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食品与发酵工业  2019, Vol. 45 Issue (19): 239-250    DOI: 10.13995/j.cnki.11-1802/ts.021094
  分析与检测 本期目录 | 过刊浏览 | 高级检索 |
QuEChERS-超高效液相色谱-飞行时间质谱法快速筛查蔬菜中154种农药残留
李建勋1, 范蓓1, 周杰2, 甄云鹏3, 单吉浩1,*
1(农业农村部农产品质量安全收贮运管控重点实验室,中国农业科学院农产品加工研究所,北京,100193)
2(河北冠卓检测科技股份有限公司,河北 石家庄,050000)
3(沃特世科技(上海)有限公司,上海,100026)
Rapid screening of 154 pesticide residues in vegetables by QuEChERS-ultra high performance liquid chromatography-time mass spectrometry
LI Jianxun1, FAN Bei1, ZHOU Jie2, ZHEN Yunpeng3, SHAN Jihao1,*
1(Key Laboratory of Agro-products Quality and Safety Control in Storage and Transport Process, Ministry of Agriculture and Rural Affairs, Institute of Food Science and Technology, Chinese Academy of Agricultural Sciences,Beijing 100193, China)
2(Hebei Guanzhuo Testing Technology Co., Ltd, Shijiazhuang 050000, China)
3(Waters Technologies (Shanghai) Limited, Shanghai 100026, China)
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摘要 利用超高效液相色谱-四极杆-飞行时间质谱(ultra-performance liquid chromatography-quadrupole-time-of-flight-mass spectrometry, UPLC-Q-TOF/MS)技术建立了快速筛查芹菜和西红柿中154种农药多残留的新方法。采用QuEChERS方法进行样品前处理,样品经含1%(体积分数)乙酸乙腈溶液提取,同时加入MgSO4和NaCl盐析,提取液经填料净化后直接测定。目标药物经ACQUITY UPLC TMBEH C18柱分离,以乙腈和0.1%(体积分数)甲酸水溶液为流动相进行梯度洗脱,采用正离子全信息串联质谱扫描模式(MSE)进行检测。结果表明,2种蔬菜中154种农药在1~100 μg/kg呈良好的线性相关性(R2≥0.995);154种农药的筛查限(SDLs)为1~100 μg/kg,定量限(LOQs)为1~100 μg/kg;3个加标水平的平均回收率为52%~127%,相对标准偏差为0.3%~39.0%。该方法快速简便、灵敏度较高,可用于芹菜和西红柿中154种农药多残留的快速筛查。
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李建勋
范蓓
周杰
甄云鹏
单吉浩
关键词:  蔬菜  QuEChERS  超高效液相色谱-四极杆-飞行时间质谱(UPLC-Q-TOF/MS)  农药残留    
Abstract: A new method for screening 154 pesticide residues in celery and tomato was established by UPLC-Q-TOF/MS. The QuEChERS method was used for sample preparation, and the sample was extracted with acetonitrile solution containing 1% (V/V) acetic acid and salted out with anhydrous magnesium sulfate and sodium chloride. The extract was purified by adsorption material and then determined directly. The target drug was separated by C18 column and gradient elution was performed with acetonitrile and 0.1% (V/V) formic acid aqueous solution as mobile phase. Full information tandem mass spectrometry (MSE) with positive ion was used to detect the target drug. The results showed that in the range of 1-100 μg/kg, the 154 pesticides in two vegetables showed good linear correlations (R2≥0.995), and the screening detection limits (SDLs) and limits of quantification (LOQs) of 154 pesticides in the two vegetables were both in the range of 1-100 μg/kg. The average recoveries for 154 pesticides at three spiked levels ranged from 52% to 127%, with relative standard deviations(RSDs) of 0.3%~39.0%. The method is rapid, simple and sensitive, which can be used for rapid screening of 154 pesticide residues in celery and tomato.
Key words:  vegetables    QuEChERS    UPLC-Q-TOF/MS    pesticide residues
     修回日期:  2019-06-20                发布日期:  2019-11-15      期的出版日期:  2019-10-15
基金资助: 农业农村部2019年国家农产品质量安全风险评估项目(GJFP2019015); 河北省重点研发计划大健康服务和生物医药专项项目(17274802D)
通讯作者:  博士,助理研究员(单吉浩副研究员为通讯作者,E-mail:shanjihao2007@163.com)。   
引用本文:    
李建勋,范蓓,周杰,等. QuEChERS-超高效液相色谱-飞行时间质谱法快速筛查蔬菜中154种农药残留[J]. 食品与发酵工业, 2019, 45(19): 239-250.
LI Jianxun,FAN Bei,ZHOU Jie,et al. Rapid screening of 154 pesticide residues in vegetables by QuEChERS-ultra high performance liquid chromatography-time mass spectrometry[J]. Food and Fermentation Industries, 2019, 45(19): 239-250.
链接本文:  
http://sf1970.cnif.cn/CN/10.13995/j.cnki.11-1802/ts.021094  或          http://sf1970.cnif.cn/CN/Y2019/V45/I19/239
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