摘要
目的建立一种非衍生化前处理,亲水亲脂平衡柱(hydrophile-lipophile balance,HLB)净化结合液相色谱-串联质谱技术(liquid chromatography-tandem mass spectrometry,LC-MS/MS)测定茶叶中氯酞酸、茅草枯、草芽畏的检测方法。方法样品经20 mL 1%乙酸水+10 mL二氯甲烷提取,HLB(300 mg/3 mL)滤过净化,十八烷基硅烷(octadecylsilane,C18)色谱柱分离,液相色谱-串联质谱仪负离子模式测定,外标法定量检测。结果3种除草剂在色谱柱上分离良好,在0.01~2.00μg/mL范围内线性良好(r^(2)>0.998),在0.05、0.25、0.50和1.00 mg/kg 4个添加水平下,3种农药在茶叶空白基质中平均回收率为71.1%~119.2%,相对标准偏差为3.3%~18.3%。3种除草剂在茶叶中的检出限在0.002~0.009 mg/kg之间,定量限在0.008~0.029 mg/kg之间。结论该方法前处理简单快捷,无需衍生化,对检测人员和环境友好,可作为大批量检测茶叶中氯酞酸、茅草枯、草芽畏残留的方法。
Objective To establish a non-derivatized extraction method for the simultaneous determination of chlorthal-diacid,dalapon and trysben in tea by liquid chromatography-tandem mass spectrometry(LC-MS/MS)combined with hydrophile-lipophile balance(HLB)clean-up.Methods Tea samples were extracted by 20 mL of 1%acetic acid in water and 10 mL of methylene chloride;clean-up by HLB(300 mg/3 mL)filtration.Separation of the target analytes was achieved on an octadecylsilane(C18)chromatographic column,and quantitation was performed by LC-MS/MS in negative ion mode.Results The 3 kinds of herbicides were effectively separated on the C_(18) column with good linearity in the range of 0.01–2.00μg/mL(r^(2)>0.997).At 4 spiked levels of 0.05,0.25,0.50 and 1.00 mg/kg,the average recoveries of the 3 kinds of pesticides in the blank matrix of tea ranged from 71.1%to 119.2%,with the relative standard deviations between 3.3%and 18.3%.The limits of detection were ranged from 0.002–0.009 mg/kg,and the limits of quantitation were ranged from 0.008–0.029 mg/kg of the 3 kinds of herbicides.Conclusion The developed method offers a simple and rapid pretreatment procedure,eliminating the need for derivatization.It is friendly to the inspectors and the environment,and can be used as a method for large-scale detection of chlorthal-diacid,dalapon and trysben residues in tea.
作者
李霞雪
杨巧慧
郑云华
廖强
曾艳
杨树萍
LI Xia-Xue;YANG Qiao-Hui;ZHENG Yun-Hua;LIAO Qiang;ZENG Yan;YANG Shu-Ping(Ya’an Agricultural Products Quality Monitoring and Inspection Center,Ya’an 625000,China;Ya’an Quality Inspection and Testing Institute,Ya’an 625000,China;Ganzi Tibetan Autonomous Prefecture Agricultural Product Quality and Safety Center,Ganzi 626000,China)
出处
《食品安全质量检测学报》
2025年第11期146-153,共8页
Journal of Food Safety and Quality
基金
四川省市场监督管理局科技项目(SCSJS2023009)
四川省农产品质量安全风险监测项目(川农函[2024]98号)。
关键词
氯酞酸
茅草枯
草芽畏
茶叶
非衍生化
液相色谱-串联质谱法
chlorthal-diacid
dalapon
trysben
tea
non-derivatization
liquid chromatography-tandem mass spectrometry
