摘要
目的建立一种超临界流体色谱串联质谱法测定大鼠血浆中雷洛昔芬的质量浓度。方法采用沉淀蛋白法对血浆样品进行预处理;以大豆苷元作为内标,色谱柱为ACQUITY UPC2TM BEH柱(100 mm×3 mm,1.7μm),采用梯度洗脱方式,流动相:A为CO2(纯度体积分数≥99.99%),B为甲醇溶液(含8 mmol·L-1醋酸铵和体积分数为3%的水溶液);质谱:采用电喷雾离子源,正离子方式检测,多反应监测扫描。结果血浆中雷洛昔芬在2.00~2000μg·L-1内线性关系良好(r=0.9986),定量下限为2.00μg·L-1,日内、日间精密度(RSD)在3.8%~10.8%内,准确度(RE)在-0.3%~11.1%内,提取回收率在73.8%~78.3%内,基质效应在91.7%~99.3%内。结论该方法符合生物样品的测定要求,可用于大鼠血浆中雷洛昔芬质量浓度的测定,为探讨盐酸雷洛昔芬片及盐酸雷洛昔芬磷脂复合物在大鼠体内的药动学行为提供方法依据。
Objective To establish a method for the determination of raloxifene in rat plasma by supercritical fluid chromatography tandem mass spectrometry(SFC-MS/MS).Methods Plasma sample was pretreated by protein precipitation.Daidzein was used as the internal standard substance.Chromatographic analysis was performed on the ACQUITY UPC2 TM BEH column(100 mm×3 mm,1.7μm).Raloxifene and internal standard(daidzein)were eluted by a gradient of carbon dioxide(A,≥99.99%)and methanol(B,containing 8 mmol·L-1 ammonium acetate and 3%water)at a flow-rate of 1.0 mL·min-1.The mass spectrometer was operated in a positive ionization mode.The mass transitions of raloxifene and daidzein were m/z 474.5→112.2 and 254.8→137.0,respectively.Results The linear range was 2.00-2000μg·L-1 and the lower limit of quantitation was 2.00μg·L-1.The intra-day and inter-day precision ranged from 3.8%to 10.8%and the accuracy ranged from-0.3%to 11.1%.The extraction recoveries were between 73.8%and 78.3%.The matrix effect of reloxifene was in the range of 91.7%-99.3%.Conclusion The method can be applied to investigate the pharmacokinetics of raloxifene hydrochloride tablet and raloxifene hydrochloride phospholipid complex in rats.
作者
李慧新
卢思润
李鹏艳
罗美岭
刘建军
张天虹
LI Huixin;LU Sirun;LI Pengyan;LUO Meiling;LIU Jianjun;ZHANG Tianhong(Wuya College of Innovation,Shenyang Pharmaceutical University,Shenyang 110016,China)
出处
《沈阳药科大学学报》
CAS
CSCD
北大核心
2020年第7期611-617,共7页
Journal of Shenyang Pharmaceutical University
