Determination of organophosphorous pesticides in cider by GC-MS coupled with cloud point extraction
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摘要: 本文对苹果汁中45种有机磷类农药的提取、净化技术和气相色谱质谱检测条件进行了研究。以苹果汁为基质材料,45种有机磷类农药在1、5、10μg/L三个水平上对苹果汁进行添加回收率实验。结果表明:45种有机磷类目标物在优化条件下的回收率为71.16%~117.94%,相对标准偏差1.20%~15.13%(n=5),方法检出限为0.01~0.22μg/L。45种有机磷类农药能够实现很好的分离,线性范围在10~2000μg/L,线性相关系数大于0.984。本方法操作简单,结果准确,由于几乎不使用有机溶剂也减少了分析过程对环境和人体的危害。Abstract: This article focused on the technique using GC-MS to determine the presence and concentrations of 45 kinds of organophosphorous pesticides in cider. 45 pesticides were tested with the recovery experiment of cider at three levels: 1, 5, 10 μg/L. The results showed that the 45 pesticides gave satisfactory recoveries ranging from 71.16% to 117.94% with the RSDs from 1.20% to 15.13% ( n = 5) , the limitation of this method was between 0.01 μg/L and 0.22 μg/L.45 pesticides were well separated and the linear relationship was good enough which the correlation coefficients were greater than 0.984 for concentrations from 10 to 2000 μg/L for most pesticides. Compared with conventional techniques, it was more accurate, lowcost, highly efficient and environmental friendly. Furthermore, for the limited use of organic solution, it has little harm to environment and human's health for the limited use of organic solution during the analysis process.
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[1] 汤婕, 汤锋, 岳永德, 等.气相色谱法 (GC-FPD) 快速测定蔬菜、水果中18种有机磷农药残留[J].安徽农业大学学报, 2013, 40 (6) :1054-1058. [2] 周蓉, 曹赵云, 赵肖华, 等.分散固相萃取-分散液液微萃取/气相色谱-串联质谱法测定蔬菜中19种有机磷农药残留[J].分析测试学报, 2017, 36 (1) :67-72. [3] 刘琪, 孙雷, 张骊.超高效液相色谱-串联质谱法测定猪肝中有机磷农药残留量的研究[J].分析测试学报, 2010, 29 (7) :747-750. [4] Domotorova Milena, Matisova Eva, Kirchner Michal, et al.MSPD combined with fast GC for ultratrace analysis of pesticide residues in non-fatty food[J].Acta Chimica Slovenica, 2005, 52 (4) :422-428.
[5] Xu Dun-ming, Yang Fang, Lu Sheng-yu, et al.Determination of indoxacarb residue in foodstuffs of plant and animal origin by GC-ECD and LC-MS/MS[J].Agricultural Sciences in China, 2008, 7 (10) :1228-1234.
[6] 张仕云, 郑仲华, 丘峰, 等.气相色谱-质谱法快速测定葡萄酒中7种有机磷农药[J].食品与发酵科技, 2016, 52 (6) :91-95. [7] 何超, 刘跃华, 黄海涛, 等.气相色谱法测定烟草中有机磷农药残留量[J].理化检验 (化学分册) , 2010, 46 (6) :663-668. [8] 潘守奇, 孙军, 董静, 等.气相色谱法同时测定蔬菜中24种有机磷农药残留[J].分析实验室, 2010, 29 (1) :115-118. [9] Anastassiades Michelangelo, Lehotay Steven J, Stajnbaher Darinka, et al.Fast and easy multiresidue method employing acetonitr ile extraction/partitioning and dispersive solid-phase extraction for the determination of pesticide residues in product[J].J AOAC International, 2003, 86 (2) :412-431
[10] Caro E, Marce R M, Cormack P A G, et al.Novel Enrofloxacin imprinted polymer applied to the solid phase extraction.Fluorinated quinolones from urine and tissue samples[J].Analytical Chimica Acta, 2006, 562 (2) :145-151.
[11] Aline oriano opes, Jerusa Simone Garcia, Rodrigo Ramos Catharino.Cloud point extraction applied to casein proteins of cow milk and their identification by masss pectrometry[J].Analytica Chimica Acta, 2007, 590:166-172.
[12] Alireza Rezaie Rod, Shahin Borhani, Farzaneh Shemirani.Cloud point preconcentration and flame atomic absorption spectrometry:application to the determination of manganese in milk and water samples[J].Eur Food Res Technol, 2006, 223:649-653.
[13] 肖珊美, 罗小会.浊点萃取-酶抑制-分光光度法测定蔬菜中有机磷农药残留量[J].理化检验化学分册, 2015, 51 (5) :713-715. [14] 李文廷, 向杨华, 王静.浊点萃取-气相色谱质谱法检测中药材中的有机磷农药残留[J].云南化工, 2016, 43 (4) :64-67. [15] 莫小荣, 郑春慧, 陈建伟, 等.浊点萃取-异辛烷反萃取-气相色谱测定茶叶中拟除虫菊酯农药残留[J].分析化学研究报告, 2009, 37 (8) :1178-1182. [16] 周宏琛, 朱涛, 王勇, 等.“日本肯定列表制度”农药残留新标准对我国农产品出口的影响[J].现代食品科技, 2006, 22 (4) :197-199.
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