固相微萃取-气相色谱-串联质谱法测定蜂蜜中双甲脒及其代谢产物残留

Simutaneous determination of amitraz and its metabolite 2,4-dimethylaniline in honey by solid-phase microextraction coupled with gas chromatography-tandem mass spectrometry

建立了同时测定蜂蜜中的双甲脒及其代谢产物2,4-二甲基苯胺残留量的固相微萃取-气相色谱-串联质谱法。对固相微萃取的实验条件（萃取纤维、萃取时间、p H值等）进行了选择和优化,并建立了气相色谱-串联质谱（GC-MS/MS）的仪器检测方法。结果表明：在优化的实验条件下,双甲脒和2,4-二甲基苯胺的最低检出限分别为0.5μg/kg和3.0μg/kg;在0.01~1.0 mg/kg的浓度范围内,二者的添加回收率范围分别为81.9%~98.2%和75.5%~90.6%,相对标准偏差分别为5.0%~15.4%和7.9%~17.2%。该方法操作简便、灵敏度高、准确可靠,适用于蜂蜜中双甲脒及2,4-二甲基苯胺的检测。

A method was developed for simutaneous determination of amitraz and its metabolite 2,4-dimethylaniline（ DMA） in honey by solid-phase microextraction（ SPME） coupled with gas chromatography-tandem mass spectrometry（ GC-MS / MS）. The SPME conditions（ fiber selection,extraction time,p H,etc.） were optimized,and the GC-MS / MS method was established. The limits of detection for amitraz and DMA were 0. 5 μg / kg and 3. 0 μg / kg,respectively. In the linearity range of 0. 01 ~ 1. 0 mg / kg,the spiked recoveries for amitraz were in the range of 81. 9% ~ 98. 2%,and the relative standard deviations（ RSDs） were in the range of 5.0% ~ 15. 4%; the spiked recoveries for DMA were 75. 5% ~ 90. 6%,and the RSDs ranged from 7. 9% to 17. 2%. The proposed method was validated to be simple,sensitive and accurate. It can be used for the determination of amitraz and DMA in honey.