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建立固相萃取逐步分离-紫外分光光度法测定果蔬中残留的噻苯咪唑、邻苯基苯酚、联苯的检测方法。样品经高速涡轮旋转石油醚∶乙酸乙酯(2∶1)提取,30%甲醇溶液上样,C18固相萃取柱富集、净化、分离三种残留防腐剂,分别采用30%乙醇(酸,pH 2.5)溶液、55%甲醇(碱,pH 11.5)溶液、75%乙醇(酸,pH2.5)溶液依次洗脱分离固相柱中被保留的噻苯咪唑、邻苯基苯酚、联苯,对洗脱液进行紫外分光光度法检测。结果表明:三种防腐剂在1～10μg.mL-1的范围内呈良好线性关系,相关系数r>0.999 8。样品加标回收率为72.1%～103.5%,相对标准偏差在1.2%～7.7%,样品最低检测限分别为0.09,0.5和0.1μg.mL-1。该方法简便、灵敏、快速,能够满足同时测定果蔬中防腐剂残留量的要求。
A method for the determination of thiabendazole, o-phenylphenol and biphenyl residues in fruits and vegetables by UV-Vis spectrophotometry was developed. The samples were extracted with petroleum ether: ethyl acetate (2:1), 30% methanol solution and enriched with C18 solid phase extraction column. The three residual preservatives were purified and separated using 30% ethanol (acid, pH 2.5) solution, 55% methanol (base, pH 11.5) solution, 75% ethanol (acid, pH2.5) were sequentially eluted and separated from the solid phase column thiabendazole, o-phenylphenol, biphenyl, The eluate was detected by UV spectrophotometry. The results showed that there was a good linear relationship between the three preservatives in the range of 1 ~ 10μg.mL-1, the correlation coefficient r> 0.999 8. The recoveries of spiked samples ranged from 72.1% to 103.5% with relative standard deviations from 1.2% to 7.7%. The lowest detection limits were 0.09, 0.5 and 0.1 μg.mL-1 respectively. The method is simple, sensitive and rapid, and can meet the requirements of simultaneously determining the amount of preservative residues in fruits and vegetables.