气相色谱法测定蔬菜中倍硫磷、倍硫磷亚砜和 倍硫磷砜的残留量

Determination of fenthion, fenthion sulfoxide and fenthion sulfone residue in vegetables by gas chromatography

中文关键词:  气相色谱法  倍硫磷  倍硫磷亚砜  倍硫磷砜

英文关键词:gas chromatography  fenthion  fenthion sulfoxide  fenthion sulfone

中文摘要:

      目的 建立同时测定蔬菜中倍硫磷、倍硫磷亚砜和倍硫磷砜的气相色谱法。方法 样品经乙腈提取, 氯化钠分层后取有机相进行浓缩, 并置换溶剂成丙酮进行气相分析, 采用DB-5色谱柱, 载气流速1 mL/min, 程序升温条件为: 初始温度150 ℃, 保持2 min, 以8 ℃/min的速率升至200 ℃, 保持20min, 再以10 ℃/min的速率升至250 ℃, 保持8 min。结果 倍硫磷、倍硫磷亚砜和倍硫磷砜的分离度均大于1.5, 在0.02~4 μg/mL浓度范围内线性关系良好, 方法检出限在0.02~0.03 mg/kg之间, 3个不同浓度回收率为83.1%~118.2%。 结论 该方法灵敏度和精密度均满足实际样品检测需求, 可用于蔬菜中倍硫磷及其代谢物倍硫磷亚砜和倍硫磷砜的日常检测。

英文摘要:

      Objective To establish a method for simultaneous determination of fenthion, fenthion sulfoxide and fenthion sulfone residues in vegetables by gas chromatography. Methods The samples were extracted by acetonitrile, separated by sodium chloride, concentrated in organic phase, and the solvent was replaced by acetone, and then analyzed by gas chromatography. The temperature programmed conditions were as follows: the initial temperature was 150 ℃, keeping 2 min, rising to 200 ℃ at 8 ℃/min, keeping 20 min, then rising to 250 ℃ at 10 ℃ /min, keeping 8 min. Results The separation of parathion, parathion sulfoxide and parathion sulfone were all greater than 1.5. They had good relationships with the concentration of 0.02-4 μg/mL, and the limits of detection were 0.02-0.03 mg/kg. The recovery rates were 83.1%-118.2% at 3 spiked levels. Conclusion The sensitivity and precision of this method can meet the requirements of actual sample detection, which can be used for daily detection of fenthion, fenthion sulfoxide and fenthion sulfone residues in vegetables.