QuEchERS/超高液相色谱-串联质谱法同时测定饲料中6种β-阻断剂类药物

Simultaneous delerminalion of 6 β-blockers in feed using ultra performance liquid chromalography-tandem mass spectrometry

本实验建立了饲料中阿替洛尔、纳多洛尔、醋丁洛尔、艾司洛尔、卡拉洛尔、卡维地洛6种β-阻断剂类药物的UPLC-MS/MS测定及确证方法。样品经乙腈-甲醇（3∶7,V/V）溶液振荡提取后,加入Qu Ech ERS吸附剂净化,经氮气吹干后用30%乙腈溶液定容,采用电喷雾正离子模式检测,同位素内标法定量。结果表明：6种β-阻断剂类药物在1-500μg/L线性相关系数均大于或等于0.9990,检出限为0.02-0.16μg/kg,定量限为0.07-0.54μg/kg;添加浓度水平为5、10、20μg/kg时,平均回收率为81.8%-119.6%,RSD为4.8%-11.3%。该方法灵敏度高,线性范围宽,且实用性强,可对饲料中6种β-阻断剂类药物进行定性和定量分析。

A method was established for the determination of 6 13-blockers in feed using Ultra performance Liquid chro- matography-tandem mass spectrometry （UPLC-MS/MS）.The samples were extracted with aeetonitrile-methanol （3：7,V/V）by shake,the extracts was purified with the mixed QuEchERS adsorbents,under nitrogen gas stream,followed by blowing to dryness,reconstitution with aeetonitrile-water（3：7, V/V）before the analysis by UPLC-MS/MS.The analytes were determined by electrospray ionization in positive ion mode,and quantified by isotope internal standard method.As a result,good linear relationship（r≥0.9990）was observed within the concentration range of 1.0 - 500.0 μg/LThe limit of detection of 6 β-blockers were 0.02 - 0.16 μg/kg,and limits of quantification were 0.07 - 0.54μg/kg.At adding levels of 5.0,10.0 and 20.0 μg/kg, average reeoveries were between 81.8% - 119.6% ,the RSD was 4.8% - 11.3%.The method was sensitive with wide linearity range and strong practicability,which could be used on qualitative and quantitative analysis of β-blockers in feed.