Xu Dunming, Lu Shengyu, Chen Dajie, Lan Jinchang, Zhang Zhigang, Yang Fang, Zhou Yu
Xiamen Entry-Exit Inspection and Quarantine Bureau, Xiamen 361026, China.
Se Pu. 2013 Mar;31(3):218-22. doi: 10.3724/sp.j.1123.2012.10003.
An effective method was developed and applied to determine the residues of ten pesticides of pyrazoles and pyrroles in tea by accelerated solvent extraction coupled with gas chromatography-tandem mass spectrometry (ASE-GC-MS/MS). The samples were extracted with ethyl acetate-hexane (1:1, v/v) for 5 min at 1.03 x 10(7) Pa and 100 degree C for one cycle. Then, they were purified by Envi-Carb/PSA column, and eluted by ethyl acetate-hexane (1:1, v/v). The analytes were determined by GC-MS/MS and quantified by external standard method. The limits of quantification were 0.003 mg/kg for fenpyroximate, 0.001 mg/kg for fipronil-sulfide, 0.002 mg/kg for fipronil, 0.005 mg/kg for fipronil-sulfone, 0.002 mg/kg for chlorfenapyr, 0.006 mg/kg for flusilazole, 0.001 mg/kg for difenzoquat, 0.001 mg/kg for pyraflufen-ethyl, 0.000 3 mg/kg for tebufenpyrad and 0.005 mg/kg for tolfenpyrad. The results show that the proposed method is sensitive and accurate for the determination of the ten pesticide residues.
建立了一种有效的方法,采用加速溶剂萃取-气相色谱-串联质谱法(ASE-GC-MS/MS)测定茶叶中10种吡唑类和吡咯类农药残留。样品用乙酸乙酯-正己烷(1:1,v/v)在1.03×10⁷ Pa和100℃下萃取5分钟,进行一个循环。然后,通过Envi-Carb/PSA柱净化,并用乙酸乙酯-正己烷(1:1,v/v)洗脱。采用GC-MS/MS测定分析物,外标法定量。唑螨酯的定量限为0.003 mg/kg,氟虫腈硫醚为0.001 mg/kg,氟虫腈为0.002 mg/kg,氟虫腈砜为0.005 mg/kg,氯虫苯甲酰胺为0.002 mg/kg,氟硅唑为0.006 mg/kg,敌草快为0.001 mg/kg,乙氧氟草醚为0.001 mg/kg,四螨嗪为0.000 3 mg/kg,唑虫酰胺为0.005 mg/kg。结果表明,该方法对10种农药残留的测定灵敏、准确。