HPLC-MS/MS法同时测定动物源性食品中9种吡咯里西啶类生物碱的含量

建立了高效液相色谱-串联质谱法(HPLC-MS/MS)检测动物源性食品中9种吡咯里西啶类生物碱残留的分析方法。蜂蜜、乳制品及动物肝脏样品分别用0.05 mol/L盐酸、1%三氯乙酸、5%乙酸乙腈溶解,强阳离子固相萃取柱(Waters Oasis MCX)进行富集和净化后,用Phenomenex Kinetex C₁₈(4.6 mm×100 mm,2.6μm)色谱柱进行分离,以甲醇-0.1%甲酸-5 mmol/L乙酸铵水溶液为流动相进行梯度洗脱,在电喷雾正离子多反应监测模式下进行检测。9种吡咯里西啶类生物碱在0～100 ng/mL质量浓度范围内线性关系良好,相关系数均大于0.99。在10、20和50μg/kg加标水平下,5种不同基质中9种吡咯里西啶类生物碱的平均回收率为71.0%～103%,相对标准偏差(RSD)为3.0%～9.8%,方法的检出限为3μg/kg,定量下限为10μg/kg。该方法简单、快速、准确,适用于动物源性食品中吡咯里西啶类生物碱的同时测定。

Determination of 9 Pyrrolizidine Alkaloids in Animal derived Foods by HPLC-MS/MS

A method of high performance liquid chromatography-tandem mass spectrometry(HPLC-MS/MS)was developed for the determination of nine pyrrolizidine alkaloid residues in animal-derived foods.Honey,dairy and animal liver samples were dissolved with 0.05 mol/L hydrochloric acid,5%trichloroacetic acid and acetonitrile containing 1%acetic acid,respectively,then enriched and purified with a strong cationic solid phase extraction column(Waters Oasis MCX).The separation was carried out on a Phenomenex Kinetex C18 column(4.6 mm×100 mm,2.6μm)by gradient elution with methanol-0.1%formic acid-5 mmol/L ammonium acetate as mobile phase.The separated compounds were detected in positive electrospray ionization(ESI+)under multiple reaction monitoring(MRM)mode.The calibration curves for 9 alkaloids were linear in the mass concentration range of 0-100 ng/mL with correlation coefficients(r)larger than 0.99.The average recoveries at there spiked levels of 10,20 and 50μg/kg ranged from 71.0%to 103%,with relative standard deviations(RSD)of 3.0%-9.8%.The limits of detection and limits of quantitation(LOQs)of the method were 3μg/kg and 10μg/kg,respectively.The method is simple,rapid and accurate,and is suitable for the simultaneous determination of pyrrolizidine alkaloids in animal-derived foods.