活性白土在青菜有机磷农药检测中的研究
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摘要
目的筛选对青菜基质成分净化效果最好的吸附剂,并探究其对气相色谱检测青菜中有机磷农药的影响。方法青菜经乙腈提取后,用6种吸附材料分别进行基质成分净化,利用紫外-可见光光谱图分析筛选对青菜基质成分净化效果最好的吸附剂,并考察其加入量对净化效果的影响;通过比较加标回收率,考察该吸附材料对青菜中有机磷农药检测准确度的影响。结果活性白土和石墨化碳黑能显著降低青菜提取液在436 nm和668 nm附近的吸光度。在气相色谱检测中,随着活性白土加入量的增大,敌敌畏、灭线磷、毒死蜱、杀螟硫磷、三唑磷的回收率逐渐减小,甲胺磷、乙酰甲胺磷、久效磷、氧乐果、乐果的回收率先降低后升高。结论活性白土对青菜的基质成分净化效果好,但也对农药具有较强的吸附作用,其在农药残留检测中的应用还有待进一步研究。
Objective To screen the best absorbents for purifying the matrix components of green vegetable, and investigate its effects on the gas chromatography detection of organophosphorus pesticides in green vegetable. Methods After extraction of samples of green vegetable by acetonitrile, adsorption materials were added to purify, the effect of adsorption materials on the matrix composition of the vegetable was analyzed by UV-Vis spectrum. The detection accuracy of organophosphorus pesticides was investigated by comparing the recovery. Results Activated clay and graphitized carbon black could effectively reduce the absorbance of the vegetable around 436 nm and 668 nm. With the increasing addition of activated clay, the recoveries detected by the gas chromatography of methamidophos, dichlorvos, chlorpyrifos, fenitrothion, and triazophos were gradually decreased, but the recoveries of methamidophos, acephate, omethoate, monocrotophos, and dimethoate were firstly decreased and then increased. Conclusion Activated clay has good purification effect on the matrix components of green vegetable, but it also has strong adsorption on pesticides. Its application in pesticide residue detection needs further study.
Objective To screen the best absorbents for purifying the matrix components of green vegetable, and investigate its effects on the gas chromatography detection of organophosphorus pesticides in green vegetable. Methods After extraction of samples of green vegetable by acetonitrile, adsorption materials were added to purify, the effect of adsorption materials on the matrix composition of the vegetable was analyzed by UV-Vis spectrum. The detection accuracy of organophosphorus pesticides was investigated by comparing the recovery. Results Activated clay and graphitized carbon black could effectively reduce the absorbance of the vegetable around 436 nm and 668 nm. With the increasing addition of activated clay, the recoveries detected by the gas chromatography of methamidophos, dichlorvos, chlorpyrifos, fenitrothion, and triazophos were gradually decreased, but the recoveries of methamidophos, acephate, omethoate, monocrotophos, and dimethoate were firstly decreased and then increased. Conclusion Activated clay has good purification effect on the matrix components of green vegetable, but it also has strong adsorption on pesticides. Its application in pesticide residue detection needs further study.
引文
[1]NY/T 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].NY/T 761-2008 Pesticide multiiresidue screen methods for determination of organophosphorus pesticides,organochlorine pesticides,pyrethroid pesticides and carbamate pesticedes in vegetables and fruits[S].
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[21]江正洪,曾海平,翁惠新,等.活性白土负载AlCl_3催化剂对脱除芳烃中微量烯烃反应的性能研究[J].矿物岩石,2010,30(4):17-20.Jiang ZH,Ceng HP,Weng HX,et al.The activity in removing trace olefins of aromatic hydrocarbons by using activated clay supported AICI3[J].J Miner Petrol,2010,30(4):17-20.
[22]李百健,吴超,邵京.柑橘皮果胶的制备及其脱色工艺[J].湖北农业科学,2013,52(23):162-166.Li BJ,Wu C,Shao J.Process of pectin extraction from orange peel and its decolorization[J].Hubei Agric Sci,2013,52(23):162-166.
[23]张明明,刘玉兰,杨金强,等.油脂中邻苯二甲酸酯类塑化剂的吸附脱除研究[J].粮油食品科技,2015,23(5):32-36.Zhang MM,Liu YL,Yang JQ,et al.Research on adsorption removal of phthalic acid esters in oil[J].Sci Tech Cereals Oils Foods,2015,23(5):32-36.
