分散固相萃取结合气相色谱-四极杆-飞行时间质谱测定茶叶中13种三唑类农药残留
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(1.北京工商大学 食品与健康学院, 北京 100048;2.中国检验检疫科学研究院, 北京 100176)

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Determination of 13 Triazole Pesticide Residues in Tea by Dispersive Solid Phase Extraction Combined with Gas Chromatography- Quadrupole-Time of Flight Mass Spectrometry
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(1.School of Food and Chemical Engineering, Beijing Technology and Business University,Beijing 100048, China;2.Chinese Academy of Inspection and Quarantine,Beijing 100176,China)

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    摘要:

    建立同时测定茶叶中13种三唑类农药残留的气相色谱-四极杆-飞行时间质谱检测方法。样品采用体积分数1%醋酸乙腈为提取液,均质提取,提取液在含有多壁碳纳米、N-丙基乙二胺和石墨化炭黑3种净化填料的离心管中涡旋净化,正己烷定容,经VF-1701ms毛细管柱分离,在全扫描模式下采集,外标法定量。检测结果表明:实验方法检出限为1~50μg/kg,13种农药在10、50、100μg/kg的添加水平下,回收率在72%~110%,相对标准偏差≤18%(n=5),相关系数均大于0.995。建立的实验方法准确、灵敏,且节省溶剂、方便快速,可满足茶叶中13种三唑类农药残留的定性定量检测要求。

    Abstract:

    A method for simultaneous determination of 13 triazole pesticide residues in tea by gas chromatography-quadrupole-time of flight mass spectrometry was established. Samples were extracted homoge-neously with 1% (volume fraction ) acetonitrile acetate. The extracts were purified in a centrifugal tube containing three kinds of purification fillers:multi-walled carbon nano, N-propyl ethylenediamine, and graphitized carbon black. Capillary column VF-1701ms was used to collect the samples under the fullscan mode. Thirteen kinds of tea samples were quantified by the external standard method. The results showed that the detection limit of the experimental method was 1-50μg/kg. The recovery of 13 pesticides was 72%-110% at the levels of 10,0, and 100μg/kg. The relative standard deviation was less than 18% (n=5), and the correlation coefficient was greater than 0.995. The established method is accurate, sensitive, solvent-saving, convenient, and rapid, and can meet the qualitative and quantitative detection requirements of 13 triazole pesticide residues in tea.

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滕晓宇,李建勋,胡雪艳,庞国芳,范春林.分散固相萃取结合气相色谱-四极杆-飞行时间质谱测定茶叶中13种三唑类农药残留[J].食品科学技术学报,2019,37(5):103-110.

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  • 收稿日期:2019-01-15
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  • 在线发布日期: 2019-11-08
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