高效液相色谱串联质谱法测定人血浆中缬沙坦的浓度  

A liquid chromatography/tandem mass spectrometry method for the quantification of valsartan in human plasma

作　　者：王启平[1] 陈省[1] 李贞[2] 

机构地区：[1]深圳市宝安区沙井人民医院,广州医学院附属深圳沙井医院,广东深圳518104 [2]北京大学人民医院,北京100044

出　　处：《中国医院药学杂志》2010年第20期1759-1761,共3页Chinese Journal of Hospital Pharmacy

摘　　要：目的:建立一种快速、灵敏地测定人血浆中缬沙坦浓度的高效液相色谱串联质谱法(HPLC-MS/MS)。方法:血浆样品经乙腈沉淀后,以甲醇-乙腈-10mmol.L-1醋酸胺(pH4.0,20:30:50)为流动相,采用Lichrospher C18柱(150mm×2.1mm,5μm,汉邦科技有限公司),通过电喷雾离子化离子阱时间串联质谱,以选择多重反应监测(MRM)方式进行检测。用于定量分析的二级碎片离子分别为m/z418(缬沙坦)和m/z423(内标坎地沙坦)。结果:线性范围为4～4000μg.L-1,最低定量浓度为4μg.L-1,日内RSD为1.9%～4.2%,日间RSD为5.6%～5.9%,每个样品测试时间仅3min。结论:该法灵敏度高,操作简便、快速、准确,适用于临床药动学研究。OBJECTIVE To establish a rapid and sensitive liquid chromatography / tandem mass spectrometry （LC/MS/ MS） method for quantification of valsartan in human plasma. METHODS After a simple protein precipitation using acetoni trile, the analytes were separated on a Lichrospher C18 （ 150 mm× 2. 1 mm, 5 μm） column using methanol： acetonitrile： 10 mmol·L^-1 ammonium acetate （pH 4. 0,20：30：50, v/v/v） as mobile phase at a flow rate of 0. 3 mL·min^-1. Valsartan and candesartan were eluted at 2. 65 min and 2.3 min, respectively, ionized using ESI source, and then detected by multiple reaction monitoring （MRM） mode. The precursor to product ion transitions of m/z 436 418 and m/z 441-423 were used to quantify valsartan and candesartan, respectively. RESULTS The method was linear in the concentration range of 4-4 000 μg·L^-1 for valsartan. The limit of quantification was 4 μg·L^-1 . The intra-day and inter-day RSD were 1.9%-4. 2% and 5. 6%-5.9%. Each plasma sample was chromatographed within 3 min. CONCLUSION The method was proved to be suitable for clinical investigation of valsartan pharmacokinetics, which offers advantages of specificity, speed, and greater sensitivity over the previously reported methods.

关 键 词：缬沙坦 高效液相色谱串联质谱法 血浆 

分 类 号：R969[医药卫生—药理学]