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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。
An ultra-fast liquid chromatography-quadrupole / linear ion trap mass spectrometry method was developed for the simultaneous determination of nine β-blockers (BBs) in pig tissues. The homogenized sample was double-purified rapidly by β-glucuronidase / aryl sulfatase hydrolysis, acetonitrile extraction, diatomaceous earth and BondElut dispersed solid phase extraction packing. The homogeneous sample was purified with 0.1% (v / v) The mobile phase was separated on a Kinetex TMC18-XB column (150 mm × 2.1 mm, 2.6 μm) by ultra-fast liquid chromatography and optimized for multiple reaction monitoring (MRM) ion pairs using a pre-defined multiple reaction monitoring (sMRM) Acquisition (IDA) - enhanced ion scan (EPI) mode detection, online EPI library qualitative analysis, internal standard quantification. The results showed that the linearity of nine BBs was good (r≥0.995), the limit of quantification (LOQ, S / N≥10) reached 0.5μg / kg. The three addition levels of 0.5, 1.0 and 5.0μg / kg) recovery was 87.5% ~ 111.8%; RSD was 4.0% ~ 12.5%. The method is rapid, accurate and sensitive and can be applied to the simultaneous determination of multiple BBs residues in pig tissue samples.