食品科学

• 分析检测 • 上一篇    下一篇

QuEChERS法提取净化结合气-质联法快速检测茶叶中农药残留

叶江雷,金贵娥,吴云辉,郑文慧   

  1. 1.厦门海洋职业技术学院,福建 厦门 361102;2.厦门大学 近海海洋环境科学国家重点实验室,福建 厦门 361005;
    3.厦门茶叶进出口有限公司,福建 厦门 361006
  • 出版日期:2013-06-25 发布日期:2013-06-17

Rapid Determination of Pesticide Residues in Tea by QuEChERS and Gas Chromatography-Mass Spectrometry (GC-MS)

YE Jiang-lei,JIN Gui-e,WU Yun-hui,ZHENG Wen-hui   

  1. 1. Xiamen Ocean Vocational College, Xiamen 361102, China;2. State Key Laboratory of Marine Environmental Science, Xiamen University, Xiamen 361005, China;3. Xiamen Tea Import and Export Co. Ltd., Xiamen 361006, China
  • Online:2013-06-25 Published:2013-06-17

摘要:

建立分散固相萃取(QuEChERS)法提取净化结合气-质联用(GC-MS)技术检测茶叶中47种农药残留的方法。提取剂(2 mL乙腈、40mg NaCl)与干燥茶样(0.5g、20目)旋涡混合(2min)后离心(5000r/min、5min),吸取上清液(1mL)与净化剂(25mg PSA、7.5mg GCB、150mg MgSO4、40mg NaCl)旋涡混合(2min)后离心(5000r/min、5min),上清液直接注入气相色谱-质谱联用仪检测。通过对样品的颗粒度、数量,提取剂种类及数量,混合(旋涡)方式,净化剂数量等进行优化,方法的加标回收率在81%~102.2%之间,精密度在6.5%~18.3%之间,线性范围在0.00195~1.0mg/kg之间(R2>0.97),检测限在0.0009~0.0214mg/kg之间,定量限在0.0029~0.0712mg/kg之间,基本符合日本和欧盟对农残“一律标准”的要求。

关键词: 茶叶, 农药残留, 分散固相萃取, 气相色谱-质谱法

Abstract:

A method to determine 47 pesticide residues in tea using QuEChERS and GC-MS was established. For the
extraction of pesticide residues, dry samples were vortex-mixed with 40 mg of NaCl dissolved in 2 mL of MeCN and
centrifuged (5000 r/min for 5 min). Then 1 mL aliquot of the supernatant was taken and vortex-mixed for 2 min after the
addition of 25 mg of PSA, 7.5 mg of GCB, 150 mg of MgSO4 and 40 mg of NaCl and entrifuged (5000 r/min for 5 min).
The resulting supernatant was injected in to a GC-MS for analysis of pesticide residues. Under the optimized conditions of
particle size and amount of samples, extraction solvent type and volume and mixing method and purificant, the recovery of
the method for spiked samples ranged from 81% to 102.2%, and precision from 6.5% to 18.3% (RSD). The linear range was
0.00195-1.0 mg/kg (R2 > 0.97), limit of detection (LOD) 0.0009-0.0214 mg/kg, and limit of quantitation (LOQ) 0.0029-
0.0712 mg/kg. This method could substantially meet the “Uniform Limits” of Japan and the EU for analysis of pesticide
residues.

Key words: tea, pesticide residue, dispersive solid phase extraction, gas chromatography-mass spectrometry (GC-MS)