改进QuEChERS法快速测定鸡蛋和鸡肉中氯苯胍

A Modified QuEChERS Method Rapidly Determination of Robenidine in Eggs and Chicken

建立一种改进QuEChERS结合高效液相色谱-串联质谱(HPLC-MS/MS)快速测定鸡蛋和鸡肉中氯苯胍残留量的分析方法。样品经甲酸-乙睛-水混合溶液(4∶1∶0.01,V/V)超声提取,乙睛饱和的正己烷除脂后C_(18)分散固相萃取净化。选择色谱柱(ZORBAX SB-Aq,3.0 mm×100 mm,3.5μm)进行分离,乙睛-0.1%甲酸水溶液梯度洗脱,在多反应监测正离子模式下对鸡蛋和鸡肉中氯苯胍进行分析测定。结果表明,经优化条件,氯苯胍在1~50 ng/mL质量浓度范围内有良好的线性关系(R2=0.9994)。检出限(S_(LOD),r_(SN)=3)为5.0μg/kg,定量限(S_(LOQ),r_(SN)=10)为10μg/kg。对2种基质分别进行3个水平的添加试验(n=6),氯苯胍平均回收率为80.3%~94.1%,相对标准偏差为0.1%~3.0%。该方法高效,快速,简便,适用于鸡蛋和鸡肉中氯苯胍的测定。

A modified QuEChERS(quick,easy,cheap,effective,rugge and safe)method was combined with high performance liquid chromatography-tandem mass spectrometric for rapidly determination of the robenidine in eggs and chickens.The sample was extracted by ultrasonic with the combination of formic acid-acetonitrile-water solution(4∶1∶0.01,V/V),and purified by C_(18) dispersion solid phase extraction after degreasing with n-hexane saturated acetonitrile.Selecting chromatographic column(ZORBAX SB-Aq,3.0 mm×100 mm,3.5μm)for separation,by gradient elution using acetonitrile-0.1%formic acid water as mobile phase,robenidine in eggs and chicken was analyzed and determined in multiple reaction monitoring(MRM)positive ion mode.The results showed that robenidine showed a good linear relationship in the concentration range of 1-50 ng/mL.The limit of detection(S_(LOD),r_(SN)=3)was 5μg/kg and the limit of quantity(S_(LOQ),r_(SN)=10)was 10μg/kg.The average recovery of samples was 80.3%-93.8%,and the relative standard deviation was 0.1%-3.0%.This method was simple in pretreatment rapidly and high-efficiently suitable for the determination of robenidine in egg and chicken samples.