化学分析计量CHEMICAL ANALYSIS AND METERAGE第31卷，第3期2022年3月V ol. 31，No. 3Mar. 202253doi:10.3969/j.issn.1008–6145.2022.03.012快速溶剂萃取–气相色谱–质谱法测定土壤中苯胺类化合物胡新飒（河南省南水北调中线渠首生态环境监测中心，河南南阳 474475）摘要 建立快速溶剂萃取（ASE ）–气相色谱–质谱（GC–MS ）法测定土壤中苯胺、邻硝基苯胺、间硝基苯胺、对硝基苯胺、二硝基苯胺5种苯胺类化合物的方法。
样品经丙酮–二氯甲烷混合溶剂（体积比为1∶1）提取，用硅酸镁小柱净化，经无水硫酸钠脱水，氮吹浓缩至1.0 mL ，用GC–MS 法测定，外标法定量。
5种苯胺类化合物的质量浓度在0.2～2.0 μg/mL 范围内与特征离子色谱峰面积具有良好的线性关系，相关系数均不小于0.995，方法检出限为0.7～5.7 μg/kg 。
当空白土壤样品加标质量分数分别为60、140 μg/kg 时，苯胺回收率为51.0%～64.2%，其余4种硝基苯胺的回收率为68.0%~121.5%，测定结果的相对标准偏差为1.2%～7.4%（n =6）。
该方法适用于低含量苯胺类化合物的土壤测定。
关键词 土壤；苯胺类化合物；气相色谱–质谱法；快速溶剂萃取中图分类号：O657.7 文献标识码：A 文章编号：1008-6145(2022)03–0053–05Determination of aniline compounds in soilby rapid solvent extraction–gas chromatography–mass spectrometryHU Xinsa(Ecological Environment Monitoring Center at the Head of Canal in the Middle Route of South-to-North Water Transfer in Henan Province,Nanyang 474475, China)Abstract A method for the determination of aniline, o -nitroaniline, m -nitroaniline, p -nitroaniline and dinitroaniline in soil by rapid solvent extraction(ASE)–gas chromatography–mass spectrometry (GC–MS) was established. The sample was extracted with acetone–dichloromethane mixed solvent(volume ratio was 1∶1), purified with magnesium silicate column, dehydrated with anhydrous sodium sulfate, concentrated to 1.0 mL by nitrogen blowing, determined by gas chromatography–mass spectrometry and quantified by external standard method. The mass concentration of five aniline compounds had a good linear relationships with the characteristic ion chromatographic peak area in the range of 0.2–2.0 μg/mL, the correlation coefficients were all not less than 0.995, the method detection limits of five aniline compounds were 0.7–5.7 μg/kg. The recovery of aniline was 51.0%–64.2%, and the recoveries of the other four nitroaniline were 68.0%–121.5% when the spiked mass fractions of blank soil samples were 60 and 140 μg/kg respectively, and the relative standard deviations of the determination results were 1.2%–7.4%(n =6). The method is suitable for the determination of low content aniline compounds in soil.Keywords soils; aniline compounds; gas chromatography–mass spectrometry; rapid solvent extraction苯胺类化合物化学性质活泼，广泛应用于印染、化妆品、制药、橡胶等工业领域。
万方数据 万方数据 万方数据 万方数据 万方数据 万方数据重金属超积累植物的研究进展作者：庞玉建， 宗浩， PANG Yu-jian， ZONG Hao作者单位：四川师范大学化学与材料科学学院,成都,610068刊名：四川环境英文刊名：SICHUAN ENVIRONMENT年，卷(期)：2008,27(2)被引用次数：4次1.Books RR.Lee J.Reeves RD Detection of nickeli ferous rocks by analysis of herbarium specimens of indicator plants 1977(07)2.Baker AJM.Brooks RR.Pease AJ Studies on copper and cobalt tolerance in three closely related taxa within the genus Silence L.(Caryophyllaceae) from Zaire[外文期刊] 1983(73)3.沈振国.刘友良重金属超积累植物的研究进展 1998(02)4.Flathman P nza G R Phytoremediation:current views on an emerging green technology 1998(07)5.宋书巧.周永张.周兴土壤砷污染特点与植物修复探讨[期刊论文]-热带地理 2004(01)6.Murphy A.Taiz L Comparison of metallothionein gene expression and non-protein thiols in ten Arabidopsis thaliana 1995(109)7.Grill E.Winnacker EL Phytochelatins:The principal heavy-metal complexing peptides of higher plant [外文期刊] 1985(230)8.Maitani T The composition of metals bound to Class Ⅲ metallothionein (Phytochelatin and Its Desglycyl Peptide) induced by various metals in root cultures of Rubia tinctorum[外文期刊] 1996(110)9.郎明林.张玉秀.