分散固相萃取—高效液相色谱法测定水果中多菌灵和噻菌灵

Determination of residues of carbendazim and thiabendazole pesticides in fruits by dispersive solid—phase extraction (dispersive SPE) and HPLC

分析了现行苯并咪唑类农药残留检测方法中存在的问题,并对分散固相萃取—高效液相色谱法检测苯并咪唑类农药残留方法进行了研究。通过对方法的条件进行优化、改进,获得高效、快捷、经济的前处理方法,成功建立了分散固相萃取—高效液相色谱法。其中使用C18和PSA吸附剂组合将多菌灵的回收率由文献中大于110%降到91.8%～104.7%,噻菌灵的回收率由文献中的17%～44%提高到88%～102%,满足了要求。在苹果、香蕉、桃、柑橘、葡萄、草莓6种水果上进行方法验证,研究结果表明,农药浓度在0.01～3.0mg/kg内呈良好的线性关系,线性相关系数在0.999以上,平均回收率在88%～104.7%,方法的RSD值小于5%。方法的准确度和精密度都满足要求,为相关标准的制定提供了依据。

Based on analyzing the problems of the methods for examining the residue of benzimidazole pesticides including carbendazim and thiabendazole, a fast, effective, economic, precise, accurate dispersive solid-phase （dispersive SPE）extraction and HPLC analytical method has been developed for the qualitative and quantitative determination of carbendazim and thiabendazole residues and supplied the basis of enacting relative standards. The compound of dispersive sorbent PSA and C18 was studied for amending the method. It reduced the carbendazim recovery rate from 110% to 91.8% to 104.7% and heightened the thiabendazole recovery rate from 17% to 44% to 88% to 102%. The procedure was improved and linearity,precision, accuracy, limits of detection and recovery of the method were determined. Regression analyses for the pesticides were linear at concentrations ranging from 0.01 mg/kg to 3.0 mg/kg showing correlation coefficient greater than 0.999. And recoveries for two fortified pesticides in six types of fruits were between 90.7% to 104.7% with relative standard deviation of 〈5%.