摘要
目的:建立测定皮下注射草乌甲素的小鼠血浆中草乌甲素浓度的液相色谱-质谱-质谱联用方法。方法:50μL小鼠血浆样品加入内标物左吡坦和pH9.2磷酸缓冲液,经乙醚提取后,以甲醇:缓冲液(85∶15)为流动相(缓冲液为20mmol/L乙酸胺和0.1%甲酸的水溶液),流速300μL/min,采用C18柱分离,经电喷雾化的四极杆串联质谱,以多离子反应监测方式进行检测。结果:线性范围为0.1~1000ng/mL,回收率大于80%。结论:该方法取样量小,专属性强,操作简便,可用于血浆中草乌甲素浓度的测定。
AIM: To develop the method for analyzing bulleyacinitine A in plasm from mice through the treatment of subcutaneous injection of bulleyacinitine A by liquid chromatography tandem mass spectrometry ( LC-MS/ MS). METHODS: 50 μL mouse plasma sample added zolpidem as internal standard and pH 9.2 buffer solution was extracted with ethylether, followed by liquid chromatography and mass spectrometric detection. The mobile phase was consisted of methanol-buffer solution (85:15 )( buffer solution consisted of 20 mmol/L ammonium acetate and 0. 1% formic solution). The flow rate was 300μL per minute. The separation column was C18 column. The electrospray ionization tandem mass spectrometry and the multiple reaction monitoring mode were applied to detecting the bulleyacinitine A in plasma. RESULTS: The assay was linear from 0.1 to 1 000 ng/mL. The recovery rate was more than 80%. CONCLUSION: The method could be used to detect bulleyacinitine A level in mouse plasma, which offers advantages of sensitiveness, specificity and simpleness.
出处
《中成药》
CAS
CSCD
北大核心
2008年第10期1499-1502,共4页
Chinese Traditional Patent Medicine
关键词
草乌甲素
血浆
液相色谱-质谱-质谱
bulleyacinitine A
liquid chromatography tandem mass spectrometry, plasma
mouse