色谱

色谱

• 研究论文 • 上一篇    下一篇

固相萃取-高效液相色谱法同时测定苹果中残留的克菌丹和灭菌丹

王淑菊1,于彦彬2,谭培功3,苗在京2,魏亦山2   

  1. 1.Ocean University of China, Qingdao 266003, China; 2.Ministry of Agriculture Supervision and Test Center for Agriculture Products Quality (Qingdao), Qingdao 266109, China; 3.Qingdao Environmental Monitoring Center, Qingdao 266003, China
  • 收稿日期:2006-08-21 修回日期:2006-12-28 出版日期:2007-03-30 发布日期:1985-12-25
  • 通讯作者: 谭培功

Simultaneous Determination of Captan and Folpet Pesticide Residues in Apples by Solid-Phase Extraction and High Performance Liquid Chromatography

WANG Shuju1, YU Yanbin2, TAN Peigong3, MIAO Zaijing2, WEI Yishan2   

  1. 1.Ocean University of China, Qingdao 266003, China; 2.Ministry of Agriculture Supervision and Test Center for Agriculture Products Quality (Qingdao), Qingdao 266109, China; 3.Qingdao Environmental Monitoring Center, Qingdao 266003, China
  • Received:2006-08-21 Revised:2006-12-28 Online:2007-03-30 Published:1985-12-25
  • Contact: TAN Peigong

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摘要： 采用硅镁吸附剂和硅胶作吸附剂,建立了固相萃取-高效液相色谱法同时测定苹果中残留的克菌丹和灭菌丹的分析方法。研究了甲醇-乙腈-水(含0.1 mmol/L乙酸-乙酸钠缓冲溶液（pH 3.80）)三元体系下克菌丹和灭菌丹的最佳分离条件,在波长210 nm下检测,克菌丹和灭菌丹的线性范围为0.40～8.00 mg/kg，线性相关系数均大于0.9999；最低检出限克菌丹为0.27 mg/kg、灭菌丹为0.20 mg/kg；保留时间的相对标准偏差（RSD）≤0.60%。苹果样品中3个添加水平的平均加标回收率为克菌丹69.3%～106%,RSD为3.7%～4.7%；灭菌丹101%～108%,RSD为1.3%～5.4%。

关键词: 高效液相色谱法, 固相萃取, 硅胶, 国产吸附剂, 混合吸附剂, 克菌丹, 灭菌丹, 苹果

Abstract: A method for the simultaneous determination of captan and folpet pesticide residues in apples was developed by solid-phase extraction and high performance liquid chromatography. The sample was extracted with acetonitrile and cleaned-up by a mixture of homemade sorbent and silica gel with hexane-dichloromethane-acetonitrile (50∶49∶1, v/v) as the eluent. The cleaned effects by using Florisil column, amino column, the mixed sorbent were compared, and the effect of the mixed sorbent was the best. The optimal analytical conditions were follow as: an methanol-acetonitrile-water (50∶5∶45, v/v) containing 0.1 mmol/L acetic-acetate buffer (pH 3.80) as the mobile phase, detection at 210 nm. The method had a good linear relationship in the range of 0.40-8.00 mg/kg for captan and folpet (r＞0.9999). The detection limits of captan and folpet were 0.27 mg/kg and 0.20 mg/kg, respectively. The relative standard deviations (RSDs) of retention time were no more than 0.60%. The average recoveries of captan and folpet from the apples spiked at three levels ranged from 69.3%-106% and 101%-108%, with RSD of 3.7%-4.7% and 1.3%-5.4%, respectively.

Key words: apple , captan, folpet, high performance liquid chromatography (HPLC), homemade sorbent, mixed sorbent, silica gel, solid-phase extraction