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

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%。

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

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.