•  
  •  
  •  
  •  
  •  
  •  
  •  
  •  
期刊检索


检索
检索项:
检索词:
总目录
  • WCSB9︱2019(第九届)世界采样和混样大会 查看全文>>
  • 关于召开第十五届全国青年分析测试学术报告会的通知 查看全文>>
友情链接
气相色谱-质谱法测定温室大棚土壤中13种有机磷酸酯
    点此下载全文
作者单位
桑永珠,厉文辉,刘杰民,曲琛,赵研君,蔡寒梅,洪思程 1.国标(北京)检验认证有限公司2.北京科技大学化学与生物工程学院3.中国建材检测认证集团有限公司 
基金项目:国家重点研发计划(2016YFC0700901);国家自然科学基金(21878018)
中文摘要:该文建立了气相色谱-质谱法(GC-MS)检测温室大棚土壤中磷酸三乙酯、磷酸三丙酯、磷酸三正丁酯、磷酸三异丁酯、磷酸三丁氧乙酯、磷酸三(2-乙基己基)酯、磷酸三(2 氯乙基)酯、磷酸三(1 氯 2-丙基)酯、磷酸三(1,3-二氯-2-丙基)酯、磷酸三苯酯、磷酸三甲苯酯、磷酸甲苯二苯酯、2 乙基己基二苯基磷酸酯13种有机磷酸酯(OPEs)的分析方法,并优化了提取溶剂、提取方式、提取时间、萃取柱种类和色谱条件等实验参数。样品以正己烷-丙酮(体积比1∶1)为提取溶剂超声提取,经Florisil固相萃取柱净化,再采用气相色谱-质谱法(选择离子监测模式)检测,内标法定量。结果显示:13种化合物在1~500 μg/L质量浓度范围内线性良好,相关系数(r2)为0.999 3~0.999 7,检出限(LOD,S/N=3)为0.04~2.31 μg/L,定量下限(LOQ,S/N=10)为0.13~7.69 μg/L,在3个加标浓度(1.0、10、50 μg/L)下的回收率为54.5%~130%,相对标准偏差(RSD)为1.7%~9.9%。采用该方法对北京地区温室蔬菜大棚中41份土壤样品进行分析发现,除磷酸三丙酯(TPrP)外,其余12种OPEs均有检出,含量为1.90~632 ng/g(干重),平均值为87.8 ng/g,中位值为39.7 ng/g。其中磷酸三丁氧乙酯(TBEP)是温室土壤中最主要的OPEs,约占12种有机磷酸酯总含量(∑12OPEs)的20%。该方法操作简便、快速、精密度良好,可用于土壤中13种OPEs的测定。
中文关键词:超声提取  气相色谱-质谱法(GC-MS)  有机磷酸酯  温室大棚土壤
 
Simultaneous Determination of 13 Organophosphate Esters in Greenhouse Soil by Gas Chromatography-Mass Spectrometry
Abstract:In this study,a gas chromatography-mass spectrometry(GC-MS) was developed for the simultaneous detection of 13 kinds of organophosphate esters(OPEs) in greenhouse soil,including triethyl phosphate,tripropyl phosphate,tri-n-butyl phosphate,triisobutyl phosphate,tributoxyethyl phosphate,tris(2-ethylhexyl) phosphate,tris(2-chloroethyl) phosphate,tris(1-chloro-2-propyl) phosphate,Tris(1,3-dichloro-2-propyl) phosphate,triphenyl phosphate,tricresyl phosphate,toluene diphenyl phosphate and 2-ethylhexyl diphenyl phosphate.The experimental parameters such as extraction solvents,extraction methods,extraction times,extraction column types and chromatographic conditions were optimized.The soil samples were ultrasonically extracted with n hexane-acetone(1∶1,by volume),and then purified with a Florisil solid phase extraction column,followed by analysis of GC-MS in selected ion monitoring mode and quantitative analysis by internal standard method.Results showed that there were good linear relationships for 13 target compounds in the mass concentration range of 1-500 μg/L,with their correlation coefficients(r2) of 0.999 3-0.999 7.The limits of detection(LODs,S/N=3) and limits of quantitation(LOQs,S/N=10) were in the ranges of 0.04-2.31 μg/L and 0.13-7.69 μg/L,respectively.The soil spiked recoveries at three spiked levels of 1.0,10 and 50 μg/L ranged from 54.5% to 130%,with relative standard deviations(RSDs) of 1.7%-9.9%.This method was applied to the analysis of 41 soil samples from vegetable greenhouses in Beijing.Except for tripropyl phosphate,12 kinds of OPEs were detected in all samples,with the concentration range of 1.90-632 ng/g(dry weight,dw),the mean value of 87.8 ng/g and the median value of 39.7 ng/g.Tributyloxyethyl phosphate is the most abundant OPEs,contributing about 20% of the total content of 12 kinds of organophosphate esters(∑12OPEs).This method is simple,rapid,sensitive and accurate,and could meet the demands for analysis of 13 OPEs in soil.
Key Words:ultrasonic extraction  gas chromatography-mass spectrometry(GC-MS)  organophosphate esters  greenhouse soil
引用本文:桑永珠,厉文辉,刘杰民,曲琛,赵研君,蔡寒梅,洪思程.气相色谱-质谱法测定温室大棚土壤中13种有机磷酸酯[J].分析测试学报,2020,39(12):1538-1543.
摘要点击次数: 244
全文下载次数: 350
查看全文  查看/发表评论  下载PDF阅读器