固相萃取-超高效液相色谱串联质谱法测定城市污水中5种β-受体阻断剂  

Determination of 5 β-Adrenergic Receptor Blockers in Sewage by Solid Phase Extraction and Ultra Performance Liquid Chromatography/Tandem Mass Spectrometry

作　　者：柳晋杰[1,2] 张晶[2] 邵兵[2] 李青山[1] 

机构地区：[1]山西医科大学药学院,山西太原030001 [2]北京市疾病预防控制中心,北京100013

出　　处：《环境科学研究》2009年第7期862-867,共6页Research of Environmental Sciences

基　　金：国家自然科学基金项目(20807007,20837003)

摘　　要：β-受体阻断剂是一类常用的心血管疾病治疗药物.建立了城市污水中索他洛尔、普萘洛尔、卡维地洛、奈比洛尔和纳多洛尔5种β-受体阻断剂的超高效液相色谱-串联质谱联用检测方法.水样经MCX固相萃取小柱富集、净化,采用0.1%甲酸水溶液与乙腈为流动相进行梯度洗脱,经BEH C18色谱柱分离,通过多反应监测模式进行测定.该方法对5种β-受体阻断剂的线性范围为0.1-100.0μg/L,相关系数（R^2）均大于0.99.污水中索他洛尔、普萘洛尔、卡维地洛、奈比洛尔和纳多洛尔的定量限为0.2-2.0 ng/L,加标回收率为54.1%-113.4%,相对标准偏差小于22%,可用于城市污水中相关物质的分析测定.β-Adrenergic receptor blocker is an important kind of pharmaceutical mainly used in cardiovascular disease therapy. An ultra performance liquid chromatography/tandem mass spectrometry （UPLC-MS/MS） method was developed to analyze simultaneously 5 β-adrenergic receptor blockers （sotalol, propranolol, carvedilol, nebivolol and nadolol） in sewage. Target compounds in sewage samples were concentrated and purified by an Oasis MCX cartridge, and then separated on a BEH C18 column using a binary mobile phase gradient with water containing 0.1% formic acid and acetouitrile. As a result, a wen-shaped peak was obtained on the chromatogram of every analyte under the multireaction monitoring （MRM） mode. The assay for 5 β-adrenergic receptor blockers were linear over the range of 0.1-100.0 μg/L, with correlation coefficient（ R2） 〉 0.99. Limits of quantitation （LOQ） of target compounds in sewage sample ranged from 0.2 to 2.0 ng/L. Recoveries of the 5 β-adrenergic receptor blockers （spiked in sewage samples at three concentration levels） ranged from 54.1%-113.4 %, with relative standard deviations （RSD） less than 22 %. This method can be applied to the determination of target drugs in sewage samples.

关 键 词：超高效液相色谱-串联质谱(UPLC-MS/MS) Β-受体阻断剂 城市污水 固相萃取 

分 类 号：X701[环境科学与工程—环境工程]