摘要
研究猪肝样品中莱克多巴胺测定的样品前处理方法。样品直接用HCl酸解并超声提取,同时添加70%72%的高浓度HClO4对酸解样品进行蛋白沉淀,然后经MCX固相萃取柱净化后,用液相色谱-串联质谱法检测。用正交试验考察了酸的种类、浓度、提取时间、提取温度和HClO4体积对提取效率的影响,最佳条件为：HCl浓度为0.2mol/L,提取时间为40min,提取温度为25℃,HClO4用量为200μL。从0.5、5.0和10.0μg/kg添加水平检测结果可以看出,方法平均回收率为82.0%102%,日内和日间精密度〈4%,符合国家标准对检验方法的要求。该方法灵敏度高,精密度好,成本低,能简便、快速对样品中的莱克多巴胺进行提取,实现对动物源性食品的快速监测。
A pretreatment method was developed for the determination of ractopamine in pig liver.The hydrochloric acid and perchloric acid in high concentrations（70%-72%）were respectively added to the sample to extract the target and deposit protein,and then a further purification was carried out by MCX solid phase extraction.The final detection was performed by high performance liquid chromatography-tandem mass spectrometry.The influencing factors,including acid type,acid concentration,extraction time,temperature and perchloric acid volume,were studied by orthogonal experiment.0.2 mol/L of hydrochloric acid,120 min of extraction,25℃ and 200μL of perchloric acid were found to be the suitable conditions.The average recoveries ranged from 82.0%to 102% at the spiked levels of 0.50,5.00 and 10.0μg/kg,and RSDs of within-day and between-day were lower than 4%.Therefore,the method conforms to the national standard demand.This sensitive,accurate and low-cost method can rapidly extract ractopamine in samples,and may be extensively used to determine β2-agonists in animal derived food.
出处
《分析科学学报》
CAS
CSCD
北大核心
2016年第3期435-438,共4页
Journal of Analytical Science
基金
泉州市科技局科技项目(No.20132113)
关键词
猪肝
莱克多巴胺
样品前处理
固相萃取
Pig liver
Ractopamine
Pretreatment
Solid phase extraction
