多壁碳纳米管固相萃取/超高效液相色谱-串联质谱测定烤烟中粉唑醇残留量

Determination of flutriafol residue in flue-cured tobacco by multi-wall carbon nanotubes solid phase extraction/ultra performance liquid chromatography-tandem mass spectrometry

中文关键词:  多壁碳纳米管  烤烟  粉唑醇  超高效液相色谱-串联质谱法

英文关键词:multi-walled carbon nanotubes  flue-cured tobacco  flutriafol  ultra performance liquid chr omatography-tandem mass spectrometry

中文摘要:

      目的 建立多壁碳纳米管固相萃取净化结合超高效液相色谱-串联质谱法(Ultra performance liquid chromatography-tandem mass spectrometry, UPLC-MS/MS)测定烤烟中粉唑醇残留量的方法。方法 烤烟样品用0.1%甲酸乙腈溶液提取, NaCl盐析, 多壁碳纳米管(MS-NANO-V)净化, 并采用超高效液相色谱-串联质谱法检测, 以0.1%甲酸水溶液-甲醇溶液作为流动相, 外标法定量。结果 粉唑醇在0.001~1 mg/L浓度范围内的相关系数为0.9989, 呈现良好的线性关系。在0.005、0.5、5 mg/kg 3个添加水平下, 粉唑醇在烤烟中的平均回收率范围为90%~102%, 相对标准偏差范围为4.9%~9.6%。方法的定量限为0.005 mg/kg。结论 该方法高效、准确, 操作简便、精密度好, 适用于烤烟中粉唑醇残留量的检测。

英文摘要:

      Objective To establish a method for the determination of flutriafol residue in flue-cured tobacco by multi-walled carbon nanotubes solid-phase extraction combined with ultra performance liquid chromatog raphy-tandem mass spectrometry (UPLC-MS/MS). Methods The samples were extracted with 0.1% formic acid and acetonitrile solution, then salted out with NaCl, purified with multi-walled carbon nanotubes (MS-NANO-V), and detected by UPLC-MS/MS. The mobile phase was 0.1% formic acid solution–methanol, and the contents were quantified by external standard method. Results Flutriafol had good linear relationships in the range of 0.001? 1.0 mg/L, and the correlation coefficient was 0.9989. The average recoveries of flutriafol in flue-cured tobacco were 90%?102% with the 3 spiked levels of 0.005、0.5 and 5 mg/kg, the relative standard deviations were 4.9%?9.6%. The limit of quantification was 0.005 mg/kg. Conclusion The method is efficient, accurate, simple and precise, and is suitable for the determination of residual powder azolidol in flue-cured tobacco.