Hu Bizhn, Song Weihua, Xie Lipin, Shao Tiefen
Shaoxing Entry-Exit Inspectian and Quarantine Bureau, Shaoxing 321000, China.
Se Pu. 2008 Jan;26(1):22-8.
A method has been developed for the determination of 33 pesticide residues in tea, including organophosphorous, organochlorine and pyrethroid pesticides. The target analytes were extracted with the solution of acetone/dichloromethane (1:1, v/v) using accelerated solvent extraction (ASE) and then purified using gel permeation chromatography (GPC) to eliminate most of the coextracts, such as pigments, lipids and waxes. They were further purified using Carb-NH2 and Florisil solid-phase extraction (SPE) cartridges prior to the identification using gas chromatography-mass spectrometry (GC-MS). The quantitative analysis was performed with flame photometric detector (FPD) for organophosphorous pesticides and electron capture detector (ECD) for organochlorine and pyrethroid pesticides. At the spiked level of 0.05 mg/kg, the recoveries for most pesticides were between 70%-120%; the relative standard deviations were less than 20%; the limits of detection varied from 0.005 to 0.05 mg/kg (defined in terms of 10 times of the baseline noise). This method is precise, sensitive and highly efficient in extraction. After routine applications, the results indicated that this method is suitable for the determination of pesticide residues in the tea for export.
已开发出一种用于测定茶叶中33种农药残留的方法,这些农药包括有机磷、有机氯和拟除虫菊酯类农药。目标分析物采用加速溶剂萃取(ASE),用丙酮/二氯甲烷(1:1,v/v)溶液进行萃取,然后使用凝胶渗透色谱(GPC)进行净化,以去除大部分共萃取物,如色素、脂质和蜡质。在使用气相色谱-质谱联用仪(GC-MS)进行鉴定之前,它们还需使用Carb-NH2和弗罗里硅土固相萃取(SPE)小柱进一步净化。有机磷农药的定量分析采用火焰光度检测器(FPD),有机氯和拟除虫菊酯类农药的定量分析采用电子捕获检测器(ECD)。在加标水平为0.05 mg/kg时,大多数农药的回收率在70%-120%之间;相对标准偏差小于20%;检测限在0.005至0.05 mg/kg之间(以基线噪声的10倍定义)。该方法在萃取方面精确、灵敏且高效。经过常规应用,结果表明该方法适用于出口茶叶中农药残留的测定。