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

Simultaneous determination of nineβ-blockers in porcine tissues byultra-fast liquid chromatographycoupled with quadrupole/linear ion trapmass spectrometry

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 Kinetex TM C18-XB 色谱柱（150 mm＆#215;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。

A highly sensitive method using ultra-fast liquid chromatography coupled with qua-drupole/linear ion trap mass spectrometry（UFLC-Q/Trap MS）was developed to simultaneous-ly screen and confirm nine β-blockers（BBs）in porcine tissues（porcine muscle,liver and kid-ney）. The method was used for trace determination of atenolol,pindolol,acebutolol,metopro-lol,carazolol,labetalol,bisoprolol,propranolol and penbutolol. The homogenized tissues were hydrolyzed by β-glucuronidase/aryl sulfatase and extracted with acetonitrile,followed by con-tinuous 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＆#215;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 per-formed 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 por-cine liver,kidney and muscle,the nine BBs showed good linearity with all the correlation coef- 〈br〉 ficients（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.