【摘要】 建立了同时检测猪组织中9种β-受体阻断剂(BBs)残留的超快速液相色谱-四极杆/线性离子阱质谱方法。均质试样经β-葡糖醛苷酶/芳基硫酸酯酶水解,乙腈提取,硅藻土与BondElut分散固相萃取填料双重快速净化,以0.1%(v/v)甲酸水溶液-甲醇为流动相使用KinetexTMC18-XB色谱柱(150 mm×2.1 mm,2.6μm)超快速液相色谱分离,优化多反应监测(MRM)离子对后,采用预设定多反应监测(sMRM)-信息依赖性采集(IDA)-增强子离子扫描(EPI)模式检测,在线EPI谱库定性分析,内标法定量。结果表明,9种BBs在线性范围内的线性关系良好(r≥0.995);定量限(LOQ,S/N≥10)均达到0.5μg/kg;3个添加水平(0.5、1.0和5.0μg/kg)下的回收率为87.5%~111.8%;RSD为4.0%~12.5%。该方法快速、准确、灵敏,可有效用于猪组织样品中多种BBs残留的同时测定。更多还原

【Abstract】 A highly sensitive method using ultra-fast liquid chromatography coupled with quadrupole/linear ion trap mass spectrometry(UFLC-Q/Trap MS)was developed to simultaneously screen and confirm nineβ-blockers(BBs)in porcine tissues(porcine muscle,liver and kidney).The method was used for trace determination of atenolol,pindolol,acebutolol,metoprolol,carazolol, labetalol,bisoprolol,propranolol and penbutolol.The homogenized tissues were hydrolyzed byβ-glucuronidase/aryl sulfatase and extracted with acetonitrile,followed by continuous purification procedures of disperse solid phase extraction(d-SPE)with diatomaceous earth and BondElut cartridge.The ultra-fast chromatographic separation was conducted on a KinetexTM C18-XB column(150 mm×2.1 mm,2.6μm)using 0.1%(v/v)formic acid aqueous solution and methanol as mobile phases in gradient elution.The optimized ion transitions were employed in the mixed-mode of scheduled multiple reaction monitoring(sMRM)-information dependent acquisition(IDA)-enhanced product ion(EPI)scan.Qualification analysis was performed through spectra-matching with on-line lab-built MS/MS library.For quantification stable isotope-labelled analogues of the analytes were used as internal standards.As a result,in porcine liver,kidney and muscle,the nine BBs showed good linearity with all the correlation coefficients(r)more than0.995in the range of 0.1-20μg/L.The limits of quantification(LOQ,S/N≥10)were 0.5μg/kg for all the analytes.The developed method gave average recoveries of 87.5%-111.8%spiked at 0.5,1.0and 5.0μg/kg with the relative standard deviations of 4.0%-12.5%.The proposed method can be used to screen and confirm the nine BBs in a single run,which makes it effective in surveillance and detection of the BBs residues in porcine tissues.更多还原