超快速液相色谱-四极杆/线性离子阱质谱同时检测猪组织中9种β-受体阻断剂残留

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。

Simultaneous determination of nine β-blockers in porcine tissues by ultra-fast liquid chromatography coupled with quadrupole/linear ion trap mass spectrometry

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 nine β-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 by β-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 Kinetex^TM C18-XB column (150 mm×2.1 mm, 2.6 μm) 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 than 0.995 in the range of 0.1-20 μg/L. The limits of quantification (LOQ, S/N≥10) were 0.5 μg/kg for all the analytes. The developed method gave average recoveries of 87.5%-111.8% spiked at 0.5, 1.0 and 5.0 μg/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.