摘要
建立气相色谱-质谱联用法同时测定茶叶中西玛津、莠去津、氟虫脲、百菌清、毒死蜱、喹硫磷6种农药残留的分析方法。样品粉碎后用乙腈提取,经Cleanert TPT萃取柱净化,旋蒸,正己烷定容。用气相色谱-质谱法,以选择离子模式检测,采用内标法进行定量。方法在20~1 500μg/L质量浓度范围内展示出良好的分离度,线性相关系数均大于0.998。检出限以3倍信噪比计算,西玛津、莠去津、氟虫脲、百菌清、毒死蜱、喹硫磷的检出限分别为0.000 95, 0.000 70, 0.005 1, 0.002 6, 0.001 4和0.001 7 mg/kg。在0.04~0.9 mg/kg的添加水平下,平均回收率在75.4%~114.6%,相对标准偏差(n=6)在0.3%~7.8%。结果表明,试验方法简单快速、分离度好、重现性好、精密度高,可满足同时检测茶叶中6种农药的要求。
A gas chromatography-mass spectrometry was established to simultaneously determine the residues of 6 pesticides including simazine, atrazine, fipronil, chlorothalonil, and chlorpyrifos in tea. The crushed samples were extracted with acetonitrile, purified by Cleanert TPT extraction column, rotary evaporation, and fixed to volume with n-hexane. The samples were analyzed by gas chromatography-mass spectrometry under selected ion mode, and quantitatively analyzed by internal standard method. The method showed good separation degree in the concentration range of 20-1 500 μg/L, and the linear correlation coefficient was greater than 0.998. According to S/N=3, the detection limit of simazine, atrazine, flufenoxuron, chlorhalonil, chlorpyrifos and quinalphos were 0.000 95, 0.000 70, 0.005 1, 0.002 6, 0.001 4, and 0.001 7 mg/kg, respectively. At the addition levels of 0.04-0.9 mg/kg, the average recoveries were in the rage of 75.4%-114.6%, and the relative standard deviation(n=6) was in the rage of 0.3%-7.8%. The results showed that the method was simple and fast, with good separation degree, good reproducibility and high precision. It could meet the requirements of simultaneous detection of these six pesticides in tea.
作者
刘伟悦
刘梦瑶
LIU Weiyue;LIU Mengyao(Beijing Zhangyiyuan Jinqiao Tea Co.,Ltd.,Beijing 101102)
出处
《食品工业》
CAS
2021年第7期327-330,共4页
The Food Industry
基金
北京张一元金桥茶叶有限公司立项(ZYYJQ2020001)。
关键词
气相色谱-质谱联用法
茶叶
快速检测
农药残留
gas chromatography-mass spectrometry usage
tea
rapid detection
pesticide residue
