摘要
目的建立固相萃取-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的方法。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(100 mm×2.1 mm,1.6μm)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。结果在15种禽类及其制品基质中做加标曲线,在1~20μg/kg浓度范围内线性关系良好,相关系数为0.995~0.999。在1.0、2.0、10.0μg/kg 3个水平下加标回收率为90.7%~117.9%,相对标准偏差0.8%~9.4%。结论该方法稳定可靠,可适用于多种禽类及其制品中利巴韦林残留量的分析。
Objective To establish a method for determining the total residue of ribavirin in complex matrices 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,1.6μm)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 A spiked curve was performed on 15 types of poultry and their product matrices,and the linear relationship was good within the concentration range of 1–20μg/kg,with a correlation coefficient of 0.995–0.999.The recoveries at 3 levels 1.0,2.0 and 10.0μg/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 its products.
作者
史娜
耿健强
郑跃
郭蕊
周密
姜洁
SHI Na;GENG Jian-Qiang;ZHENG Yue;GUO Rui;ZHOU Mi;JIANG Jie(Beijing Institute of Food Inspection and Research(Beijing Municipal Center for Food Safety Monitoring and Risk Assessment),Key Laboratory of Key Technologies of Major Comprehensive Guarantee of Food Safety,State Administration for Market Regulation,Beijing 100094,China)
出处
《食品安全质量检测学报》
CAS
2024年第16期203-210,共8页
Journal of Food Safety and Quality
关键词
利巴韦林
亲水相互作用色谱-串联质谱法
禽类及其制品
ribavirin
hydrophilic interaction chromatography-tandem mass spectrometry
poultry and its products
