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机构地区:[1]上海交通大学附属第六人民医院药剂科,上海市200233
出 处:《中国药房》2011年第34期3198-3200,共3页China Pharmacy
摘 要:目的:建立快速、灵敏的方法同时测定人血浆中对称性二甲基精氨酸(SDMA)和非对称性二甲基精氨酸(ADMA)的浓度。方法:血浆样品经乙腈沉淀蛋白后,以高效液相色谱串联质谱电喷雾法进行测定,色谱柱为Thermo Hypercarb,流动相为乙腈∶甲酸铵-甲酸缓冲溶液(梯度洗脱),流速为0.40mL·min-1。采用电喷雾离子源(ESI源),以选择多反应监测(MRM)方式进行正离子检测,监测离子对分别是m/z203.1→172.1(SDMA)、m/z203.1→46.1(ADMA)和m/z272.2→171(右美沙芬)。结果:血浆中SDMA和ADMA的线性范围均为25~500ng·mL-1,定量下限均为25ng·mL-1。平均方法回收率均>97%,日内、日间RSD均<17%。结论:该方法专属性好,灵敏度高,准确快捷,适用于生物样品的快速检测。OBJECTIVE:To develop a sensitive and rapid method for simultaneous determination of symmetric dimethylarginine (SDMA) and asymmetric dimethylarginine (ADMA) in human plasma. METHODS: Plasma samples were extracted by protein precipitation with acetonitrile. LC-MS/MS was adopted. The determination were separated on Thermo Hypercarb column with mobile phase consisted of acetonitrile:arnmonium formate-formic acid at a flow rate of 0.40 mL-min^-1(gradient elution). A tandem mass spectrometer equipped with electrospray ionization source (ESI) was used as detector and operated in the positive ion mode. Multiple Reaction Monitoring (MRM) using the precursor/production combinations of m/z 203.1→172.1, m/z 203.1→46.1 and rrdz 272.2→171 were used to quantify SDMA, ADMA and dextromethorphan, respectively. RESULTS:The linear ranges were 25-500 ng· mL^-1 for SDMA and ADMA uniformly. The lowest limits of quantitation of two compounds were 25 ng·mL^-1. Average method recovery rate was more than 97% and RSDs of intra-day and inter-day were lower than 17%. CONCLUSION: The method is proved to be specific, sensitive, accurate and rapid. It is suitable for rapid determination of biological samples.
关 键 词:对称性二甲基精氨酸 非对称性二甲基精氨酸 高效液相色谱串联质谱电喷雾法 血药浓度 药动学
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