混合型阳离子交换固相萃取-液相色谱-串联质谱法测定肉样中特布他林、沙丁胺醇、莱克多巴胺和克伦特罗残留

Determination of terbutaline,salbutamol,ractopamine,and clenbuterol residues in meat samples based on mixed-cationic exchange solid-phase extraction and liquid chromatography-tandem mass spectrometry

目的建立一种灵敏和准确地检测肉制品中特布他林、沙丁胺醇、莱克多巴胺和克伦特罗4种β2-受体激动剂残留的快速分析方法。方法肉制品经2%磷酸甲醇-水溶液(80∶20,V/V)涡旋提取10 min,离心,上清液经乙酸酸化后采用混合型阳离子交换固相萃取小柱(MCX)净化,以乙腈和0. 1%(V/V)甲酸水溶液作为流动相,在反相C18柱上进行梯度洗脱与色谱分离,以三重四级杆串联质谱(MS/MS)进行检测,内标法定量。结果 4种β2-受体激动剂在0. 2μg/L^100. 0μg/L呈现较好的线性关系(r≥0. 999 2),方法的检出限(LODs)为0. 03μg/kg^0. 08μg/kg。当加标水平为1. 0μg/kg、40. 0μg/kg和80. 0μg/kg时,肉制品中4种β2-受体激动剂的加标回收率为86. 2%~101. 3%,相对标准偏差(RSD)为1. 1%~8. 3%。结论本法可用于猪肉、猪肝、牛肉和牛肝等肉制品中常见β2-受体激动剂残留检测与分析。

Objective To develop a sensitive and accurate method for simultaneous determination of four β2-agonists including terbutaline,salbutamol,ractopamine,and clenbuterol in meat samples. Methods The meat samples were firstly extracted by 2% phosphoric acid-methanol-water solution( 80 ∶20,V/V) for 10 minutes by vortex,followed by centrifugation. The supernatant was acidized using acetic acid and purified by mixed-cationic exchange( MCX) solid-phase extraction cartridges,and then the LC separation was carried out on a reversed-phase C18 column with a linear gradient elution program using acetonitrile,with water containing 0. 1%( V/V) formic acid as elution solvent. The triple quadrupole tandem mass spectrometer was applied for quantitative analysis by internal standard method. Results The four target β2-agonists were of good linearity in the range of 0. 20 μg/L-50. 0 μg/L,with correlation coefficients( r) greater than 0. 999 2. The limits of detection( LODs)were within 0. 03 μg/kg-0. 08 μg/kg. Spiking recoveries of the four target compounds ranged from 86. 2% to 101. 3% at the three spiked levels of 1. 0 μg/kg,40. 0 μg/kg and 80. 0 μg/kg. The relative standard deviations( RSDs) were within 1. 1%-8. 3%. Conclusion The developed method in this study could be used for routine analysis of β2-agonists in pork,pork liver,beef,and beef liver samples.