超高效亲水色谱-串联质谱法快速检测鸡肉及其制品中的利巴韦林及其代谢物的总残留量

建立了鸡肉及其制品中利巴韦林和磷酸化利巴韦林代谢物总残留量的亲水作用色谱-串联质谱分析方法(HILIC-MS/MS)。样品采用含1%(v/v)乙酸的乙腈超声提取,于37 ℃条件下以酸性磷酸酶酶解,正己烷除脂后用C₁₈与PSA填料分散固相萃取净化。采用酰胺基超高效亲水作用色谱柱,在乙腈和0.1%甲酸组成的梯度洗脱流动相中分离,在电喷雾正离子电离多反应监测模式下监测,结果表明,样品中利巴韦林残留量在1~200 μg/kg之间时,线性相关系数大于0.999,方法检出限(LOD, S/N≥3)为1 μg/kg,定量限(LOQ, S/N≥10)为5 μg/kg,在3个添加水平下的回收率为67.8%~112.7%,相对标准偏差为6.1%~13.6%。经测定多种实际样品,证明该方法简便、快速、准确,可以满足日常鸡肉及其制品中利巴韦林及其代谢物总残留量的分析要求。

Rapid determination of total residues of ribavirin and its metabolites in chicken and chicken products by ultra-performance hydrophilic interaction chromatography-tandem mass spectrometry

An analytical method was developed for the determination of total residues of ribavirin and its phosphorylated metabolites in chicken and its products by hydrophilic interaction chromatography-tandem mass spectrometry. The samples were extracted with acetonitrile containing 1% (v/v) acetic acid under ultrasonic condition and then enzymatically hydrolysed with acid phosphatase at 37 ℃. After liposoluble substances being removed with hexane, C₁₈ and PSA dispersion solid phase extraction (DSPE) was introduced to cleanup procedures. The separation was performed on an ultra-performance hydrophilic interaction chromatographic (HILIC) amide column under a gradient elution using acetonitrile and 0.1% formic acid. The analytes were detected in the positive electrospray ionization and multi-reaction monitoring (MRM) mode. In the range of 1-200 μg/kg, the correlation coefficient was greater than 0.999. The limit of detection (LOD, S/N≥3) was 1 μg/kg and the limit of quantification (LOQ, S/N≥10) was 5 μg/kg. The recoveries of ribavirin spiked at three levels ranged from 67.8% to 112.7% with the relative standard deviations (RSDs) of 6.1%-13.6%. The results of the determination of ribavirin in various real samples showed that the method is simple, rapid, accurate and suitable for the determination of total residues of ribavirin and its metabolites in chicken and its products.