固相萃取-高效液相色谱法测定蔬菜中三唑酮、 百菌清和乙烯菌核利残留量

Determination of triadimefon, chlorthalonil and vinclozolin residues in vegetables by solid phase extraction-high performance liquid chromatography

中文关键词:  固相萃取  高效液相色谱法  蔬菜  三唑酮  百菌清  乙烯菌核利  残留量

英文关键词:solid phase extraction  high performance liquid chromatography  vegetable  triadimefon  chlorthalonil  vinclozolin  residue

中文摘要:

      目的 建立固相萃取-高效液相色谱-二极管阵列检测法测定蔬菜中三唑酮、百菌清和乙烯菌核利残留量的方法。方法 蔬菜样品用乙腈超声提取, 加入氯化钠进行盐析脱水, 提取液过中性氧化铝柱净化, 用正己烷/丙酮(90:10, V:V)淋洗液洗脱, 洗脱液水浴氮吹近干, 流动相定容后采用高效液相色谱法进行测定, 外标法定量。结果 三唑酮、百菌清和乙烯菌核利质量浓度在0.02~5.0 mg/L范围内与其峰面积呈良好的线性关系, 方法检出限为0.02 mg/kg, 加标回收率为89.5%~105.1%, 精密度(relative standard deviation, RSD)为0.85%~4.25%。结论 该方法操作简单、准确, 可应用于蔬菜中三唑酮、百菌清和乙烯菌核利的检测。

英文摘要:

      Objective To establish a method for the determination of triadimefon, chlorthalonil and vinclozolin residues in vegetables by solid phase extraction-high performance liquid chromatography (SPE-HPLC) with diode array detector (DAD). Methods Vegetable samples were extracted by ultrasonic with acetonitrile, then the extracts were dehydrated by sodium chloride salt-out, and were purified and concentrated on Alumina-N column with n-hexane/acetone (90:10, V:V) as eluant. The eluate was evaporated to dryness by nitrogen evaporator and the residues were diluted with mobile phase, which was used for HPLC analysis. External standard calibration was adopted in the determination. Results Linear relationship between values of peak area and mass concentration of chlorthalonil and triadimefon were good in the range of 0.02~5.0 mg/L. The limit of detection of this method was 0.02 mg/kg, with the recovery rate 89.5%~105.1% and relative standard deviation (RSD) 0.85%~4.25%. Conclusion This method is accurate and easy to operate, and it can be used for the determination of triadimefon, chlorthalonil and vinclozolin in vegetables.