摘要
采用高效液相色谱-串联质谱法同时测定水产品中硝基呋喃和硝基咪唑类药物残留量。样品用盐酸水解，在酸性环境下进行衍生化反应16h，乙酸乙酯萃取。以PhenomenexLunaC18色谱柱为分离柱，以不同体积比的乙腈和乙酸（0．2＋99．8）溶液混合液为流动相进行梯度洗脱，采用电喷雾正离子源多反应监测模式检测。采用同位素内标法定量。方法的检出限（3S／N）在0．15～0．30μg·kg11之间。以空白样品为基体进行加标回收试验，所得回收率在83．3％～115%之间，测定值的相对标准偏差（n=6）在2．3％～14％之间。
HPLC-MS/MS was applied to the simultaneous determination of residual amounts of nitrofurans and nitroimidazoles in aquatic products. The sample was hydrolyzed in hydrochloric acid medium, and derivatized in an acidic condition for 16 h. Ethyl acetate was used as extraction solvent. Phenomenex Luna C18 chromatographic column was used as stationary phase, and mixtures of acetonitrile and acetic acid solution （0. 2-＋-99. 8） mixed in different ratio were used as mobile phase in gradient elution. ESI＋ and multi-reaction monitoring were adopted in MS/MS analysis. Isotope was used as internal standard. Detection limits （3S/N） found were ranged from 0. 15 to 0.30 μg @ kg-1. On the base of blank sample, test for recovery was made by standard addition method, values of recovery found were in the range of 83.3%-115%, with RSD＇s （n=6） in the range of 2.3%-14%
出处
《理化检验（化学分册）》
CAS
CSCD
北大核心
2015年第8期1168-1173,共6页
Physical Testing and Chemical Analysis(Part B:Chemical Analysis)
基金
江西出入境检验检疫局科技计划项目(2011JX007)