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[27]刘玉兰,张东东,温运启,等.葵花籽油中多环芳烃及色泽的吸附脱除研究[J].中国粮油学报,2017,32(6):100-106.Liu YL,Zhang DD,Wen YQ,et al.Adsorption removal of polycyclic aromatic hydrocarbons and color of sunflower oil[J].J Chin Cereal Oil Ass,2017,32(6):100-106.
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[2]GB 23200.8-2016食品安全国家标准水果和蔬菜中500种农药及相关化学品残留量的测定气相色谱-质谱法[S].GB 23200.8-2016 National food safety standard-Determination of 500pesticides and related chemicals residues in fruits and vegetables-Gas chromatography-mass spectrometry[S].
[3]冯丽丽,胡晓芳,于晓娟,等.气相色谱法测定有机磷农药残留的常见问题探讨[J].环境监测管理与技术,2013,25(3):47-50.Feng LL,Hu XF,Yu XJ,et al.Research on some problems in determination of organophosphorus pesticide by gas chromatography[J].Admin Tech Environ Monit.2013,25(3):47-50.
[4]潘兴富,杜会方,闫慧芳,等.古洛糖酸内酯在5种有机磷农药检测中的应用研究[J].卫生研究,2010,39(2):221-223.Pan XF,Du HF,Min HF,et al.Research the role of gulonic acid lactone in the five kinds of organic phosphorus pesticide detection[J].J Hyg Res,2010,39(2):221-223
[5]王婧.QuEChERS前处理方法在农药残留检测中的应用[J].山西农业科学,2017,45(12):2051-2055.Wang J.Study on the Application of QuEChERS pretreatment method in the detection of pesticide residues[J].J Shanxi Agric Sci,2017,45(12):2051-2055.
[6]NY/T 1380-2007蔬菜、水果中51种农药多残留的测定气相色谱-质谱法[S].NY/T 1380-2007 Determination of 51 pesticides residues in fruits and vegetables-GC-MS[S].
[7]Lehotay S.AO AC official method 2007.01 pesticide residues in foods by acetonitrile extraction and partitioning with magnesium sulfate[J].J AOAC Int,2007,90(2):485-520.
[8]EN 15662-2008 Foods of plant origin-determination of pesticide residues using GC-MS and/or LC-MS/MS following acetonitrile extraction/partitioning and cleanup by dispersive SPE-QuEChERS-method[J].
[9]丁栋,王强,顾政一,等.响应面法优化马脂脱色工艺研究[J].食品工业科技,2014,35(9):226-229,234.Ding D,Wang Q,Gu ZY,et al.Optimization of decoloration process of horse fat by response surface methodology[J].Sci Technol Food Ind,2014,35(9):226-229,234.
[10]韩海娜,王宝维,崔爱秀,等.响应面法优化鸭油精炼工艺的研究[J],中国家禽,2013,35(18):29-33.Han HA,Wang BW,Cui AX,et al.Refining process of duck fat with optimization of response[J].China Poult,2013,35(18):29-33.
[11]彭彰文,马添,马浩瑞,等.山核桃油脱色工艺及脱色效果研究[J].农产品加工,2017,(10):30-33,43.Peng ZW,Ma T,Ma HR,et al.Decoloring technique and efficiency for caryn cathnyensis oil[J].Farm Prod Proc,2017,(10):30-33,43.
[12]高红,侯思琰.废油脂制造生物柴油中脱色工艺条件研究[J].广东化工,2014,41(3):62-64.Gao H,Hou SY.Study on decoloration technology conditions of manufacturing biodiesel with waste oil&fat[J].Guangdong Chem Ind,2014,41(3):62-64.
[13]杨梦娜,孙红娟,彭同江,等.微波活化法制备高效活性白土及其脱色性能研究[J].非金属矿,2016,39(3):20-22.Yang MN,Sun HJ,Peng TJ,et al.Study on synthesis and performance of activated clay by microwave activation method[J].Non-Met Mines,2016,39(3):20-22.
[14]朱正伟,曹伟伟,马建国,等.浓香葵花籽油精炼脱色剂及脱色工艺的研究[J].中国油脂,2015,40(11):16-21.Zhu ZW,Cao WW,Ma JG,et al.Research on preparation of deodorant and decoloring technique for fragrant sunflower seed oil[J].China Oils Fats,2015,40(11):16-21.
