【摘要】 目的建立超高效液相色谱法（ultra-performance liquid chromatography,UPLC）同时测定蜂蜜中双甲脒及其代谢物（2, 4-二甲基苯胺）残留量的方法。方法样品经0.1 mol/L NaOH溶液提取、正己烷-异丙醇（2:1,V:V）混合液萃取,再采用ACQUITYUPLC?BEHC₁₈（2.1mm×100mm,1.7μm）色谱柱进行分离,以乙腈和20 mmol/L乙酸铵溶液作为流动相,柱温30℃、流速为0.20 mL/min,检测器波长在235 nm处进行检测,外标法定量。结果双甲脒及2,4-二甲基苯胺标准曲线在2.0～500.0 ng/mL范围内呈良好的线性关系,线性相关系数均大于0.999,方法检出限双甲脒为0.27μg/kg, 2,4-二甲基苯胺为0.42μg/kg,以样品加标做回收率测定,双甲脒与2,4-二甲基苯胺的回收率分别为99.6%～101.2%和99.3%～101.6%,测得的相对标准偏差均小于5%。结论该方法具有线性范围宽、检出限低,灵敏度、准确度高,重复性好等优点,能满足于蜂蜜中双甲脒及2,4-二甲基苯胺的快速检测要求。更多还原

【Abstract】 Objective To establish a method for the determination of amitraz and its metabolite（2,4-dimethylaniline） residues in honey by ultra-performance liquid chromatography. Methods The samples were diluted with 0.1 mol/L sodium hydroxide, extracted with n-hexane-isopropanol（2:1, V:V）, and then separated by ACQUITY UPLC?BEH C₁₈（2.1 mm×100 mm, 1.7 μm） with ammonium acetate（20 mmol/L）/Acetonitrile as the gradient eluent with a flow rate of 0.20 mL/min at 30 ℃. A diode array detector was used to detect at 235 nm. The external standard method was used for quantitative analysis. Results The standard curves of amitraz and 2,4-dimethylaniline of honey additives showed a good linear relationship in the range of 2.0～500.0 ng/mL, and the correlation coefficient was more than 0.999. The limit of detection for amitraz and 2,4-dimethylaniline were 0.27 μg/kg and 0.42 μg/kg, respectively. The recovery rates of spiked amitraz and 2,4-dimethylaniline were99.6%～101.2% and 99.3%～101.6%, respectively. The relative standard deviations were less than 5%. Conclusion The method has the advantages of wide linear ragne, low detection limit, high sensitivity, high accuracy and good repeatability. It can meet the requirements for the determination of amitraz and 2,4-dimethylaniline in honey.更多还原