摘要
目的建立了一种禽肉、蛋中抗球虫类药物的高效液相色谱-串联质谱检测方法。方法通过优化质谱与色谱条件,采用两两比较方差分析比较不同前处理间的基质效应,确定检出限及定量限,建立空白基质标准曲线,在1、5、10倍定量限进行加标回收实验。结果实验得出基质样品经2%甲酸乙腈提取、Captiva EMR-Lipid固相萃取小柱净化,在SVEA C18色谱柱中以0.1%甲酸-50 mmol/L乙酸铵水溶液和乙腈为流动相时,实现23种抗球虫药物的残留测定。在多反应监测模式采集数据并结合外标法进行定性定量分析的条件下所得的关系呈现线性,且其R^(2)≥0.99。此外,总体平均回收率>80%,总体相对偏差<10%。结论该方法对禽肉、蛋中的抗球虫药物残留的测定十分有效。
Objective In this paper,an effective high performance liquid chromatography tandem mass spectrometry(HPLC-MS/MS) method was established for determining the coccidiostats in poultry meat and eggs. Methods Mass spectrometry conditions and chromatographic conditions were optimized. Matrix effects between different pretreatments were compared by two-way comparative variance analysis. Detection limits and quantitative limits were determined. Standard curves of blank matrix were established. Standard recovery experiments were carried out at 1,5 and 10 times quantitative limits. Results The well determination of 23 kinds of coccidiostats were achieved after the applied substrate samples extracted by 2% formic acid acetonitrile,purified by Captiva EMR-Lipid,and penetrated to a channel of SVEA C18 chromatographic column(0.1% formic acid-50 mmol/L ammonium acetate and acetonitrile as a mobile phase). Under the condition of multi-reaction monitoring mode data collection and external standard method for qualitative and quantitative analysis,the R^(2) of resulting linear relationship was ≥0.99.Moreover,the overall average recovery and overall relative deviation was >80% and <10% respectively. Conclusion This method is effective for the determination of coccidiostats residues in eggs and poultry meat.
作者
李莹
羊银
柳溪
翟雨佳
LI Ying;YANG Yin;LIU Xi;ZHAI Yu-jia(Instrument Analysis Department,Tianjin.Institute for Food Safety Inspection Technology,Tianjin,300308,China)
出处
《职业与健康》
CAS
2021年第12期1613-1618,共6页
Occupation and Health
基金
天津市市场监督管理委员会科技计划项目(2018-W02)。
关键词
抗球虫药
禽肉
蛋
多残留检测
高效液相色谱-串联质谱
Coccidiostat
Poultry meat
Eggs
Multi-residues determination
High performance liquid chromatography tandem mass spectrometry
