高效液相色谱-线性离子阱质谱法测定畜禽肌肉中β_2-受体激动剂及β-阻断剂类药物残留  

Determination of 23 β_2-agonists and 5 β-blockers in animal muscle by High Performance Liquid Chromatography-linear ion trap mass spectrometry

作　　者：吴永宁[1,2] 苗虹[1] 范赛[1,2] 赵云峰[1,2] 

机构地区：[1]中国疾病预防控制中心营养与食品安全所,北京100021 [2]中国农业大学动物医学院,北京100193

出　　处：《中国科学（B辑）》2009年第8期774-784,共11页Science in China(Series B)

基　　金：国家自然科学重点基金(批准号:20837003);"十一五"国家科技支撑计划(编号:2006BAK02A27;2006BAK01A02-5)项目资助

摘　　要：利用高效液相色谱-线性离子阱质谱(HPLC-ITMS)以同位素稀释技术测定了肌肉组织中23种β2-受体激动剂及5种β-阻断剂.肌肉样品经5%的三氯乙酸溶液酸解提取,以弱阳离子固相萃取柱进行净化.以甲醇和含0.1%甲酸的水溶液为流动相在液相色谱柱上梯度洗脱分离,采用ESI源正离子模式在选择离子监测(SRM)模式下进行扫描.以9种经氘代同位素标记的β2-受体激动剂为内标进行定量.猪肉中23种β2-受体激动剂及5种β-阻断剂的线性范围为5～200μg/L,相关系数(r)大于0.995,各化合物在肌肉中的检出限均能达到0.2μg/kg.以空白猪肉样品进行的加标水平为5、10、20μg/kg的加标回收试验,各化合物的回收率在47.3%～123.7%之间,相对标准偏差在3.2%～25.7%之间.对猪肉样品和鸡肉样品进行了测定,得到了满意的结果.该方法灵敏度高,定性准确,可以用于畜禽肌肉中β2-受体激动剂和β-阻断剂类药物残留的确证检测.A delicate method has been developed for the simultaneous determination of 23 β2-agonists and 5 β-blockers illegal drugs in muscle tissues by high performance liquid chromatography-linear ion trap mass spec- trometry using isotope dilution technique. The muscle samples are acid hydrolyzed and extracted with 5% tri- chloracetic acid in water, and then cleaned up using MCX solid phase extraction （SPE） cartridge. Methanol and 0.1% formic acid are used as mobile phases for gradient elution, a Waters Atlantis^T3 column is used for separation, and ESI positive ion scan mode is used with selective reaction monitor（SRM）. 9 β2-agonists labeled by the deuterium isotope were used as internal standards for quantification. The linear ranges of 23 β2-agonists and 5 β-blockers are 5-200 μg/L, the coefficient of correlation is not less than 0.995, and the limit of detection for each compound in the muscle tissue is below 0.2 μg/kg. The recoveries of each compound in the spiked samples at three levels 5, 10, 20 μg/kg are in the range of 47.3%-123.7%, and the relative standard deviations are in the range of 3.2%-25.7%. The developed method is sensitive and specific for the determination of β-agonists and β-blockers in pork and chicken muscle samples.

关 键 词：Β2-受体激动剂 Β-阻断剂 肌肉 检测 HPLC-ITMS 

分 类 号：TS207.5[轻工技术与工程—食品科学]