超高效液相色谱-串联质谱法测定水果及谷物中多抗霉素B残留量

Determination of Polyoxin B Residues in Fruit and Grains by Ultra High Performance Liquid Chromatography Tandem Mass Spectrometry

建立了一种快速有效的超高效液相色谱串联质谱法检测分析水果及谷物中多抗霉素B残留量的方法。色谱柱为Waters CORTECS®HILIC(150 mm×2.1 mm,2.7μm),流动相为0.1%甲酸(含5 mmol·L^(-1)甲酸铵)水溶液和乙腈,梯度洗脱,流速为0.40 mL·min-1。采用多反应监测模式(Multiple Reaction Monitoring,MRM),采用ESI正电离源,定量离子对508.1/305。样品经0.2%甲酸水溶液超声提取,离心取上清液,经由PLS柱(亲水亲脂平衡固相萃取柱)净化,过膜后直接测定,外标法定量。结果表明,多抗霉素B在2~50μg·L^(-1)线性关系良好,相关系数r2>0.999。在3个浓度加标水平条件下,即多抗霉素B浓度为0.10 mg·kg^(-1)、0.20 mg·kg^(-1)和1.00 mg·kg^(-1)时,回收率为91.1%~112.3%,相对标准偏差为6.7%~10.1%。该方法操作简便、回收率高,可用于批量水果及谷物中多抗霉素B残留的检测。

A new method was developed for the determination of polyoxin B in fruit and grain by ultra performance liquid chromatography tandem mass spectrometry.The chromatography column was Waters CORTECS®HILIC(150 mm×2.1 mm,2.7μm),the mobile phase is 0.1%formic acid(containing 5 mmol·L^(-1)ammonium formate)aqueous solution and acetonitrile,with gradient elution,the flow rate is 0.40 mL·min-1.Adopting multiple reaction monitoring(MRM)mode,using ESI positive ionization source,and quantifying ion pairs 508.1/305.The sample was extracted by ultrasound with a 0.2%formic acid aqueous solution,the supernatant was centrifuged,purified by PLS column,and directly measured after passing through the membrane.The external standard method was used for quantification.The linear range of the method was 2~50μg·L^(-1),with the external standard method and r2>0.999.Under the conditions of three concentration spiking levels,namely,when the concentration of polyoxin B is 0.10 mg·kg^(-1),0.20 mg·kg^(-1),and 1.00 mg·kg^(-1),the recovery rate is 91.1%~112.3%,and the relative standard deviations were in the range of 6.7%~10.1%.This method is easy to operate and has a high recovery rate,and can be used for the residual testing of polyoxin B in bulk fruits and grain.