[15]郑来宁,刘玉兰,王动民,等.浸出混合油脱溶工艺对米糠毛油吸附脱色效果的影响[J].粮食与食品工业,2015,22(6):4-7.Zheng Ln,Liu Yl,Wang Dm,et al.The influence of miscella desolventizing technology on the adsorptive bleaching effect of crude rice bran oil[J].Cereal Food Ind,2015,22(6):4-7.
[16]张文启,奚旦立,李永峰,等.白土一活性污泥法处理煤气废水的试验研究[J].中国给水排水,2008(7):60-62.Zhang WQ,Xi DL,Li YF,et al,Experimental study on carclazyte/activated sludge process for coal gasification wastewater treatment[J].China Water Wastewater,2008(7):60-62.
[17]Al-jlil,Saad-A.Adsorption of cobalt ions from waste water on activated Saudi clays[J].Appl Water Sci,2017,7(1):383-391.
[18]付红普,宜沛沛,高晓明,等.活性白土-Bi_2WO_6光催化剂的制备及其光催化降解含酚废水[J].工业催化,2015,23(1):69-74.Fu HP,Yi PP,Gao XM,et al.Preparation and application of activated white clay-Bi_2WO_6 photocatalyst for degradation of phenol-containing wastewater[J].Ind Catal,2015,23(1):69-74.
[19]韦庆婷.TiO_2基光催化剂的合成及其活性白土负载与应用[D].延安:延安大学,2009.Wei QT.The load and application of clay synthesis and photocatalytic activity of TiO_2[D].Yan'an:Yan'an University,2009.
[20]吴爽,陈旭,陈平.铝柱撑活性白土催化合成苯甲醛乙二醇缩醛[J].香料香精化妆品,2011,(5):10-12,16.Wu S,Chen X,Chen P.Catalytic synthesis of benzaldehyde glycol acetal with al-pillared activated clay[J].Flav Frag Cosmet,2011,(5):10-12,16.
[21]江正洪,曾海平,翁惠新,等.活性白土负载AlCl_3催化剂对脱除芳烃中微量烯烃反应的性能研究[J].矿物岩石,2010,30(4):17-20.Jiang ZH,Ceng HP,Weng HX,et al.The activity in removing trace olefins of aromatic hydrocarbons by using activated clay supported AICI3[J].J Miner Petrol,2010,30(4):17-20.
[22]李百健,吴超,邵京.柑橘皮果胶的制备及其脱色工艺[J].湖北农业科学,2013,52(23):162-166.Li BJ,Wu C,Shao J.Process of pectin extraction from orange peel and its decolorization[J].Hubei Agric Sci,2013,52(23):162-166.
[23]张明明,刘玉兰,杨金强,等.油脂中邻苯二甲酸酯类塑化剂的吸附脱除研究[J].粮油食品科技,2015,23(5):32-36.Zhang MM,Liu YL,Yang JQ,et al.Research on adsorption removal of phthalic acid esters in oil[J].Sci Tech Cereals Oils Foods,2015,23(5):32-36.
[24]冯艳平,张海,王勇,等.活性白土吸附脱除鱼油中胆固醇的工艺研究[J].中国油脂,2013,38(11):7-10.Feng YP,Zhang H,Wang Y,et al.Removal of cholesterol from fish oil by activated clay adsorption[J].China Oils Fats,2013,38(11):7-10.
[25]陈金定,刘玉兰,张振山,等.玉米油中黄曲霉毒素B,的吸附脱除效果研究[J].中国油脂,2016,41(2):78-81.Chen JD,Liu YL,Zhang ZS,et al.Adsorption removal effect on aflatoxin B_1 from maize oil[J].China Oils Fats,2016,41(2):78-81.
[26]刘玉兰,裴娅晓,许利丽,等.吸附法脱除玉米油中玉米赤霉烯酮的研究[J].粮食与油脂,2016,29(9):6-10.Liu YL,Pei YX,Xu LL,et al.Removal of zearalenone from maize oil by absorption[J].Cereals Oils,2016,29(9):6-10.
[27]刘玉兰,张东东,温运启,等.葵花籽油中多环芳烃及色泽的吸附脱除研究[J].中国粮油学报,2017,32(6):100-106.Liu YL,Zhang DD,Wen YQ,et al.Adsorption removal of polycyclic aromatic hydrocarbons and color of sunflower oil[J].J Chin Cereal Oil Ass,2017,32(6):100-106.
[28]Tsai WT,Lai CW,Hsien KJ.Effect of particle size of activated clay on the adsorption of paraquat from aqueous solution[J].J Colloid Interface Sci,2003,263(1):29-34.
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