Rat Serum. Serum samples(100 μL) were mixed with ethyl acetate followed by extraction. The supernatant was dried under N2 and re-dissolved by acetonitrile,1 μL of which was injected onto LC-MS. The analysis was carried out under the negative mode of electronic-spray ionization(SIM). Chromatographic column was BEH C18(50 mm×2.1 mm×1.7 μm). The mobile phase was acetonitrile-0.1% formic acid in water(62∶38). The mass-to-charge ratio(m/z) of betulinic acid and internal standard were 455.4. The linear range of betulinic acid was within the concentration of 3.328-832 ng·mL^-1. The LOD was 3.328 ng·mL^-1. The extraction recoveries were all higher than 80%. The intra-and inter-dayprecisions(RSD) were less than 10%. The intra-and inter-day accuracy was 92%-96%. The betulinic acid concentration in rat serum was detected successfully. The method was stable. It was suitable for determining the betulinic acid concentration in rat serum.
作者
任娟
孙兴
詹雁
谭镭
阮佳
徐超群
REN Juan;SUN Xing;ZHAN Yan;TAN Lei;RUAN Jia;XU Chaoqun(Chengdu University of TCM,Chengdu 610075,Sichuan,China;Sichuan Provincial Academy of TCM,Chengdu 610041,Sichuan,China)
出处
《中华中医药学刊》
CAS
北大核心
2018年第12期2950-2953,共4页
Chinese Archives of Traditional Chinese Medicine
基金
国家重大新药创制项目(2017ZX09301-055)
四川省科研院所科技成果转化资金项目(1501110)
四川省科技支撑计划项目(15ZC1978)
四川省公益性科研院所基本科研业务专项项目
关键词
LC-MS
白桦脂酸
含量测定
内标法
LC -MS
betulinic acid
content determination
internal standard method
