食品科学 ›› 2013, Vol. 34 ›› Issue (10): 169-172.doi: 10.7506/spkx1002-6630-201310036

• 分析检测 • 上一篇    下一篇

高效液相色谱法测定白葡萄汁中苯甲酰脲类农药

周建科,韩朝家,唐翠苓,付艳芳   

  1. 河北大学理化分析中心,河北省分析科学技术重点实验室,河北 保定 071002
  • 收稿日期:2012-03-17 修回日期:2013-03-29 出版日期:2013-05-25 发布日期:2013-05-07
  • 通讯作者: 周建科 E-mail:zhoujianke@yahoo.com.cn
  • 基金资助:

    国家计量基标准(化学部分)资源共享平台建设项目

Determination of Benzoylurea Insecticides in White Grape Juice by High Performance Liquid Chromatography

ZHOU Jian-ke,HAN Chao-jia,TANG Cui-ling,FU Yan-fang   

  1. Research Center of Physics and Chemistry Analysis, Key Laboratory of Analytical Science and Technology of Hebei Province, Hebei University, Baoding 071002, China
  • Received:2012-03-17 Revised:2013-03-29 Online:2013-05-25 Published:2013-05-07

摘要:

以二氯甲烷为萃取剂,甲醇为分散剂,采用分散液液微萃取-正相高效液相色谱法测定白葡萄汁中4种苯甲酰脲类农药(氟苯脲、杀铃脲、除虫脲、氟铃脲)。色谱条件:Apollo Silica柱;正己烷-无水乙醇(97:3,V/V)为流动相;流速:1.0mL/min;紫外检测波长:200nm。在0.33~100μg/mL范围内4组分线性良好,方法检出限在5.80~6.60ng/mL之间,平均回收率范围是73.72%~97.85%,相对标准偏差范围是1.33%~4.62%。该方法快速、检出限低、重现性好,可用于白葡萄汁中苯甲酰脲类农药的测定。

关键词: 高效液相色谱法, 苯甲酰脲, 液液分散微萃取, 白葡萄汁

Abstract:

Residues of benzoylurea insecticides (teflubenzuron, triflumuron, diflubenzuron and hexaflumuron) in white
grape juice were determined by dispersive liquid-liquid micro-extraction combined with normal-phase high performance
liquid chromatography. In the dispersive liquid-liquid micro-extraction, the extraction solvent was methylene chloride and
dispersive solvent was methanol. The analytes were separated on Apollo Silica column with a mobile phase made up of
n-hexane and anhydrous alcohol (97:3, V/V) at a flow rate of 1.0 mL/min and detected at 200 nm. Good linearity was found
in the range of 0.33 to 100 μg/mL with correlation coefficients above 0.999. The limits of detection were between 5.80 ng/mL and
6.60 ng/mL. The average recoveries of the benzoylurea insecticides ranged from 73.72% to 97.85%, with relative standard
deviations between 1.33% and 4.62%. The proposed method is rapid and highly reproducible and shows a limit of detection.
Therefore it is applicable for the determination of benzoylurea insecticide residues in white grape juice.

Key words: high performance liquid chromatography (HPLC), benzoylurea, dispersive liquid-liquid micro-extraction, white grape juice

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