摘要
目的建立人体血浆中雷莫拉宁的超高效液相色谱串联三重四级杆质谱(UHPLC-MS/MS)测定方法。方法血浆样品经甲醇沉淀蛋白后,4℃下静置30 min,离心,取上清液,氮吹至近干,再复溶于0.2%甲酸水溶液。以BEH-C18色谱柱,甲醇-0.2%甲酸水为流动相,采用梯度洗脱模式进行分离,运用ESI+模式进行质谱测试,外标法定量分析。结果在20~100μg/L范围内,雷莫拉宁的回归方程呈良好的线性关系,r=0.9970。方法的检出限为3μg/L,定量下限为10μg/L;加标回收率为76.6%~92.6%,RSD为3.0%~4.4%。结论该方法简便、快速、准确可靠,适用于人体血浆中雷莫拉宁的检测。
Objective To establish an analytical method for the determination of ramoplanin in human plasma by using ultrahigh performance liquid chromatography coupled with triple quadruple mass spectrometry(UHPLC-MS/MS).Methods The plasma sample was precipitated with methanol for 30 min at 4℃and then separated by high speed centrifugation.The supernatant was evaporated by nitrogen to dryness and re-dissolved in 0.2%formic acid solution.Separation of ramoplanin was achieved by a BEH-C18 column with mobile phases of methanol and 0.2%formic solution.Ramoplanin was detected by ultrahigh performance liquid chromatography tandem mass spectrometry under the gradient elution mode and ESI+mode and quantified by external standard method.Results Good linearity was obtained in the range of 20-100μg/L with the correlation coefficient of 0.9970 and the detection limit of 3μg/L and the quantification limit of 10μg/L.The spiked recoveries were in the range of 76.6%-92.6%with RSD values of 3.0%-4.4%.Conclusion The results demonstrated that the method is simple and reliable,and shows great promise for the determination of ramoplamin in plasma samples.
作者
谭磊
邓芬芳
卢祝靓子
李晓晶
罗晓燕
于鸿
潘心红
TAN Lei;DENG Fen-fang;LU Zhu-liang-zi;LI Xiao-jing;LUO Xiao-yan;YU Hong;PAN Xin-hong(Department of Physical and Chemical Analysis,Guangzhou Center for Disease Control and Prevention,Guangzhou,Guangdong 510440,China)
出处
《环境与健康杂志》
CAS
北大核心
2021年第3期259-261,共3页
Journal of Environment and Health
基金
广州市卫生健康科技项目(20201A011065)
广东省医学科研基金(A2019060)
关键词
雷莫拉宁
色谱法
超高效液相
串联质谱
人体血浆
Ramoplanin
Chromatography,ultra-high performance liquid
Tandem mass spectrometry
Human plasma