超高效液相色谱-线性离子阱同时检测动物源性样品中7种β_2-受体激动剂

Simultaneously determination of seven β_2-receptor agonists by UHPLC-QTrap in animal derived sample

目的建立测定动物源性样品中马布特罗、塞曼特罗、莱克多巴胺、克伦特罗、沙丁胺醇、特布他林、苯氧丙酚胺等7种β2-受体激动剂残留量的超高效液相色谱-串联质谱（UHPLC-MS/MS）的分析方法和阳性样品确证方法。方法动物源性样品经乙酸铵缓冲溶液酶解提取,用阳离子交换柱净化,以流动相A：1 mmol/L乙酸铵-0.1%甲酸水、流动相B：1 mmol/L乙酸铵-0.1%甲酸乙腈水（90∶10,V/V）,经Agilent C18色谱柱（2.1 mm×50 mm,1.8μm）分离,阳性样品通过QTrap四级杆质谱仪的增强型子离子扫描模式作进一步确证。本研究同时考察了7种β2-受体激动剂的基质效应。结果动物源性样品中β2-受体激动剂残留量的检测存在较强的基质效应。7种β2-受体激动剂在0.25~50 ng/g浓度范围内,呈良好线性,线性相关系数r〉0.99,加标回收率为86.6%~108.7%,方法检出限为0.1~0.5 ng/g。结论该方法采用了内标法定量以减小基质效应带来的定量误差,检出限较低、定量准确、仪器分析时间短,可用于检测动物源性样品样中β2-受体激动剂的残留量,同时对阳性样品作进一步确证。

Objective To establish an ultra high performance liquid chromatography tandem mass spectrometry（ UHPLCMS / MS） analytical methods and confirmatory method for positive samples to determine seven β2-receptor agonists including mabuterol,cimaterol,ractompamine,clenbuterol,salbutamol,terbutaline and isoxsuprine in animal derived samples.Methods The animal derived samples were enzymatic hydrolyzed and extracted with ammonium acetate buffer solution. The supernatant was treated by cation exchange column solid phase extraction（ SPE）,followed by nitrogen concentrating and analyzed by UHPLC-MS / MS. The suspicious positive sample was further confirmed by specific scanning mode of QTrap tandem mass spectrometry. This study also investigated the matrix effects of seven β2-receptor agonists. Results The results showed that there was a strong matrix effects of the method. The correlation coefficients were good in the concentration range of 0. 25-50 ng / g. The limit of detection was 0. 1-0. 5 ng / g. The average recovery for β2-receptor agonists was in the range of86. 6%-108. 7%. Conclusion The internal standard quantitative method could be used to reduce the quantitative error from the matrix effect. This method could be used for determination of β2-receptor agonists in animal derived samples with a low detection limit,good accuracy and fast. The positive samples could be further confirmed.