基质分离固相萃取-液相色谱-串联质谱法快速测定牛肉中4种β2-受体激动剂类兽药残留

Rapid determination of 4 kinds of β2-agonist veterinary drug residues in beef by matrix separation solid phase extraction purification combined with liquid chromatography-tandem mass spectrometry

中文关键词:  β2-受体激动剂类兽药  液相色谱-串联质谱法  CNW兽药定量检测分散固相萃取纯化包

英文关键词:β2-agonist veterinary drugs  liquid chromatography tandem mass spectrometry  CNW veterinary drug quantitative detection and dispersive solid phase extraction purification method

中文摘要:

      目的 建立基质分离固相萃取结合液相色谱串联质谱法(liquid chromatography tandem mass spectrometry, LC-MS/MS)快速测定牛肉中克伦特罗、莱克多巴胺、沙丁胺醇、特布他林等4种β2-受体激动剂类兽药残留。方法 样品经葡萄糖醛苷酶/硫酸酯酶酶解、盐析后经CNW兽药定量检测分散固相萃取纯化包净化。采用LC-MS/MS电喷雾正离子模式、多反应监测采集(multiple reaction monitoring acquisition, MRM)测定。结果 当4种β2-受体激动剂类兽药化合物空白样本加标水平在2.5、12.5、50 ?g/kg时, 回收率为95.39%~106.59%, 相对标准偏差(relative standard deviation, RSD)为0.98%~13.26%。4种目标化合物的检出限为0.1~0.3 ?g/kg, 定量限为0.3~1.0 ?g/kg。针对市售66件牛肉样品中目标化合物进行检测, 结果均未检出。结论 与传统通过性固相萃取法相比, 兽药定量检测分散固相萃取纯化法净化效果更好, 基质效应更低。CNW兽药定量检测分散固相萃取法可用于牛肉中克伦特罗、莱克多巴胺、沙丁胺醇、特布他林4种β2-受体激动剂类兽药残留快速检测。

英文摘要:

      Objective To a establish a method for the rapid determination of 4 β2-agonist veterinary drug residues in beef, including clenbuterol, ractopamine, salbutamol and terbutaline by matrix separation solid phase extraction combined with liquid chromatography-tandem mass spectrometry (LC-MS/MS). Methods The samples were hydrolyzed by gluconidase/sulfatase, salted out, purified by CNW veterinary drug quantitative detection and dispersive solid phase extraction purification method, and determined by LC-MS/MS electrospray positive ion mode and multiple reaction monitoring acquisition (MRM). Results When the standard levels of 4 kinds of β2-agonist veterinary drug compounds in blank samples were spiked at 2.5, 12.5, and 50 ?g/kg, the recoveries were 95.39%?106.46%, and the relative standard deviation were 0.98%?13.26%. The limits of detection of the 4 kinds of target compounds were 0.1?0.3 ?g/kg, and the limits of quantification were 0.3?1.0 ?g/kg. The target compounds were detected in 66 beef samples on the market, but the results were not detected. Conclusion Compared with the traditional solid-phase extraction method, quantitative determination of veterinary drugs dispersive solid phase extraction purification method has better purification effect and lower matrix effect. CNW veterinary drug quantitative detection dispersive solid-phase extraction method can be used for rapid detection of 4 kinds of β2-agonist veterinary drug residues clenbuterol, ractopamine, salbutamol, and terbutaline in beef.