凝胶渗透色谱净化-高效液相色谱法同时检测葡萄中多菌灵和噻菌灵残留

目的]建立同时检测葡萄中多菌灵和噻菌灵残留的高效液相色谱方法。方法]用乙腈从葡萄样品中提取多菌灵和噻菌灵,提取物先用凝胶渗透色谱（GPC）净化,然后采用高效液相色谱法-荧光检测器测定,外标法定量。对样品前处理和色谱分离条件进行了研究和优化。结果]2种杀菌剂在0.01～2.00μg/ml范围内线性良好,相关系数分别为0.9990和0.9996。添加2个浓度水平（0.1、0.4mg/kg）2种杀菌剂的在葡萄中的回收率均在90.3%～97.4%,相对标准偏差不大于2%。以3倍信噪比（S/N=3）确定该方法的检出限,多菌灵和噻菌灵分别为0.0035和0.0015mg/kg,均符合农药残留检测的常规要求。结论]该方法简便、快速、净化效果较好,可同时满足葡萄中2种杀菌剂残留的检验工作需要。

Determination of Carbendazim and Thiabendazole Residues in Grape by HPLC with Gel Permeation Chromatography Purification

Objective] The study aimed to establish the high performance liquid chromatography (HPLC) method for carbendazim and thiabendazole residues in Grape at same time. Method] Carbendazim and thiabendazole were extracted from the grape samples with acetonitrile. Extracts were first purified with gel permeation chromatography (GPC),and then were determined by HPLC-Gel permeation chromatography and quantified by the external standard method. The conditions of pretreatment and the chromatography separation were studied and optimized. Result] 2 bactericides had good linearity relation in the range of 0.01-2 ug/ml,with the correlation coefficient of 0.999 0 and 0.999 6. The average recoveries of 2 bactericides at two levels of 0.1 and 0.4 mg/kg ranged from 90.3% to 97.4% and the relative standard deviations were not greater than 2%.When the detection limit of this method was confirmed according to the Signal-to-Noise at 3 times (S/N=3),the carbendazim and thiabendazole were 0.003 5 and 0.001 5 mg/kg resp.,which could meet for the conventional requirements for the detection of the pesticide residue. Conclusion] The method was easier,faster and had better purification effect and it could meet the requirements for simultaneous determination of carbendazim and thiabendazole.