建立了一种分子印迹固相萃取-超高效液相色谱-串联质谱同时测定猪肉中5种β2-受体激动剂残留的方法。样品经过均质处理后置于乙酸铵／乙酸缓冲液中，加入内标物和β-葡萄糖醛酸酶／芳基硫酸酯酶，于55℃酶解2 h，调节溶液 pH后通过分子印迹固相萃取柱净化，然后采用 BEH C18色谱柱分离，以甲醇-0.1％（ v／v）甲酸水溶液为流动相，采用梯度洗脱，在电喷雾正离子多反应监测模式下用内标法定量。检出限（ LOD，S／N=3）和定量限（ LOQ，S／N=10）分别为0.005~0.009μg／kg和0.015~0.025μg／kg。在0~10μg／kg范围内线性关系良好，相关系数≥0.9933。添加水平为0.25、1、5μg／kg时，回收率为80.4％~92.9％，相对标准偏差为1.2％~6.3％。该方法具有灵敏度高、重复性好、回收率高等优点，适合同时进行多种β2-受体激动剂残留的测定。
An ultra-high performance liquid chromatography-tandem mass spectrometry ( UPLC-MS/MS)method with molecularly imprinted solid phase extraction for the determina-tion of five β2-gonists residues in pork has been developed. After the sample preparation,the ammonium acetate/acetic acid buffer was added,followed by the internal standard and β-glu-curonidase/arylsulfatase enzyme. The solution was incubated at 55 ℃ for 2 h. After adjusting the pH of the solution,it was purified by a molecularly imprinted solid phase extraction col-umn,then analyzed on a BEH C18 column with methanol-0. 1%( v/v ) formic acid aqueous solution as the mobile phases in gradient elution mode. The MS/MS analysis was in positive ion mode and multiple reaction monitoring mode. The analytes were quantified by the internal standard method. The limits of detection( LODs,S/N = 3 ) and the limits of quantification ( LOQs,S/N=10)were 0. 005-0. 009 μg/kg and 0. 015-0. 025 μg/kg,respectively. In the range of 0-10 μg/kg,the correlation coefficients of linear calibration curves were not less than 0. 993 3. At the spiked levels of 0. 25,1. 0 and 5. 0 μg/kg,the recoveries were 80. 4%-92. 9%with the relative standard deviations of 1. 3%-6. 3%. The method is of high sensitivity,good reproducibility,high recovery,and is useful for the simultaneous determination of multiple β2-agonists residues.
参考文献
| [1] | Juan, C.;Igualada, C.;Moragues, F.;León, N.;Ma?es, J..Development and validation of a liquid chromatography tandem mass spectrometry method for the analysis of β-agonists in animal feed and drinking water[J].Journal of chromatography, A: Including electrophoresis and other separation methods,201039(39):6061-6068. |
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