色谱

色谱 ›› 2013, Vol. 31 ›› Issue (4): 372-379.DOI: 10.3724/SP.J.1123.2012.01034

• 研究论文 • 上一篇    下一篇

液相色谱-四极杆/ 飞行时间质谱快速筛查与确证苹果、番茄和甘蓝中的281种农药残留

赵志远1,2,石志红1,康健2,3,彭兴2,4,曹新悦2,5, 范春林2*,庞国芳2,吕美玲6   

  1. 1. 河北大学化学与环境科学学院, 河北 保定 071002;2. 中国检验检疫科学研究院, 北京 100123;
    3. 燕山大学环境与化学工程学院, 河北 秦皇岛 066004;4. 北京工商大学食品学院, 北京 100048;
    5. 山东农业大学食品科学与工程学院, 山东 泰安 271018;6. 安捷伦科技(中国)有限公司, 北京 100102
  • 收稿日期:2013-01-17 出版日期:2013-04-22 发布日期:2013-04-24
  • 通讯作者: Tel:(010)85783526,E-mail:caiqfcl@yahoo.cn
  • 基金资助:

    “十二五”国家科技支撑项目(2012BAD29B01).

Rapid screening and confirmation of 281 pesticide residues in apples, tomatos and cabbages by liquid chromatography/quadrupole time-of-flight mass spectrometry

ZHAO Zhiyuan1,2, SHI Zhihong1, KANG Jian2,3, PENG Xing2,4, CAO Xinyue2,5, FAN Chunlin2*, PANG Guofang2, L Meiling6   

  1. 1. College of Chemistry and Environmental Science, Hebei University, Baoding 071002, China; 2. Chinese Academy of Inspection and Quarantine, Beijing 100123, China; 3. College of Environment and Chemical Engineering, Yanshan University, Qinhuangdao 066004, China; 4. College of Food and Chemical Engineering, Beijing Technology and Business University, Beijing 100048, China; 5. College of Food Science and Engineering, Shandong Agricultural University, Taian 271018, China; 6. Agilent Technologies (China) Limited, Beijing 100102, China
  • Received:2013-01-17 Online:2013-04-22 Published:2013-04-24

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摘要：

建立了苹果、番茄和甘蓝中281种农药残留的QuEChERS结合液相色谱-四极杆/飞行时间质谱(LC-Q-TOF/MS)快速筛查方法。方法采用1%醋酸乙腈提取样品,经丙基乙二胺(PSA)净化,LC-Q-TOF/MS测定。281种农药在苹果、番茄和甘蓝中3个添加水平下的回收率在70%～120%范围的比例分别为98.6%、99.3%和98.2%;回收率的相对标准偏差(RSD)均≤20%(n=5);在0.25～10倍最大残留限量(MRL)的含量范围内,线性相关系数r2≥0.99的农药比例分别为95.7%、96.1%和98.2%;检出限分别为0.03～4.47、0.01～4.49和0.02～3.61 μg/kg。本方法采用精确质量数据库和谱图库检索的方式,实现了不用农药标准品对照而完成对果蔬中农药残留的快速筛查,提高了定性鉴别的准确性。应用所建立的方法对30个市售果蔬样品进行筛查,共检出13种农药残留。其中,甘蓝中甲胺磷的含量超过了GB 2763-2012《食品安全国家标准\5食品中农药最大残留限量》和欧盟的MRL;番茄中鱼藤酮的含量超出欧盟的MRL。

关键词: QuEChERS, 多残留, 果蔬, 农药, 数据库检索, 液相色谱-四极杆/飞行时间质谱

Abstract:

The application of QuEChERS coupled to liquid chromatography/quadrupole time-of-flight mass spectrometry (LC-Q-TOF/MS) for screening 281 pesticide residues in apples, tomatos, and cabbages has been investigated. The established method includes the extraction by acetonitrile/acetic acid (99∶1, v/v), and clean-up by primary secondary amine (PSA) sorbent. The resultant residues were further analyzed by LC-Q-TOF/MS. For apples, tomatos, and cabbages, the percentages of pesticides with the average recoveries (n=5) in the range of 70%-120% were 98.6%, 99.3%, and 98.2%, respectively; and the relative standard deviations (RSDs) for the recoveries were not more than 20%; in the concentration range of 0.25-10 MRL, the percentages of the pesticides with the correlation coefficients (r2) greater than 0.99 were 95.7%, 96.1%, and 98.2%, respectively; the LODs were 0.03-4.47 μg/kg, 0.01-4.49 μg/kg and 0.02-3.61 μg/kg, respectively. Rapid screening and confirmation can be achieved with accurate mass database and library search without the standard compounds. The method has been applied to 30 fruit and vegetable samples randomly purchased from the local markets, and the 13 pesticides were detected. It was found that the level of methamidophos in one cabbage sample exceeded the MRL regulated by China of GB 2763-2012 and the MRL regulated by European Union (EU), and the level of rotenone in one tomato sample exceeded the MRL regulated by EU.

Key words: database search, fruits and vegetables, liquid chromatography/quadrupole time-of-flight mass spectrometry (LC-Q-TOF/MS), multi-residues, pesticides, QuEChERS

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