亲水相互作用色谱-串联质谱法测定禽类及其制品中利巴韦林残留总量

Determination of total residue of ribavirin in poultry and its products by Hydrophilic Interaction Chromatography-Tandem Mass Spectrometry

中文关键词:  利巴韦林  亲水相互作用色谱  禽类及其制品

英文关键词:ribavirin  hydrophilic interaction chromatography  poultry and its products

中文摘要:

      目的:针对多种复杂基质中利巴韦林残留量的测定,建立了基于固相萃取-亲水相互作用色谱-串联质谱法的利巴韦林残留总量的测定方法。方法:均质后的样品经20 g/L三氯乙酸提取,酸性磷酸酯酶水解,苯硼酸型离子交换固相萃取柱净化后,由实心核颗粒HILIC色谱柱(规格100 mm×2.1 mm,1.6 μm)分离,流动相为5 mmol/L乙酸铵水溶液(含0.1%甲酸)-乙腈,梯度洗脱。在正离子扫描多反应监测模式下检测,内标峰面积法定量。结果:经方法验证,在15种禽类及其制品基质中,利巴韦林的检出限为1.0 μg/kg,在3个水平(1.0 μg/kg,2.0 μg/kg,10.0 μg/kg)下加标回收率为90.7-117.9%,相对标准偏差0.8-9.4%。结论:方法稳定可靠,可适用于多种禽类及其制品中利巴韦林残留量的分析。

英文摘要:

      ABSTRACT:Objective:A method for determining the total residue of ribavirin in complex matrices was established based on solid-phase extraction-hydrophilic interaction chromatography-tandem mass spectrometry.Methods:After homogenization, the sample was extracted with 20 g/L trichloroacetic acid, and then acid phosphatase hydrolysis was performed. The resulting solution was purified by a benzeneboronic acid-type ion exchange solid phase extraction column, and then separated by a solid core HILIC chromatographic column (100 mm×2.1 mm, 1.6 μm) with a mobile phase of 5 mmol/L ammonium acetate aqueous solution (containing 0.1% formic acid)-acetonitrile using a gradient elution method. Detection was performed in positive ion scan multiple reaction monitoring mode, and quantification was done by internal standard peak area method. Results:The method was validated, and the detection limit of ribavirin was 1.0μg/kg in 15 kinds of poultry and their product matrices. The recoveries at three levels (1.0 μg/kg, 2.0 μg/kg, and 10.0 μg/kg) were 90.7-117.9%, and the relative standard deviations were 0.8-9.4%. Conclusion:The method is stable and reliable, and it can be applied to the analysis of ribavirin residues in various poultry and their products.