云南省元谋县村民尿液中异菌脲残留影响因素分析
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摘要
目的检测云南省元谋县农村居民尿中异菌脲残留浓度,分析异菌脲残留量与居民使用农药时采取防护措施之间的关系。方法抽取云南省元谋县230名农民进行问卷调查及尿样采集,采用超高效液相色谱串联质谱法(UHPLC-MS/MS)测定尿中异菌脲残留量。尿液经Waters Oasis MCX柱固相萃取,用甲醇和5%的氨水甲醇溶液洗脱后离心浓缩,乙腈定容;以0.01%的甲酸乙腈溶液和0.01%的甲酸水溶液为流动相梯度洗脱,经Cosmosil色谱柱(4.6mm×150mm)分离,采用电喷雾离子源正离子模式进行质谱检测。结果 230份尿样共检出102份有异菌脲残留,检出率为44.35%,研究发现两个乡镇间居民尿液中异菌脲残留检出率差异有统计学意义(χ~2=6.16,P<0.05);5个村庄间居民尿液中异菌脲残留检出率差异有统计学意义(χ~2=11.49,P<0.05),阳性人群尿液中异菌脲残留量差异有统计学意义(F=3.60,P<0.01);尿液中异菌脲残留未检出人群佩戴口罩、手套、防护服的频率高于检出人群(Z=-4.50、-4.30、-4.94,P<0.01)。结论使用农药时采取防护措施能有效的减少农药与人体的接触,提示居民应合理使用农药,加强自身防护措施,从而减少农药对健康的危害。
Objective To detect iprodione residues in urine samples of rural residents in Yuanmou county of Yunnan,and to analyze the influencing factors. Methods Quota sampling method was used to randomly select 230 rural residents to participate in our questionnaire survey and their urine samples were collected for the detection of iprodione concentration by ultra high performance liquid chromatography-tandem mass spectrometry(UHPLC-MS/MS).The urine sample was solid-phase extracted by Waters Oasis MCX and eluted with methanol and methanol solution of 5% aqueous ammonia.After centrifugation and concentration,it was separated on Cosmosil packed column(4.6mm×150mm)with acetonitrile solution of 0.01% formic acid and aqueous solution of 0.01% formic acid as mobile phase by gradient elution.Electrospray ionization source was applied and operated in positive ion mode. Results Iprodione residue was detected in 102 urine samples with the positive rate of 44.35%.The positive rates of iprodione residues were significantly different between rural residents from two local towns(χ~2=6.16,P<0.05)as well as among rural residents from 5villages(χ~2=11.49,P<0.05).The concentration of iprodione residues was also different among residents with positive samples(F=3.60,P<0.01).Residents with negative iprodione in urine samples were more likely to wear masks,rubber gloves and protective clothing when exposing to pesticides(Z=-4.50,-4.30,-4.94,P<0.01). Conclusions Rural residents should properly protect themselves from direct exposure to the pesticides in order to avoid the hazardous effects of pesticides to the body.
Objective To detect iprodione residues in urine samples of rural residents in Yuanmou county of Yunnan,and to analyze the influencing factors. Methods Quota sampling method was used to randomly select 230 rural residents to participate in our questionnaire survey and their urine samples were collected for the detection of iprodione concentration by ultra high performance liquid chromatography-tandem mass spectrometry(UHPLC-MS/MS).The urine sample was solid-phase extracted by Waters Oasis MCX and eluted with methanol and methanol solution of 5% aqueous ammonia.After centrifugation and concentration,it was separated on Cosmosil packed column(4.6mm×150mm)with acetonitrile solution of 0.01% formic acid and aqueous solution of 0.01% formic acid as mobile phase by gradient elution.Electrospray ionization source was applied and operated in positive ion mode. Results Iprodione residue was detected in 102 urine samples with the positive rate of 44.35%.The positive rates of iprodione residues were significantly different between rural residents from two local towns(χ~2=6.16,P<0.05)as well as among rural residents from 5villages(χ~2=11.49,P<0.05).The concentration of iprodione residues was also different among residents with positive samples(F=3.60,P<0.01).Residents with negative iprodione in urine samples were more likely to wear masks,rubber gloves and protective clothing when exposing to pesticides(Z=-4.50,-4.30,-4.94,P<0.01). Conclusions Rural residents should properly protect themselves from direct exposure to the pesticides in order to avoid the hazardous effects of pesticides to the body.
