超高效液相色谱法同时测定蜂蜜中双甲脒及其代谢物残留量
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ACQUITY UPLC?BEH C18(2.1 mm×100 mm, 1.7 μm)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0.27 μg/kg, 2,4-二甲基苯胺为0.42 μg/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。
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 were 99.6%~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.
标题：超高效液相色谱法同时测定蜂蜜中双甲脒及其代谢物残留量
英文标题：Simultaneous determination of amitraz and its metabolite (2,4-dimethylaniline) residues in honey by ultra-performance liquid chromatography
作者：
谭璟慧 湖南省衡阳市疾病预防控制中心
谢宏斌 湖南省衡阳市疾病预防控制中心
李贵荣 南华大学公共卫生学院
陈静 湖南省衡阳市疾病预防控制中心
中文关键词:双甲脒,代谢物,2,4-二甲基苯胺,超高效液相色谱法,蜂蜜,
英文关键词:amitraz,metabolite,2,4-dimethylaniline,ultra-performance liquid chromatography,honey,
发表日期：2020-04-20
- 文件大小:
- 638.06 KB
- 下载次数:
- 60
-
高速下载
|
|
