摘要
报道了用大口径毛细管气相色谱柱测定茶叶中三氯杀螨醇残留量的方法。用体积分数为20%的丙酮正己烷提取茶样中的三氯杀螨醇,采用微量化前处理方法,经弗罗里硅土酸性硅藻土混合柱净化后,与氢氧化钾溶液进行碱解,以大口径毛细管柱分离,艾氏剂为内标,电子捕获检测器(ECD)测定。经过对绿茶、红茶的添加回收试验,平均回收率为94%,变异系数小于7.49%,检测低限为0.5μgkg。
Dicofol residue is harmful to health. More and more countries have established the limitation of dicofol in foods.This paper describes an efficient method of determination for the dicofol residue in tea. The dicofol was extracted from the tea sample with 20% acetone hexane, cleaned up on a column of Florisil and acidic siliceous earth (sulfuric acid 0.3 mL/g) in series. Then the column was washed with 10 mL, 20% dichloromethane hexane, the flow rate was 1 mL/min. At last dicofol was hydrolyzed with potassium hydroxide solution, forming p,p′ dichlorobenzophenone(DBP), which was separated from other ingredients through wide\|bore capillary(LZ Ⅱ,25 m×0.53 mm i.d.) and determinated by gas chromatography with electron capture detector(ECD), using Aldrin as internal standard. When the mass ratio of dicofol was in the range of 0.05 3.0 mg/kg , the recoveries were 78% 104% and the limit of determination was 0.5 μg/kg. This method is simple, sensitive and suitable for pesticide residue analysis. It can also be applied to the determination of dicofol residues in other plant samples such as vegetables,fruits and so on.
出处
《色谱》
CAS
CSCD
北大核心
2000年第1期64-66,共3页
Chinese Journal of Chromatography
关键词
气相色谱法
三氯杀螨醇
杀螨剂
残留量
gas chromatography
wide\|bore capillary column
dicofol
tea