引文
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[8]李继友,葛欣.毛细管气相色谱法定量分析异菌脲[J].农药,2010,49(11):817-818.
[9]郭藤,李娜,张洋,等.固相萃取-高效液相色谱法测定果蔬中异菌脲残留量[J].分析试验室,2014,33(7):860-863.
[10]梁林,张爱娟,潘金菊,等.超高效液相色谱-串联质谱法测定黄瓜及番茄中异菌脲残留[J].农药科学与管理,2014,35(4):45-48.
[11]Costa AI,Queiroz ME,Neves AA,et al.Determination of pesticides in lettuce using solid-liquid extraction with low temperature partitioning[J].Food Chem,2015,181:64-71.
[12]郑永权.农药残留研究进展与展望[J].植物保护,2013,39(5):90-98.
[13]Shalat SL,Donnelly KC,Freeman NC,et al.Nondietary ingestion of pesticides by children in an agricultural community on the US/Mexico border:preliminary results[J].J Expo Anal Environ Epidemiol,2003,13(1):42-50.
[14]荣维广,阮华,吴建,等.QuEChERS法结合在线凝胶色谱-气相色谱/质谱法测定人体尿液中34种农药残留[J].中国食品卫生杂志,2015,27(3):253-257.
[15]欧泽兵.个体防护装备是减少生产性农药中毒的有效途径[J].中国个体防护装备,2010(2):31-33.
[16]陆枫林,黄季琨.农药对喷洒员健康影响的研究[J].环境与职业医学,2004,21(1):39-41.
[2]US EPA.Pesticides-fact sheet for iprodione[EB/OL].(2015-9-16)[2016-12-20].https://www3.epa.gov/pesticides/chem_search/reg_actions/reregistration/fs_PC-109801_1-Nov-98.pdf.
[3]任璐,韩巨才,刘慧平.番茄早疫病菌对异菌脲的敏感基线及其抗性突变体的生物学特性[J].农药学学报,2010,12(2):155-160.
[4]吴春红,聂继云,李静,等.基质分散固相萃取-高效液相色谱法测定水果中的异菌脲残留量[J].食品科学,2009,30(14):188-190.
[5]王一洋,方菁,朱敏,等.云南省某县不同农业生产模式对农药使用行为的影响[J].环境与职业医学,2015,32(8):767-770.
[6]HúskováR,MatisováE,HrouzkováS,et al.Analysis of pesticide residues by fast gas chromatography in combination with negative chemical ionization mass spectrometry[J].J Chromatogr A,2009,1216,(35):6326-6334.
[7]Hayward DG,Wong JW.Organohalogen and organophosphorous pesticide method for ginseng root--a comparison of gas chromatography-single quadrupole mass spectrometry with high resolution time-of-flight mass spectrometry[J].Anal Chem,2009,81(14):5716-5723.
[8]李继友,葛欣.毛细管气相色谱法定量分析异菌脲[J].农药,2010,49(11):817-818.
[9]郭藤,李娜,张洋,等.固相萃取-高效液相色谱法测定果蔬中异菌脲残留量[J].分析试验室,2014,33(7):860-863.
[10]梁林,张爱娟,潘金菊,等.超高效液相色谱-串联质谱法测定黄瓜及番茄中异菌脲残留[J].农药科学与管理,2014,35(4):45-48.
[11]Costa AI,Queiroz ME,Neves AA,et al.Determination of pesticides in lettuce using solid-liquid extraction with low temperature partitioning[J].Food Chem,2015,181:64-71.
[12]郑永权.农药残留研究进展与展望[J].植物保护,2013,39(5):90-98.
[13]Shalat SL,Donnelly KC,Freeman NC,et al.Nondietary ingestion of pesticides by children in an agricultural community on the US/Mexico border:preliminary results[J].J Expo Anal Environ Epidemiol,2003,13(1):42-50.
[14]荣维广,阮华,吴建,等.QuEChERS法结合在线凝胶色谱-气相色谱/质谱法测定人体尿液中34种农药残留[J].中国食品卫生杂志,2015,27(3):253-257.
[15]欧泽兵.个体防护装备是减少生产性农药中毒的有效途径[J].中国个体防护装备,2010(2):31-33.
[16]陆枫林,黄季琨.农药对喷洒员健康影响的研究[J].环境与职业医学,2004,21(1):39-41.