Pang G F, Fan C L, Chao Y Z, Zhao T S
Qin Huangdao Import and Export Commodity Inspection Bureau, Hebei, China.
J Chromatogr A. 1994 Apr 29;667(1-2):348-53. doi: 10.1016/0021-9673(94)89087-0.
A rapid and economical simplified multi-residue method is described for the determination of multiple pyrethroid insecticides in fruits and vegetables. The residues are extracted from crops with methanol and the crop co-extractives are removed by toluene partitioning and Florisil-charcoal minicolumn chromatography. The final extract is analysed by capillary column gas chromatography with electron-capture detection. The recoveries were determined by fortifying six different crops (apples, oranges, cabbages, pears, peppers and tomatoes) with eleven pyrethroids (Py-115, allethrin, biphenthrin, fenpropathrin, cyhalothrin, permethrin, cyfluthrin, flucythrinate, fluvalinate, fenvalerate and deltamethrin) at three levels, 0.01-0.07, 0.10-0.70 and 1.0-7.0 mg/kg. Three determinations were made at each level for each crop. Recoveries of the eleven pyrethroids ranged from 70.4 to 110.0% at the three different levels. The practical determination limit of the method was in the range 3.0-30.0 micrograms/kg for all the pyrethroid insecticides. The proposed method had major advantages that simplified steps were achieved for the extraction and the clean-up, the solvent consumption was reduced and the analysis time was shortened.
描述了一种快速且经济的简化多残留方法，用于测定水果和蔬菜中的多种拟除虫菊酯类杀虫剂。用甲醇从作物中提取残留物，并通过甲苯分配和弗罗里硅土 - 活性炭微柱色谱法去除作物共提取物。最终提取物通过带有电子捕获检测的毛细管柱气相色谱法进行分析。通过在六种不同作物（苹果、橙子、卷心菜、梨、辣椒和西红柿）中添加十一种拟除虫菊酯（Py - 115、丙烯菊酯、联苯菊酯、甲氰菊酯、氯氟氰菊酯、氯菊酯、氟氯氰菊酯、氟氰戊菊酯、氟胺氰菊酯、氰戊菊酯和溴氰菊酯），添加水平为0.01 - 0.07、0.10 - 0.70和1.0 - 7.0 mg/kg，来测定回收率。每种作物在每个水平下进行三次测定。在三个不同水平下，十一种拟除虫菊酯的回收率在70.4%至110.0%之间。该方法对所有拟除虫菊酯类杀虫剂的实际测定限在3.0 - 30.0微克/千克范围内。所提出的方法具有主要优点，即简化了提取和净化步骤，减少了溶剂消耗并缩短了分析时间。
