摘要
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.
出处
《燕山大学学报》
CAS
北大核心
2016年第3期236-240,共5页
Journal of Yanshan University
基金
河北省自然科学基金资助项目(B2014203137)
燕山大学青年教师自主研究计划项目(13LGA014)
国家质检总局科技计划项目(2014IK091
2015IK094)