快速滤过型净化结合气相色谱-串联质谱法同时检测茶叶中10种拟除虫菊酯农药残留

建立了快速滤过型净化(m-PFC)结合气相色谱-串联质谱(GC-MS/MS)测定茶叶中10种拟除虫菊酯类农药残留的方法。比较了采用不同提取溶剂(乙腈、丙酮和乙酸乙酯)和不同提取方式(不加水浸泡和加水浸泡)时10种农药的提取效率;比较了2种QuEChERS净化管和m-PFC柱对茶叶提取液的净化效果和农药残留的回收率。结果表明,茶叶样品不加水浸泡,用乙腈提取效果最好;m-PFC柱对茶叶提取液净化效果良好,而且能保证较高的农药回收率。10种拟除虫菊酯农药在相应的范围内有良好的线性关系,相关系数(R 2)大于0.9980;10种农药在4个水平添加下的回收率为87.5%~111.3%,RSD为2.1%~8.9%。方法的检出限为0.001~0.015 mg/kg,定量限为0.003~0.05 mg/kg。利用该方法检测市售50例茶叶样品中10种拟除虫菊酯农药的残留,检出率为48%,但农药残留量均在国家标准限量值以下。与传统QuEChERS法和固相萃取法相比,该方法具有操作简单、准确度和精密度良好等优点,为多种拟除虫菊酯类农药在茶叶中的残留测定提供了快速检测的新方法。

Determination of 10 pyrethroid pesticide residues in tea by gas chromatography-tandem mass spectrometry coupled with multi-plug filtration cleanup

A method for the determination of 10 pyrethroid pesticide residues in tea was established by multi-plug filtration cleanup (m-PFC) method combined with gas chromatography-tandem mass spectrometry (GC-MS/MS). Different extraction solvents (acetonitrile, acetone and ethyl acetate) and extraction methods (immersion without water and immersion with water) were compared. The effect of two kinds of QuEChERS pipes and m-PFC column on the purification of tea extracts and the pesticide recoveries were compared. The results showed that the tea samples could be extracted most efficiently when using acetonitrile without immersion in water. The m-PFC column had a good purification effect on the tea extract and could guarantee a high recovery rate. Good linear relationships were observed for the 10 pyrethroid pesticides, and the correlation coefficients (R²) were greater than0.9980. The average recoveries for the 10 pyrethroid pesticides were in the range of 87.5%-111.3% at four spiked levels, and the RSDs were in the range of 2.1%-8.9%. The LODs and LOQs were 0.001-0.015 mg/kg and 0.003-0.05 mg/kg, respectively. The method was applied to the determination of the 10 pyrethroid pesticides in 50 tea samples. The detection rate of the pyrethroid pesticides was 48%, but all the pesticide residues were below the national standard limits. Compared with the traditional QuEChERS and solid phase extraction methods, this method has the advantages of operational simplicity as well as high accuracy and good precision. The establishment of this method provides a new strategy for the rapid detection of pyrethroid pesticide residues in tea.