TurboFlow在线净化/液相色谱-四极杆/静电场轨道阱高分辨质谱法快速测定动物源性食品中五氯酚残留量

Rapid Determination of Pentachlorophenol in Animal-origin Foods by TurboFlow On-line Purification/Liquid Chromatography-quadrupole/ElectrostaticField Orbitrap High-resolution Mass Spectrometry

建立基于TurboFlow在线净化/液相色谱-四极杆/静电场轨道阱高分辨质谱(Turbo Flow Online Purification Liquid Chromatography-Quadrupole Electrostatic Field Orbitrap High-resolution Mass Spectrometry,TF-QE-Orbitrap-HRMS)快速测定动物源性食品中五氯酚(Pentachlorophenol,PCP)的分析方法。采用2%乙酸乙腈提取目标物,提取液经在线净化柱CycloneTMP(0.5 mm×50 mm,50μm)净化、富集,通过CORTECSR T3分析柱(100 mm×4.6 mm,2.7μm)色谱分离,采用四极杆/静电场轨道阱高分辨质谱,以全扫描/平行反应检测(Full Scan/PRM)模式检测,内标法定量。结果表明,五氯酚在0.005~0.100 ng/mL质量浓度范围内线性关系良好,相关系数大于0.9998,定量限为0.2μg/kg,3个添加水平的加标回收率为95.6%~104.0%,相对标准偏差为1.9%~4.9%。该方法前处理高效简单、结果准确、无基质效应,适用于动物源性食品中五氯酚的大规模检测,具有一定实际意义。

To establish a rapid analysis method for the determination of Pentachlorophenol(PCP)in animal-origin foods based on TurboFlow online purification/Liquid Chromatography-Quadrupole/Electrostatic Field Orbitrap High-resolution Mass Spectrometry(TF-QE-Orbitrap HRMS).Targets were extracted by acetonitrile added with 2%acetic acid,followed by an automated turbulent flow cyclone chromatography sample clean-up system.The online purification technology TurboFlow was used for online sample cleanup instead of lengthy offline solid-phase extraction(SPE),Combining the number of target compounds with the high sample throughput,this approach fulfills the demand for a fast and cost-effective multi-analyte method.Sample extraction solution was purified and collected with a CycloneTMP column(0.5 mm×50 mm,50μm).The analytes were eluted from the extraction column and put into an CORTECSR T3 analytical column(100 mm×4.6 mm,3μm)prior to chromatographic separation and detection in Full Scan/PRM mode,and quantified by internal standard method.The results showed that the calibration curves of Pentachlorophenol was linear in the range of 0.005~0.100 ng/mL,with correlation coefficients(R2)larger than 0.9998.The limits of quantitation(LOQ)of the method was 0.2μg/kg.The recoveries at three spiked levels ranged from 95.6%to 104.0%,with relative standard deviations(RSD)of 1.9%~4.9%.With its economies,simple pretreatment steps,rapid analysis,and accuracy,the method was suitable for the quantification of Pentachlorophenol in animal-origin foods.