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| 1 | 气相色谱/三重四极杆质谱法测定环境样品中二噁英显示文摘建立了同位素稀释-气相色谱/三重四极杆质谱法(GC-MS/MS)测定环境样品中痕量二噁英(PCDD/Fs)的分析方法.方法具有良好的灵敏度和重现性,对绝对进样量为20—200 fg的17种PCDD/Fs信噪比均大于50,色谱峰面积的相对标准偏差(RSD)小于20%(n=12).方法在较宽的浓度范围内具有良好的线性,标准曲线的相对响应因子(RRF)的RSD均小于15%.利用本方法测定了大气、土壤和污泥3种不同环境样品中二噁英的浓度,其检测结果与高分辨气相色谱/高分辨质谱法(HRGC/HRMS)结果具有良好的一致性,可以满足EPA 1613B方法的技术要求. | 孙慧中 王璞 田菲菲 张庆华 | 2017 | 环境化学2017,36,7: | 8 |
| 2 | Simultaneous quantification of fifty-one odor-causing compounds in drinking water using gas chromatography-triple quadrupole tandem mass spectrometry显示文摘A wide range of compounds with various structural features can cause taste and odor(T&O)problems in drinking water. It would be desirable to determine all of these compounds using a simple analytical method. In this paper, a sensitive method combining liquid–liquid extraction(LLE) with gas chromatography-triple quadrupole tandem mass spectrometry(GC–MS/MS)was established to simultaneously analyze 51 odor-causing compounds in drinking water,including organic sulfides, aldehydes, benzenes, phenols, ethers, esters, ketones, nitrogenous heterocyclic compounds, 2-methylisoborneol and geosmin. Three deuterated analogs of target analytes, dimethyl disulfide-d6, benzaldehyde-d6 and o-cresol-3,4,5,6-d4,were used to correct the variations in recovery, and five isotope-labeled internal standards(4-chlorotoluene-d4, 1, 4-dichlorobenzene-d4, naphthalene-d8, acenaphthene-d10, phenanthrene-d10 respectively) were used prior to analysis to correct the variations arising from instrument fluctuations and injection errors. The calibration curves of the target compounds showed good linearity(R2> 0.99, level = 7),and method detection limits(MDLs) below 1/10 of the odor threshold concentrations were achieved for most of the odorants(0.10–20.55 ng/L). The average recoveries of most of the analytes in tap water samples were between 70% and 120%, and the method was reproducible(RSD < 20%, n = 7). Additionally, concentrations of odor-causing compounds in water samples collected from three drinking water treatment plants(DWTPs) were analyzed by this method.According to the results, dimethyl trisulfide, dimethyl disulfide and