超声提取-分散固相萃取-气相色谱法测定绿茶中有机磷类农药残留
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(中粮营养健康研究院/北京市营养健康与食品安全重点实验室, 北京 100020)

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陈士恒,男,工程师,博士,主要从事农药残留分析方面的研究; *杨永坛,男,高级工程师,博士,主要从事色谱质谱联用技术在食品安全中的应用研究. 通讯作者.

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中粮集团应用基础研究项目(2013-C2-F013). 


Determination of 13 Organophosphorus Pesticides Residues in Green Tea by Ultrasonic Assisted Extraction-Dispersive Solid Phase Extraction-Gas Chromatography
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(COFCO Nutrition and Health Research Institute/Beijing Key Laboratory of Nutrition, Health and Food Safety, Beijing 100020, China)

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    摘要:

    应用超声辅助提取和分散固相萃取前处理方法结合气相色谱(配火焰光度检测器)建立了绿茶中13种有机磷类农药残留的快速分析方法. 5 g茶叶样品用20mL乙腈(含1%乙酸)超声辅助提取后,以石墨化炭黑与伯仲胺混合型固相分散净化,高速离心后氮吹浓缩复溶,过滤膜,用气相色谱-火焰光度检测器进行检测. 在0.02~0.10mg/kg的添加水平,13种有机磷农药的平均回收率是84.78%~116.72%,相对标准偏差是0.12%~9.32%,检出限是0.0008~0.01mg/kg. 本方法简便快速,准确性好,成本低,该方法已用于市面上销售的绿茶产品中有机磷类农药残留测定,结果均低于国家标准GB 2763—2012的最大残留量要求.

    Abstract:

    Gas chromatography (with a FPD detector) was applied to the quick determination of 13 organophosphorus pesticides residues in green tea with sample pretreatment by ultrasonic assisted extraction and dispersive solid phase extraction. The sample (5 g) was extracted with 20 mL acetonitrile(containing 1% acetic acid) by ultrasonic, and the extract was purified by dispersive solid-phase extraction with graphitized carbon/primary secondary amine (GCB/PSA). After the high speed centrifugation, nitrogen flushing concentration, and filtration, the sample was detected by GC-FPD. At the fortification level from 0.02-0.10mg/kg, the average recovery of 13 organophosphorus pesticides was 84.78%-116.72%. Meanwhile, the relative standard deviation (n=3) was from 0.12%-9.32% and the limits of detection was 0.0008-0.01mg/kg. The method was simple, rapid, accurate, and low-cost with few impurity disturbs and suitable for organophosphorus pesticides detection in green tea. This method was applied for the detection green teas in local markets, and the results of all organophosphorus pesticides were under the maximum residue limits of GB 2763—2012.

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陈士恒,章 晴,史晓梅,杨永坛.超声提取-分散固相萃取-气相色谱法测定绿茶中有机磷类农药残留[J].食品科学技术学报,2014,32(5):63-68.

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  • 收稿日期:2013-09-30
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  • 在线发布日期: 2014-11-06
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