Determination of chlorpyrifos, triazophos and profenofos in vegetables by gas chromatography with solid phase extraction using multiwalled carbon nanotubes as adsorbent
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摘要: 本文以多壁碳纳米管为固相萃取材料,建立了蔬菜中毒死蜱、丙溴磷和三唑磷农药残留的GC-FPD分析方法。样品经乙酸乙酯匀浆提取后,用多壁碳纳米管SPE柱净化,以丙酮∶正己烷(1∶1,v/v)为洗脱剂,浓缩后用丙酮定容,再用GC-FPD进行检测。三种有机磷农药在0.00252.0mg/L范围内呈良好的线性关系,相关系数在0.99980.9999之间,回收率在83.3%96.7%之间,方法的检出限在8.21×10-41.37×10-3mg/kg之间。将该方法推广到莴苣、番茄、豇豆、梨、香菇等9种蔬菜、水果和食用菌中毒死蜱、丙溴磷、三唑磷农药残留的测定,效果较好。
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关键词:
- 多壁碳纳米管 /
- 固相萃取 /
- 气相色谱-火焰光度检测 /
- 农药残留
Abstract: A method based on multiwalled carbon nanotubes as the solid phase extraction material had been developed for the determination of chlorpyrifos, triazophos and profenofos in vegetables by gas chromatographyflame photometric detector ( GC /FPD) .The samples were extracted with ethyl acetate and purified by multiwalled carbon nanotubes column.The eluent was a mixture of acetone∶hexane ( 1∶1, v /v) .Then concentrated and dissolved by acetone before determined by GC /FPD.The results showed that these pesticides had a good linearity in the range of 0.0025~2.0mg /L and the correlations were between 0.9998 and 0.9999.The recoveries rate and limits of detection were 83.3% ~ 96.7% and 8.21 × 10- 4~ 1.37 × 10- 3mg /kg. Application of the method to the analysis of chlorpyrifos, triazophos and profenofos in several samples, we had a satisfactory result.-
Keywords:
- multiwalled carbon nanotubes /
- solid phase extraction /
- GC /FPD /
- pesticide residue
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[1] 张文童, 李锐, 章虎, 等.气相色谱-串联质谱法测定稻米中毒死蜱及其代谢物[J].理化检验 (化学分册) , 2012 (6) :667-670. [2] 袁玉伟, 叶雪珠, 王强, 等.三唑磷在稻米中的残留及其加工影响与膳食暴露评估[J].中国食品学报, 2012 (4) :187-194. [3] 罗婧, 贾娜, 施海燕, 等.丙溴磷在土壤中的吸附与迁移行为研究[J].环境科学与技术, 2011 (6) :16-19, 36. [4] 吴蕊宁, 王燕, 李言, 等.复配农药制剂丙溴磷·毒死蜱的气相色谱同时分析方法研究[J].应用化工, 2010 (1) :122-123, 138. [5] 谭斧, 肖时运.三唑磷·毒死蜱在稻田中的消解动态研究[J].农药科学与管理, 2013 (5) :40-46. [6] 余海明, 魏方林, 朱国念.三唑磷与氟虫腈复配对黏虫表皮的穿透作用[J].农药, 2010 (5) :344-346, 355. [7] 蔡曦, 钟良康, 丁坚强, 等.固相萃取-气相色谱法快速测定蔬果中23种有机磷农药残留[J].中国卫生检验杂志, 2011 (3) :566-567, 569. [8] 左海根, 占春瑞, 伍彩花, 等.气相色谱法测定大豆中24种有机磷农药的残留量[J].理化检验 (化学分册) , 2010, 10:1201-1204. [9] 王海凤, 刘海学, 王俊斌, 等.气相色谱-质谱法测定高粱籽粒中11种有机磷农药残留量[J].理化检验 (化学分册) , 2013 (6) :651-653. [10] 王敏, 韩芳, 张蕾, 等.高效液相色谱-串联质谱同位素内标法测定茶叶中25种有机磷农药残留[J].分析实验室, 2013 (4) :76-81. [11] 侯学文, 何衍彪, 徐汉虹.胆碱酷酶抑制法检测辛硫磷农药残留[J].河北师范大学学报:自然科学版, 2003, 27 (2) :151-154. [12] 梅文泉, 董宝生, 刘宏程, 等.固相萃取-气相色谱法测定茶叶中多种有机磷农药残留量[J].分析科学学报, 2011 (1) :97-100. [13] 赵海香, 史文礼, 孙大江, 等.多壁碳纳米管-固相萃取分析有机磷农药残留[J].分析化学, 2009, 10:1479-1483. [14] 张艳荣.碳纳米管的研究现状及应用[J].中国科技信息, 2008, (16) :36. [15] 张茜, 张公信, 李晓芬, 等.碳纳米管丝网印刷电极测定鞣花酸[J].云南民族大学学报:自然科学版, 2012 (3) :167-169, 177. [16] 赵海香, 贾艳霞, 丁明玉, 等.多壁碳纳米管固相萃取净化气相色谱法分析蔬菜中有机氯和拟除虫菊酯农药残留[J].色谱, 2011, 29 (5) :443-449. [17] 李圣陶, 龚吉军, 周昱, 等.多壁碳纳米管固相萃取技术的应用[J].食品工业科技, 2013, 13:373-377. [18] 彭晓俊, 庞晋山, 邓爱华, 等.改性多壁碳纳米管固相萃取-高效液相色谱法测定农产品中痕量残留的4种有机氯农药[J].色谱, 2012, 30 (9) :966-970. [19] NYT 761-2008.蔬菜和水果中有机磷、有机氯、拟除虫菊酯和氨基甲酸酯类农药多残留的测定[S].
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