固相萃取逐步分离果蔬保鲜防腐剂噻苯咪唑、邻苯基苯酚残留检测的研究

The study of residue determination of preservatives thiabendazole,o-phenylphenol in fruits and vegetables by SPE-separation

目的建立固相萃取逐步分离测定果蔬中残留的噻苯咪唑、邻苯基苯酚的检测方法。方法样品经石油醚∶乙酸乙酯(2∶1)提取,30%甲醇溶液上样,C18固相柱富集、净化、分离2种残留防腐剂,分别采用30%乙醇-酸溶液(pH 2.5)、55%甲醇-碱溶液(pH 11.5)依次洗脱分离固相柱中被保留的噻苯咪唑、邻苯基苯酚,对洗脱液进行紫外分光光度法检测。结果这2种防腐剂在1～10μg/mL的范围内呈良好线性关系,相关系数r>0.999 2。样品加标回收率为83.3%～105.5%,相对标准偏差为1.2%～7.3%,最低检测限分别为0.09、1.0μg/mL。结论本方法适用于果蔬中残留防腐剂的检测。

Objective Thiabendazole, o-phenylphenol in residues of vegetables and fruits were determined by solid-phase extraction and UV-spectrophotometry. Methods： Samples were extracted under basic condi tions with petroleum ether： ethyl acetate（2 ： 1）. C18 was used for enrichment, purification and separation. 30% ethanol-acid solution （pH 2.5）, 55% methanol alkaline solution （pH 11. 5） were eluted thiaben dazole, o-phenylphenol, respectively and were determined by UV-spectrophotometry. Results The linearrange of each compound was 1～10μ/mL and the correlation coefficients was more than 0. 999 2. Recov-eries ranged from 83.3 to 105.5 %, with relative standard deviations of 1.2 to 7.3 %. The detection limits （S/N=3） were 0.09 μg/ml （TBZ）, 1.0 μz/mL （OPP）. Conclusion The method and spectrograph is suc-cessfully applied to residues of preservatives in fruits and vegetables.