QuEChERS-高效液相色谱法测定食品中溴硝醇残留量

QuEChERS-high performance liquid chromatography for determination of residue bronopol in foods

中文关键词:  高效液相色谱  QuEChERS  改性多壁碳纳米管  溴硝醇

英文关键词:high performance liquid chromatography  QuEChERS  modified multiwalled carbon nanotubes  bronopol

中文摘要:

      目的 建立QuEChERS-高效液相色谱法测定食品中溴硝醇残留量的分析方法。方法 前处理采用QuEChERS方法, 样品粉碎后用甲醇提取, 改性多壁碳纳米管净化, Agilent ZORBAX Eclipse XDB-C18色谱柱(250 mm×4.6 mm, 5 μm)对净化液进行分离, 以甲醇-乙腈(含0.1%磷酸)体系作为流动相, 210 nm波长下检测分析。结果 在优化实验条件下, 溴硝醇在0.02~10.00 μg/mL范围内具有良好的线性关系, 相关系数大于0.9999, 检出限(S/N=3)为0.050 mg/kg, 加标回收率为95.3%~104.0%, 相对标准偏差为4.2%~5.3%, 实际样品检测中均未检出溴硝醇。结论 该方法简单、快速、准确、灵敏度高, 可应用于粮食、水果和蔬菜中溴硝醇残留的快速检测。

英文摘要:

      Objective To establish a method for determination of bronopol residue in foods by QuEChERS-high performance liquid chromatography. Methods The QuEChERS method was adopted for pretreatment. The sample was extracted using methanol after crushing, and purificated by MWNTs, then separated by Agilent ZORBAX Eclipse XDB-C18 column (250 mm×4.6 mm, 5 μm) using a methanol acetonitrile (containing 0.1% phosphoric acid) system as mobile phase, and detected at 210 nm. Results Under the optimized experimental conditions, there was a good linear relationship in the range of 0.02–10.00 μg/mL, and the correlation coefficient was greater than 0.9999. The limit of detection (S/N=3) was 0.050 mg/kg, the recovery was 95.3%–104.0%, and the relative standard deviation was 4.2%–5.3%. No bromonitrosol was detected in the actual samples. Conclusion The method is simple, rapid, accurate and sensitive, and can be applied to the rapid detection of bromonitol residues in grain, fruits and vegetables.