摘要
目的建立测定人血浆中双氯芬酸钠浓度的超高效液相色谱-串联质谱（LC-MS/MS）检测方法。方法采用蛋白沉淀法处理血浆样品。色谱柱为Waters C18（50 mm×2.1 mm,1.7μm）,流动相为乙腈-体积分数为0.06%的甲酸溶液（体积比为40∶60）,流速为0.7 m L·min-1,正离子模式多反应监测（MRM）扫描分析,离子通道分别为m/z 296.03→249.98（双氯芬酸钠）,m/z 358.10→138.92（吲哚美辛,内标物）。结果血浆中双氯芬酸钠线性为10~3 000μg·L-1（r=0.998 0）,定量下限为10μg·L-1,提取回收率在95.1%~101.3%,日内、日间精密度RSD均小于10%。结论该方法可用于双氯芬酸钠的药物动力学研究。
Objective To establish a UPLC-M S/M S method for the determination of diclofenac in human plasma.Methods The plasma procedure involved a single-step protein precipitation by acetonitrile,then a chromatography was proceeded on a Waters ACQUITY UPLC BEH C18column（50 mm × 2.1 mm,1.7 μm） using a mobile phase consisted of acetonitrile-0.06%（φ） formic acid（V ∶ V = 40∶ 60） at a flow rate of 0.7 m L·min-1.The protonated ions of analytes were detected in positive ionization in multiple reaction monitoring mode（M RM）.The mass transition pairs of m/z 296.03 →249.98 and 358.10 →138.92 were used to detect diclofenac and indomethacin.Results The calibration curve was linear over a concentration range of 10 to 3 000 μg·L-1（r = 0.998 0） and the low limit of quantitation was 10 μg·L-1.The extraction recovery rates were ranged from 95.1% to 101.3%,with-day RSD and between-day RSD were all less than 10%.Conclusions The method is simple and quick,with high specificity and sensitivity,and suitable for the research of diclofenac pharmacokinetics.
出处
《沈阳药科大学学报》
CAS
CSCD
北大核心
2014年第12期979-983,共5页
Journal of Shenyang Pharmaceutical University
