气相色谱-四极杆/飞行时间质谱法非靶向快速筛查凉茶中的农药残留
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(广州海关技术中心 广州 510623)

作者简介:

曾广丰(1988—),男,学士,工程师

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基金项目:

广州海关科技计划项目(2018GDK13);广州市科技计划项目(202002030214)


Non-target Screening of Pesticide Residues in Herbal Tea by Gas Chromatography-Quadrupole-Time of Flight Mass Spectrometry
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(Guangzhou Customs Technology Center, Guangzhou 510623)

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    摘要:

    为建立QuEChERS法净化,结合气相色谱-四极杆-飞行时间质谱法(QuEChERS/GC-Q-TOF/MS)非靶向快速筛查凉茶中农药残留的方法,将样品经乙酸乙酯提取,石墨化炭黑(GCB)和氨丙基粉(NH2)分散固相萃取净化,GC-Q-TOF/MS测定。利用20种质控化合物建立的筛查方法检出限范围为2.00~50.0 μg/kg,定量限范围5.00~150 μg/kg。3个不同加标水平(25,50,125 μg/kg)下的平均回收率为73.47%~106.3%,相对标准偏差为0.91%~9.11%(n=6)。在该定量方法基础上利用目标化合物特征离子的精确质量数、二级碎片丰度比、主要离子碎片的同位素丰度比等信息进行精确质量数据库筛查与确证,以数据库检索匹配得分≥80的最低浓度作为方法的筛查限,无标准品情况下实现了非靶向筛查凉茶中751种农药残留。方法快速、准确、分析通量高,可为凉茶中农药残留的非靶向快速筛查和质量控制提供重要依据。

    Abstract:

    A method for rapid screening of pesticide residues in herbal tea by gas chromatography coupled with quadrupole time-of-flight mass spectrometry (GC-Q-TOF/MS) was developed. The target compounds in samples were extracted by ethyl acetate, cleaned by GCB and NH2 sorbent and determined by GC-Q-TOF/MS. The detection limits of 20 controlled pesticides were within 2.00-50.0 μg/kg and the limits of quantitation were 5.0-150 μg/kg. The average recovery of the sample ranged from 73.47%-106.3% at three different spiked levels(25, 50, 125 μg/kg), with RSDs (n=6) of 0.91%-9.11%. Moreover, the acquired data was compared with the library using the accurate mass of characteristic ion, ratio of product ion and isotopic distribution of characteristic ion to screen pesticide residues in herbal tea. Screening and confirmation was achieved by library search, and the minimum concentration with a score(≥80) was used as the screening limit of the method without reference standards. This method is high efficiency, sensitive and accuracy, and can meet the requirement for non-target rapid screening of pesticide residues in herbal tea.

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曾广丰,谢建军,王志元,叶远志,李菊,侯颖烨,王璐.气相色谱-四极杆/飞行时间质谱法非靶向快速筛查凉茶中的农药残留[J].中国食品学报,2022,22(5):338-347

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  • 收稿日期:2021-05-17
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  • 在线发布日期: 2022-06-15
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