固相萃取-高效液相色谱/串联质谱法测定大鼠血浆中二十二碳六烯酸  

Determination of Docosahexenoic Acid in the Plasma of Rats by High Performance Liquid Chromatography-Tandem Mass Spectrometry Coupled with Solid-phase Extraction

作　　者：王丹[1] 万慧慧[1] 张华[1] 

机构地区：[1]精细化工国家重点实验室,大连理工大学,辽宁大连116024

出　　处：《分析科学学报》2015年第1期47-50,共4页Journal of Analytical Science

基　　金：大连理工大学引进人才科研专题(DUJ12RC(3)93)

摘　　要：建立了固相萃取-高效液相色谱／串联质谱（SPE—HPLC—MS／MS）测定大鼠血浆中二十二碳六烯酸（DHA）的分析方法。血浆样品经C18固相萃取（SPE）小柱净化后，采用ThermoC18色谱柱分离，以0．2％甲酸水溶液和乙腈为流动相，等度洗脱，在电喷雾离子源负离子模式下，采用质谱选择反应监测（SRM）模式检测，外标法定量。结果表明：DHA在0．10～60．0μg／mL范围内具有良好的线性关系（r2=0．9990）；检出限（S／N=3）为0．04μg／mL，定量限（S／N=10）为0．10μg／mL；在2、10、30μg／mL3个添加水平下，其平均回收率为94．0％～106．9％，方法的相对标准偏差（RSD）在2．15％～3．129／6之间。该方法简单、快速，准确度、灵敏度高，适用于大鼠血浆中DHA的分析检测。A simple and efficient method based on solid-phase extraction and high performance liquid chromatography-tandem mass spectrometry（SPE-HPLC-MS/MS）was developed and validated for the determination of docosahexenoic acid（DHA）in the plasma of rats. The plasma sample was purified by a C18 SPE column and separated by Thermo C18 chromatographic column, isocratic elution with 0. 20% formic acid aqueous solution and aeetonitrile as mobile phase. The detection of DHA was performed by HPLC-MS/MS with selective reaction monitoring（SRM）mode. The linear range for the determination of DHA was 0.10-60.0 μg/mL（r2 =0. 9990）. The limit of detection was 0.04 μg/mL （S/N=3） and the limit of quantification was 0.10 μg/mL（S/N= 10）. The average recoveries of DHA at three spiked levels of 2,10,30 μg/mL ranged from 94.0% to 106.9~/oo and the relative standard deviations（RSDs）were in the range of 2. 15%-3. 12%. The method is simple and quick with high accuracy and sensitivity. It is suitable for deteeting the content of DHA in the plasma of rats.

关 键 词：固相萃取 高效液相色谱-串联质谱 二十二碳六烯酸 大鼠血浆 

分 类 号：O657.63[理学—分析化学]