泡腾辅助-悬浮固化-分散液液微萃取结合液相色谱法测定食醋中多效唑和异丙甲草胺农药残留
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摘要
建立了泡腾辅助、悬浮固化、分散液液微萃取技术和液相色谱联用测定食醋中的农药残留量的方法。结合食醋本身呈酸性的特点与NaHCO3反应,在原位处生成CO2辅助萃取剂和待测样品充分接触进行萃取,无需加入分散剂或借助分散设备。采用的萃取剂十一醇具有低毒、低密度和低凝固点的特点,冰浴后萃取剂由液态转化成固态附着于离心管上端,降低了萃取相分离收集的难度。优化后的萃取条件为200μL十一醇,10 mg NaHCO3,100 mg NaCl,萃取时间为30 s。多效唑和异丙甲草胺的检出限分别为2. 06 ng/mL和0. 25 ng/mL。多效唑和异丙甲草胺在高粱醋和米醋中的回收率为65. 2%～76. 0%。方法能够用于食醋中的农药残留测定。
This work has established an effervescent assisted solidification of floating organic droplet dispersion liquid-liquid microextraction technology to analyze the pesticide residues in vinegar by HPLC. Due to the acidic property of vinegar,carbon dioxide gas was in situ generated from the reaction of vinegar and sodium bicarbonate,and thus the vinegar could be fully contacted with extractant by effervescence without adding dispersant or using dispersing equipment. In addition,extractant 1-undecanol with low toxicity,density and freezing point was adopted in this paper. After ice bath,the extractant was transformed from a liquid phase into a solid phase and attached to the upper end of the centrifuge tube,thus reducing the difficulties in collection of the extract phase. Optimal extraction conditions were as follows: 200 μL of 1-undecanol,10 mg of sodium bicarbonate,100 mg of sodium chloride,extraction time of 30 s. The limits of detection were 2. 06 ng/m L and 0. 25 ng/m L for paclobutrazol and metolachlor, respectively. The recoveries of paclobutrazol and metolachlor in sorghum and rice vinegar were between 65. 2% and 76. 0%. In a word,this effervescent assisted solidification of floating organic droplet dispersion liquid-liquid microextraction method is simple and green,and can be utilized for the determination of pesticide residues in vinegar.
This work has established an effervescent assisted solidification of floating organic droplet dispersion liquid-liquid microextraction technology to analyze the pesticide residues in vinegar by HPLC. Due to the acidic property of vinegar,carbon dioxide gas was in situ generated from the reaction of vinegar and sodium bicarbonate,and thus the vinegar could be fully contacted with extractant by effervescence without adding dispersant or using dispersing equipment. In addition,extractant 1-undecanol with low toxicity,density and freezing point was adopted in this paper. After ice bath,the extractant was transformed from a liquid phase into a solid phase and attached to the upper end of the centrifuge tube,thus reducing the difficulties in collection of the extract phase. Optimal extraction conditions were as follows: 200 μL of 1-undecanol,10 mg of sodium bicarbonate,100 mg of sodium chloride,extraction time of 30 s. The limits of detection were 2. 06 ng/m L and 0. 25 ng/m L for paclobutrazol and metolachlor, respectively. The recoveries of paclobutrazol and metolachlor in sorghum and rice vinegar were between 65. 2% and 76. 0%. In a word,this effervescent assisted solidification of floating organic droplet dispersion liquid-liquid microextraction method is simple and green,and can be utilized for the determination of pesticide residues in vinegar.
引文
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[2] YE Q,HUANG J X,SUN L,WAN K,ZHU F G,LUO C,WANG F H. Chin. J. Pest. Sci.,2017,19(5):589叶倩,黄健祥,孙玲,万凯,朱富伟,骆冲,王富华.农药学学报,2017,19(5):589
[3] Zhang J,WAN H H,ZHANG H. Chinese J. Chromatogr.,2017,35(9):963张婧,万慧慧,张华.色谱,2017,35(9):963
[4] Asadollahi T,Dadfarnia S,Shabani A M. Talanta,2010,82(1):208
[5] Lasartearagon S G,Lucena R,C Rdenas S,et al. Anal. Chim. Acta,2014,807:61
[6] Rezaee M,Assadi Y,Hosseini M R M,et al. J. Chromatogr. A,2006,1116(1-2):1
[7] YANG M,WU X,JIA Y,et al. Anal. Chim. Acta,2016,906:118
[8] Mansour F R,Danielson N D. Talanta,2017,170:22
[9] Farahmand F,Ghasemzadeh B,Naseri A. Spectrochim. Acta A,2017,188:72
[10] XIA Y,ZHANG L,ZHAO E C,JIA C H,ZHU X D. J. Instrum. Anal. 2014,33(2):192.夏英,张澜,赵尔成,贾春虹,朱晓丹.分析测试学报,2014,33(2):192.
[11] LIU X,LIU C,WANG P,YAO G J,LIU D H,ZHOU Z Q. Food Chem.,2017,245:653
[12] Craig A P,Fields C,Liang N,et al. Talanta,2016,154:481
[13] CAO J P,XIE Q L,ZHOU J M,YI Z H. J. Instrum. Anal.,2015,34(5):616曹江平,解启龙,周继梅,易宗慧.分析测试学报,2015,34(5):616
[14] MohammadiS Z,sheibani A,Abdollahi F,Shahsavani E. Arab. J. Chem.,2012,54(S2):1510
[15] BAI B Q,WANG Q. Food Safe. Qual. Detect. Technol.,2017,8(3):935白宝清,王祺.食品安全质量检测学报,2017,8(3):935