HPLC-MS/MS技术同时测定鸡蛋中5种抗球虫药

Simultaneous Determination of Five Anticoccidials in Eggs by HPLC-MS/MS

建立一种分析鸡蛋中残留5种抗球虫类药物(尼卡巴嗪、地克珠利、托曲珠利、托曲珠利砜、托曲珠利亚砜)的高效液相色谱-串联质谱(HPLC-MS/MS)检测方法。基于QuEChERS净化,样品采用含0.1%甲酸的乙腈溶液提取目标分析物,于250 mg C_(18)及50 mg PSA的混合分散固相萃取粉末净化提取。以5 mmol/L乙酸铵水溶液和甲醇为流动相,电喷雾负离子方式扫描,多反应监测模式(MRM)结合内标法进行定性定量分析。结果表明,5种目标化合物的在0.02~40.00 ng/mL范围呈良好的线性关系(R~2>0.990)。检出限(LOD,rSN=3)为0.003~0.300μg/kg,定量下限(LOQ,r_(SN)=10)为0.010~0.800μg/kg;空白样品中添加0.6,3.0和6.0μg/kg 3个水平的混合标准溶液,回收率在79.5%~99.3%之间,相对标准偏差(S_(RSD),n=6)≤10.5%。该方法简便、灵敏、准确,可满足鸡蛋中5种抗球虫药物的同时检测。

An effective high performance liquid chromatography tandem mass spectrometry method was developed for the simultaneous detection of five anticoccidials residues(nicarbazine,dexamethasone,tropizuril,tropizuril sulfone,and tropizuril sulfoxide) in eggs.The samples were extracted with 0.1% formic acid acetonitrile solution,and then the extracted supernatant was purified by QuEChERS with 250 mg C_(18) and 50 mg PSA,and determined by HPLC-MS/MS.5 mmol/L ammonium acetate-0.1% formic acid aqueous solution and methanol were used as mobile phase for gradient elution.The quantitative and qualitative ions of anticoccidials and its residual markers were monitored by negative ion scanning(ESI-) and multi ion detection mode(MRM) with internal standard method.The calibration curves showed a good linearity in the range of in the range of 0.02-40.00 ng/mL for the 5 components,with their correlation coefficients(R~2) larger than 0.990.The limits of detections(LOD,r_(SN)=3) and limits of quantitation(LOQ,r_(SN)=10) were in the ranges of 0.003-0.300 μg/kg and 0.010-0.800μg/kg,respectively.The average recoveries for the 5 targets at three different spiked concentration levels(0.6,3.0 and 6.0 μg/kg) ranged from 79.5% to 99.3%.The relative standard deviations(S_(RSD),n=6) were≤10.5%.This method was simple,sensitive and accurate,and was suitable for the simultaneous quantificaition of five anticoccidials residues in eggs.