液相色谱-三级质谱法分析尿液中β_2-受体激动剂及β-受体阻断剂多组分残留  

Determination of 12 β_2-Agonists and 4 β-Blockers in Urine by High Performance Liquid Chromatography-ion Trap Mass Spectrometry

作　　者：范赛[1,2] 邹建宏[3] 苗虹[2] 吴永宁[1,2] 赵云峰[1,2] 

机构地区：[1]中国农业大学动物医学院,北京100193 [2]中国疾病预防控制中心营养与食品安全所化学污染与健康安全重点实验室,北京100021 [3]中国人民解放军第二炮兵总医院心血管内科,北京100088

出　　处：《分析化学》2011年第8期1153-1158,共6页Chinese Journal of Analytical Chemistry

基　　金：国家自然科学基金重点基金(No.20837003);卫生部卫生科技专项(No.200902009);"十一五"科技支撑计划项目(No.2006BAK02A27)资助

摘　　要：建立了SPE柱净化结合液相色谱-三级质谱测定尿液中12种β2-受体激动剂和4种β-受体阻断剂的方法。尿液样品经冷冻离心,加入β-葡萄糖苷酸酶酶解后,以高氯酸沉淀蛋白,经HLB和MCX固相萃取柱净化。在Waters AtlantisT3色谱柱上以甲醇和含0.1%甲酸流动相进行梯度洗脱分离,采用ESI源正离子模式进行三级子离子监测,外标法定量。16种化合物的线性范围在0.005～0.160mg/kg之间,相关系数(r)大于0.995;各化合物检出限均低于0.2μg/kg。以0.005,0.01和0.02mg/L为添加水平的空白尿液的加标回收率在41.2%～88.2%之间;相对标准偏差在2.7%～19.2%之间。本方法准确可靠,灵敏度高,可用于尿液中β2-受体激动剂和β-受体阻断剂残留的定性与定量检测。A high performance liquid chromatography-ion trap mass spectrometric method combined with the technique of solid phase extraction had been developed for the determination of 12 β2-agonists and 4 β-blockers in urine samples.Urine samples were enzyme hydrolyzed by β-glucuronidase/arylsulfatase,then extracted and deproteinized by perchloric acid,and then cleaned up by Waters Oasis HLB and MCX solid phase extraction cartridges.The separation was performed on an AtlantisT3 chromatographic column with gradient elution using methanol and water containing 0.1% formic acid.ESI source performed under positive mode was used for the monitoring of the granddaughter ions.The linear ranges for 12 β2-agonists and 4 β-blockers were 0.005-0.160 mg/L,and the correlation coefficients were not less than 0.995.The detection limits of 12 β2-agonists and 4 β-blockers were less than 0.2 μg/kg.The pooled standard solution was added into blank urine samples at levels of 0.005,0.01 and 0.02 mg/L,and the recovery rates were ranged from 41.2% to 88.2% with the relative standard deviations of 12.7%-19.2%.The method is easy,fast,sensitive,and suitable for confirmation and quantification of 12 β2-agonists and 4 β-blockers in urine samples.

关 键 词：液相色谱-质谱法 Β2-受体激动剂 Β-受体阻断剂 尿液 固相萃取 

分 类 号：R927.2[医药卫生—药学]