QuEChERS-高效液相色谱法同时测定苹果中7种苯甲酰脲类农药残留

Simultaneous determination of seven benzoylurea pesticides residues in apple by QuEChERS-high performance liquid chromatography

中文关键词:  QuEChERS  高效液相色谱法  苹果  苯甲酰脲

英文关键词:QuEChERS  high performance liquid chromatography  apple  benzoylurea

中文摘要:

      目的 建立QuEChERS-高效液相色谱法(high performance liquid chromatography, HPLC)同时测定苹果中7种苯甲酰脲类农药残留量的分析方法。方法 样品加1%冰乙酸-乙腈(冰乙酸:乙腈=1:99, 体积比)、氯化钠、无水乙酸钠、无水硫酸镁提取, 离心, 上清液经无水硫酸镁和N-丙基乙二胺(N-propylethylenediamine, PSA)净化后离心, 取上清液氮气吹干, 残渣经流动相溶解后, 过0.22 μm滤膜, 高效液相色谱仪分析。结果 本方法测定7种组分在0~2.0 μg/mL范围内具有良好的线性关系, 相关系数大于0.9995, 加标回收率为81.7%~116.9%, 相对标准偏差为0.10%~1.96%。检出限在0.007~0.020 mg/kg范围, 定量限在0.02~0.07 mg/kg范围。结论 该方法操作简单, 适合苹果中除虫脲、灭幼脲、杀铃脲、氟铃脲、氟苯脲、氟虫脲和氟啶脲的检测。

英文摘要:

      Objective To establish a method for the simultaneous determination of seven benzoylurea pesticide residues in apples by QuEChERS-high performance liquid chromatography (HPLC). Methods The samples were extracted by 1% glacial acetic acid-acetonitrile (glacial acetic acid: acetonitrile=1:99, volume ratio), sodium chloride, anhydrous sodium acetate, anhydrous magnesium sulfate, and centrifuged. The supernatant was purified by N-propylethylenediamine (PSA) and centrifuged. The supernatant was dried by nitrogen. The residue was dissolved by mobile phase and filtered through a 0.22 μm filter membrane and analyzed by HPLC. Results The linear relationship between the 7 components was observed in the range of 0?2.0 μg/mL with correlation coefficient higher than 0.9995. The average recoveries and relative standard deviations (RSDs) were in the range of 81.7%?116.9% and 0.10%?1.96%, respectively. The limits of detection and the limits of quantitative were in the range of 0.007?0.020 mg/kg and 0.02?0.07 mg/kg, respectively. Conclusion The method is simple, and which is suitable for determination of diflubenzuron, chlorbenzuron, triflumuron, hexaflumuron, flubenzuron, flufenozuron and chlorfluazuron in apple.