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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 a method for the determination of the residues of 7 β 2 -receptor agonists in animal origin samples, including mabuterol, semantadine, ractopamine, clenbuterol, salbutamol, terbutaline and phenoxypropanamide Analysis of UHPLC-MS / MS and confirmation of positive samples. Methods Animal samples were extracted by ammonium acetate buffer solution and purified by cation exchange column. The mobile phase A consisted of 1 mmol / L ammonium acetate - 0.1% formic acid water, mobile phase B: 1 mmol / L ammonium acetate - 0.1% Formic acid in acetonitrile water (90:10, V / V) was separated on an Agilent C18 column (2.1 mm × 50 mm, 1.8 μm). Positive samples were confirmed by enhanced ion scan mode on a QTrap quadrupole mass spectrometer. This study also examined the matrix effects of seven β2-agonists. Results There was a strong matrix effect in the detection of β2-receptor agonist residues in animal-derived samples. Seven kinds of β2-agonists showed a good linearity in the range of 0.25-50 ng / g with a linear correlation coefficient of r> 0.99 and a standard recovery of 86.6% -108.7%. The detection limits were 0.1-0.5 ng / g. Conclusion This method uses internal standard method to reduce the quantitative error caused by matrix effect. The method has the advantages of lower detection limit, accurate quantification and short time of instrument analysis. It can be used to detect β2-agonist in animal samples Residues, while the positive samples for further confirmation.