indole were considered to be the key odorants responsible for the swampy/septic odor. 2-Methylisoborneol and geosmin were detected as the main odor-causing compounds for musty/earthy odor in DWTP B. | Chunmiao Wang Jianwei Yu Qingyuan Guo Yu Zhao Nan Cao Zhiyong Yu Min Yang | 2019 | Journal of Environmental Sciences2019,31,5: | 7 |
| 3 | 加速溶剂萃取技术应用于二噁英检测的研究进展显示文摘加速溶剂萃取技术通过提高温度和压力对混合基质中的有机物进行自动萃取.由于其具备有机溶剂用量少、萃取快速、样品回收率高等优点,可被应用于二噁英分析的样品前处理过程中.二噁英样品的提取效率与样品基质性质相关,为保证提取回收率必须选择合适的提取条件.本文从不同基质的角度综述了加速溶剂萃取技术在二噁英检测中的研究进展,同时展望了该技术未来的发展趋势. | 程嘉雯 田永 李春欣 关亚风 马继平 | 2021 | 环境化学2021,40,9: | 4 |
| 4 | 小麦中多氯联苯、有机氯农药和多溴联苯醚检测方法研究显示文摘建立了基于气相色谱-三重四极杆串联质谱的分析方法,用于小麦中多氯联苯,有机氯农药和多溴联苯醚的同时检测分析。小麦粉样品加水后,使用乙酸乙酯直接提取,采用44%硅胶净化柱进行净化,净化浓缩后的样品使用气相色谱-三重四极杆质谱进行检测,质谱检测器采用动态多反应监测(dMRM)模式。通过内标法定量。多氯联苯、有机氯农药和多溴联苯醚具有较好线性范围,其中七溴代联苯醚、八溴代联苯醚、九溴代联苯醚和十溴代联苯醚的响应与浓度呈二次曲线回归;方法检出限在0.001~1.108 ng/g之间,溴联苯醚随溴原子数量增加而检测灵敏度降低;方法回收率在57.9%~118.6%之间,相对标准偏差在1.6%~10.7%之间。该方法简单、快速、准确、经济,适用于大批量小麦样品中痕量持久性有机污染物的筛查和分析检测。 | 张炜 杨永坛 王松雪 李森 李丽 蔡娣 | 2022 | 粮油食品科技2022,30,2: | 2 |
| 5 | 基于GC-MS/MS法测定鱼肉中二噁英和二噁英类多氯联苯显示文摘建立基于GC-MS/MS方法,采用稳定性同位素稀释法测定鱼肉中二噁英及二噁英类多氯联苯。样品经快速溶剂萃取仪提取3次,以酸化硅胶除脂,经多层硅胶柱、碱性氧化铝柱和活性炭柱净化,分别收集含PCDD/Fs和DL-PCBs组分,经浓缩复溶后供GC-MS/MS测定。结果表明:在净化步骤中,PCDD/Fs和DL-PCBs受洗脱液的体积以及收集步骤的影响较大,分开收集PCDD/Fs和DL-PCBs,先对PCDD/Fs的收集液进行测定,然后将其和DL-PCBs的收集液合并完成DL-PCBs的测定,从而对DL-PCBs进行准确定量。采用鱼肉为样品基质时,该方法PCDD/Fs和DL-PCBs的内标回收率为63.3%~106.8%,RSD为0.4%~9.6%;目标物的回收率为93.6%~114.5%,RSD为0.9%~9.2%,方法线性和检出限达到国家标准GB 5009.205的要求,适用于鱼肉样品中PCDD/Fs和DL-PCBs的测定。 | 陆静 申甜甜 焦艳娜 崔凤云 朱绍华 成婧 易锡 付善良 | 2023 | 中国食品学报2023,23,9: | 0 |
| 6 | GC-MS/MS法测定猪肉中二噁英及二噁英类多氯联苯显示文摘建立基于气相色谱-串联质谱(gas chromatography-tandem mass spectrometry,GC-MS/MS)仪器,采用稳定性同位素稀释法测定猪肉中二噁英及二噁英类多氯联苯。样品经索氏提取,酸化硅胶除脂。然后经过多层硅胶柱、碱性氧化铝柱和活性炭柱净化,分别收集含二噁英(dioxins,PCDD/Fs)和二噁英类多氯联苯(dioxin like polychlorinated biphenyls,DL-PCBs)的组分。最后经浓缩溶剂交换后供GC-MS/MS测定。从样品的除脂方式、脂肪含量对净化的影响、系统空白污染来源等方面进行探讨。结果发现,凝胶渗透色谱除脂对PCDD/Fs和DL-PCBs的回收率影响较大,酸化硅胶除脂更适合超痕量的二噁英类化合物的分析和检测。二噁英检测的系统空白污染主要来自于索氏提取仪。该方法中内标的回收率为45.3%~122.4%,相对标准偏差(relative standard deviation,RSD)为1.0%~14.7%;目标物的回收率为64.9%~118.8%,RSD为1.1%~14.7%,方法线性和检出限能够达到GB 5009.205—2013《食品中二噁英及其类似物毒性当量的测定》的相关要求,适用于猪肉样品中PCDD/Fs和DL-PCBs的测定。 | 陆静 焦艳娜 成婧 申甜甜 朱绍华 付善良 | 2023 | 食品科学2023,44,18: | 0 |