快速溶剂萃取-高效液相色谱法测定蔬菜中啶虫脒残留量

HPLC Determination of Acetamiprid in Vegetables with Accelerated Solvent Extraction of Sample

摘要: 提出了高效液相色谱法测定蔬菜中啶虫脒残留量的方法。样品以甲醇为萃取溶剂经加速溶剂萃取仪在100℃静态萃取5 min,提取液浓缩后采用Dionex C18色谱柱分离,以甲醇-水(40+60)为流动相淋洗,于波长254 nm处测定。啶虫脒的质量浓度在0.01~0.2 g·L-1范围内与峰面积呈线性关系,方法的检出限(3S/N)为0.01 mg·kg-1。以蔬菜样品为基体,在5个浓度水平进行加标回收试验,啶虫脒的回收率在99.2%~101%之间,测定值的相对标准偏差(n=5)在1.3%~3.2%之间。

Abstract: A method of HPLC for the determination of acetamiprid in vegetables was proposed. The sample was extracted with methanol under static condition at 100 ℃ for 5 min by accelerated solvent extractor. The extract was concentrated and separated with Dionex C18 chromatographic column as stationary phase and the mixture of methanol-water (40+60) as mobile phase. UV-detection at 254 nm was used in the determination. Linear relationship between values of peak area and mass concentration of acetamiprid was obtained in the range of 0.01-0.2 g·L-1, with limit of detection (3S/N) of 0.01 mg·kg-1. Test for recovery was made by addition of standard acetamiprid at 5 concentration levels to vegetable samples as matrixes, values of recovery found were in the range of 99.2% to 101%. Values of RSD (n=5) found were in the range of 1.3%-3.2%.