高效液相色谱/安培检测法测定蜂蜜中苯酚残留量  

HPLC DETERMINATION OF RESIDUAL PHENOL IN HONEY WITH AMPEROMETRIC DETECTION

作　　者：方晓明 郭德华 王宝根 王爱娟 扬哲 

机构地区：[1]上海检验检疫局食品与动植物检验检疫技术中心,上海200135

出　　处：《理化检验（化学分册）》2003年第4期229-231,235,共4页Physical Testing and Chemical Analysis(Part B:Chemical Analysis)

摘　　要：研究了用高效液相色谱 /安培检测法测定蜂蜜中苯酚残留量。考察了试验参数对测定结果的影响。在所选试验条件下 ,苯酚保留时间约为 12min ,检出限为 2 .0ng·g- 1。三组不同水平的加样回收率为 91.6 10 1.9% ,相对标准偏差 2 .812 .8%。Residual phenol in honey sample was separated by distillation and purified on a small C 18 column. Phenol was then eluted from the column with methanol H 2O solution, and determined by HPLC with amperometric detection. HPLC conditions were optimized, to have the following parameters: ① specification of C 18 column was 150mm×4.6mm, 5μm; ② a mixture of 0.01mol·L -1 NaH 2PO 4 solution and 2mmol·L -1 EDTA solution in H 2O CH 3CN(4+1) was used as mobile phase after its acidity was adjusted to pH 4.0 with H 3PO 4; ③ flow rate: 0.9ml·min -1 ; ④ column temp: 17℃ and ⑤ sampling vol: 30μl. The amperometric detection was adopted because of its high sensitivity and selectivity, and only giving response to electro active substances. In the detection, glassy carbon electrode was used as working electrode, and the Ag/AgCl electrode as reference electrode. Potential of the working electrode was selected as 0.80V ( vs. Ag/AgCl electrode). Under the optimum conditions, the retention time of phenol was about 12min, and the limit of detection was 0.010μg·ml -1 , corresponding to 2.0ng·g -1 of sample. Recovery and precision tests were made at the concentration levels of 10, 100 and 500ng·g -1 . Results for recovery were in the range of 91.6% to 101.9% and for RSD were in the range of 2.8% to 12.8% respectively. The method has been checked with FI IR spectrometry, the result of which proved that the distillate collected was phenol. Analysis of 6 honey samples of different grades was performed using this method, and consistent results were obtained.

关 键 词：高效液相色谱 安培检测法 测定 蜂蜜 苯酚残留量 驱虫剂 

分 类 号：S896.1[农业科学—特种经济动物饲养] TS207.53[农业科学—畜牧兽医]