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

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0.22μm滤膜,高效液相色谱仪分析。结果本方法测定7种组分在0~2.0μg/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。

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.