高效液相色谱法同时测定果蔬中10种防腐杀菌剂

Simultaneous HPLC Determination of Ten Preservative Bactericides in Fruits and Vegetables

提出了高效液相色谱法同时测定果蔬中10种防腐杀菌剂（噻苯咪唑、邻苯基苯酚、联苯、对苯基苯酚、联苯醚、联苯胺、多菌灵、乙萘酚、乙氧基喹、抑霉唑）的方法。样品用乙酸乙酯超声萃取,所得有机相在40℃蒸发浓缩近干,残渣用甲醇溶解定容至5 mL,取20μL样品溶液注入高效液相色谱仪测定。采用ZORBAX Extend-C18柱作为固定相,并用不同比例的甲醇和pH 8.0的磷酸盐缓冲溶液作为流动相进行梯度淋洗,用紫外检测器检测。10种防腐杀菌剂的质量浓度分别在一定的范围内与其峰面积呈线性关系,方法的检出限（3S/N）在0.02~0.05 mg.L-1之间。分别以蔬菜和水果为基体,加入标准溶液进行回收试验,10种防腐杀菌剂的回收率在79.5%~123.2%之间,相对标准偏差（n=6）在0.83%~4.71%之间。

A method of simultaneous HPLC determination of 10 preservative bactericides,namely,thiabendazole,o-phenylphenate,biphenyl,p-phenylphenol,diphenylether,benzidine,carbendazim 2-naphthalenol,ethoxyquin and imazalil in fruit and vegetable samples was proposed.The sample was extracted with ethylacetate,and the extract obtained was evaporated to dryness at 40 ℃ the residue was taken up with 5 mL of CH3OH.An aliquot of 20 μL was used for HPLC determination with UV detector.The ZORBAX Extend-C18 column was used as stationary phase and mixtures of methanol and pH 8.0 PBS with various ratios were used as mobile phase in gradient elution.Linear relationship between values of peak area and mass concentration of the 10 preservative bactericides were found in definite ranges,with values of detection limit（3S/N） ranged from 0.02-0.05 mg·L-1.On the base of samples of fruit and vegetable,test for recovery were made by standard addition method.Values of recovery and RSD′s（n=6） found were in the ranges of 79.5%-123.2% and 0.83%-4.71% respectively.