超声辅助-漂浮固化分散液液微萃取-气相色谱法测定茶叶中5种拟除虫菊酯类农药残留

高玉玲; 郭秀娟; 乔石; 孙鹏

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茶叶科学 ›› 2017, Vol. 37 ›› Issue (3) : 243-250.

超声辅助-漂浮固化分散液液微萃取-气相色谱法测定茶叶中5种拟除虫菊酯类农药残留

高玉玲^1,2, 郭秀娟³, 乔石³, 孙鹏^1,*

作者信息 +

Ultrasound-assisted Dispersive Liquid-liquid Microextraction Based on the Solidification of a Floating Organic Droplet Followed by Gas Chromatography for the Determination of Five Pyrethroid Pesticides in Tea Samples

GAO Yuling^1,2, GUO Xiujuan³, QIAO Shi³, SUN Peng^1,*

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摘要

建立了超声辅助-漂浮固化分散液液微萃取（UA-DLLME-SFO）-气相色谱法（GC）测定茶叶中甲氰菊酯、氟氯氰菊酯、氯氟氰菊酯、氰戊菊酯、溴氰菊酯5种拟除虫菊酯类农药残留的方法。获得最佳试验条件为20βμL十六烷（萃取剂）和800βμL丙酮（分散剂）,质量分数为4%的氯化钠,水相pH为4,35℃超声30βmin,–3℃、10β000βr·min^-1离心5βmin后,去除水相后经气相色谱测定。结果表明：在1~150βμg·kg^-1范围内,5种拟除虫菊酯类农药呈良好的线性关系,相关系数均大于0.9994,在1~5βμg·kg^-1添加水平下,平均回收率为92.3%~99.6%,日内相对标准偏差（RSD）均低于3.5%（n=6）,日间相对标准偏差（RSD）均低于5.9%（n=3）,5种农药在茶叶中的检出限为0.11~0.24βμg·kg^-1,定量限为0.36~0.81βμg·kg^-1。该方法操作简便、快速、安全、成本低、重现性好,适用于茶叶样品中拟除虫菊酯类农药残留的分析。

Abstract

A novel ultrasound-assisted dispersive liquid-liquid microextraction based on solidification of floating organic droplet method (UA-DLLME-SFO) which combined with gas chromatography coupled with ECD detector was developed for the determination of five pyrethroid pesticides (fenpropathrin, cyfluthrin, cyhalothrin, fenvalerate, deltamethrin) in tea. The optimal liquid-liquid microextraction experiment conditions were as follows: 20βμL hexadecane was used as extraction solvent. After ultrasound for 30 min under 35℃, 800βμL of acetone (disersive solvent) were rapidly transferred. The NaCl Mass Fraction was 4% and pH was adjusted to 4. The sample solution was then centrigugated at 10 000 r·min^-1 for 5 min under －3℃ and then injected for gas chromatography analysis. It was shown that a good linearity for these pyrethroids was obtained at concentrations of 1.0 to 150.0 μg·kg^-1 with correlation coefficients higher than 0.9994. The average recoveries of the 5 pesticides in liquid milk were in the range of 92.3% to 99.6% at spiked levels between 1 to 5 μg·kg^-1, with intra-day relative standard deviations lower than 3.5%（n=6）and inter-day relative standard deviations lower than 5.9% (n=3). The limits of detection and quantification were 0.11-0.24 μg·kg^-1 and 0.36-0.81 μg·kg^-1 , respectively. The proposed method is simple, fast, safe, reliable and applicable for analyzing pyrethroid pesticides in tea samples.

导出引用

高玉玲, 郭秀娟, 乔石, 孙鹏. 超声辅助-漂浮固化分散液液微萃取-气相色谱法测定茶叶中5种拟除虫菊酯类农药残留[J]. 茶叶科学. 2017, 37(3): 243-250

GAO Yuling, GUO Xiujuan, QIAO Shi, SUN Peng. Ultrasound-assisted Dispersive Liquid-liquid Microextraction Based on the Solidification of a Floating Organic Droplet Followed by Gas Chromatography for the Determination of Five Pyrethroid Pesticides in Tea Samples[J]. Journal of Tea Science. 2017, 37(3): 243-250

中图分类号： TS272 S482

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