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[固相萃取-高效液相色谱法同时测定苹果中克菌丹和灭菌丹农药残留量]

[Simultaneous determination of captan and folpet pesticide residues in apples by solid-phase extraction and high performance liquid chromatography].

作者信息

Wang Shuju, Yu Yanbin, Tan Peigong, Miao Zaijing, Wei Yishan

机构信息

Ocean University of China, Qingdao 266003, China.

出版信息

Se Pu. 2007 Mar;25(2):226-9.

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. 999 9). 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.

摘要

建立了一种采用固相萃取和高效液相色谱法同时测定苹果中克菌丹和灭菌丹农药残留量的方法。样品用乙腈提取,并用自制吸附剂和硅胶的混合物净化,以正己烷 - 二氯甲烷 - 乙腈(50:49:1,v/v)作为洗脱剂。比较了使用弗罗里硅土柱、氨基柱和混合吸附剂的净化效果,结果表明混合吸附剂的效果最佳。最佳分析条件如下:以含0.1 mmol/L乙酸 - 乙酸盐缓冲液(pH 3.80)的甲醇 - 乙腈 - 水(50:5:45,v/v)为流动相,在210 nm波长处检测。该方法在0.40 - 8.00 mg/kg范围内对克菌丹和灭菌丹具有良好的线性关系(r > 0.999 9)。克菌丹和灭菌丹的检出限分别为0.27 mg/kg和0.20 mg/kg。保留时间的相对标准偏差(RSD)不超过0.60%。苹果中添加三个浓度水平的克菌丹和灭菌丹的平均回收率分别为69.3% - 106%和101% - 108%,RSD分别为3.7% - 4.7%和1.3% - 5.4%。

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