柴团耀植物重金属超富集机理研究进展[期刊论文]-西北植物学报 2003(11)10.Zhao H.Butler E.Rodgers J Regulation of zinc homeostasis in yeast by binding of the ZAP 1 transcriptional activator to zinc responsive promoter elements[外文期刊] 1998(44)11.KramerU.Pickering I J.PR INCE R C Subcellular localization and speciation of Nickel in hyperaccumulator and non-accumulator Thlaspi Species[外文期刊] 2000(122)12.Davies W J.Zhang J Annu Rev Plant Physiol Plant Mol Boil 1991(49)uchli A Selenium in plants:uptake,functions and environmental toxicity 1993(106)14.Bennet AC.Shaw DR Effect of preharvest desiccants on Group IV Glycine max seed viability[外文期刊] 2000(48)15.王晓.黄宗益固体废弃物设备与技术新进展[期刊论文]-建筑机械化 2003(11)16.Garbisu C.Alkorta I Phytoextraction:A cost-effective plant-based technology for the removal of metals from the environment[外文期刊] 2001(77)17.李艳霞.王敏健.王菊思.陈同斌固体废弃物的堆肥化处理技术[期刊论文]-环境污染治理技术与设备 2000(04)18.Bridgewater AV.Meier D.Radlein D An overview of fast pyrolysis of biomass 1999(30)19.赵丽华.赵中一固体废弃物处理技术现状[期刊论文]-环境科学动态 2002(03)kshmi KL.Davis C Pyrolysis as a technique for separating heavy metals fromhyperaccumulators.Part II:Lab-scale pyrolysis of synthetic hyperaccumulator biomass 2003(25)kshmi KL.Davis C Pyrolysis as a technique for separating heavy metals from hyper-accumulators.Part Ш:pilot-scale pyrolysis of synthetic hyperaccumulator biomass 2004(26)22.Sarret G.Vangronsveld J.Manceau A Accumulation forms of Zn and Pb in Phaseolus vulgaris in the presence and absence of EDTA[外文期刊] 2001(13)23.Zhao FJ.Lombi E.Breedon T.McGrath SP Zinc hyperaccumulation and cellular distribution in Arabidopsis halleri[外文期刊] 2000(23)24.Garbisu C.Alkorta I Phytoextraction:A cost-effective plant-based technology for the removal of metals from the environment[外文期刊] 2001(77)25.Hetland MD.Gallagher JR.Daly DJ Processing of plants used to phytoremediate lead-contaminated sites 200126.Sas-Nowosielska A.Kucharski R.Malkowski E Phytoextraction crop disposal ─An unsolved problem[外文期刊] 2004(128)27.Cunningham SD Ow DW Promises and prospects of phytoremediation[外文期刊] 1996(110)28.KHAM A G.KNEK C.CHAUDHRY T M Role of plants,mycorrhizae and phytochelators in heavy metal contaminated land remediation[外文期刊] 2000(1-2)29.JAFFRE T.BROO KS R R.L EE J Scbertia acuminata:a hyperaccumulator of nickel from New Caledonia[外文期刊] 1976(193)30.BA KER A J M.MCGRATH S P.SIDOL IC M D The possibility of heavy metal decontamination of polluted soils using crops of metal-accumulating plants 1994(11)31.陈同赋.韦朝阳.黄泽春华南的一些砷超集累植物种类 200032.杨肖娥.龙新宪.倪吾钟东南景天--一种新的锌超富集植物[期刊论文]-科学通报 2002(13)33.薛生国.陈英旭.林琦中国首次发现的锰超积累植物--商陆[期刊论文]-生态学报 2003(05)34.韦朝阳.陈同斌.黄泽春大叶井口边草--一种新发现的富集砷的植物[期刊论文]-生态学报 2002(05)35.刘威.束文圣.蓝崇钰宝山堇菜(Viola baoshanensis) --一种新的镉超富集植物[期刊论文]-科学通报2003(19)36.魏树和.周启星.王新一种新发现的镉超积累植物龙葵(Solanum nigrum L)[期刊论文]-科学通报 2004(24)37.Yang X E.Shi W Y.Fu C X Copper hyperaccumulators of Chinese Nitive ports:Characteristics and Possible Use for Phytoremediation 199838.骆永明强化植物修复的螯合诱导技术及其环境风险[期刊论文]-土壤 2000(02)1.殷捷.周竹渝超积累植物的研究进展[期刊论文]-三峡环境与生态2003,25(11)2.罗青龙.任珺.陶玲.杨倩重金属超积累植物的研究进展[期刊论文]-能源与环境2008(6)3.王红新.WANG Hong-xin超积累植物在治理重金属污染土壤中的研究进展[期刊论文]-资源开发与市场2010,26(11)4.陈一萍.Chen Yiping重金属超积累植物的研究进展[期刊论文]-环境科学与管理2008,33(3)5.刘茵.赵秀琴.胡红艳超积累植物[期刊论文]-生物学教学2008,33(8)6.白向玉.韩宝平.刘汉湖.王晓青.BAI Xiang-yu.HAN Bao-ping.LIU Han-hu.WANG Xiao-qing花卉植物修复重金属污染技术的国内外研究进展[期刊论文]-徐州工程学院学报（自然科学版）2010,25(3)1.朱文宇.侯明明超积累植物的资源化利用[期刊论文]-环保科技 2009(2)2.张玉秀.刘金光.金铃.彭晓静近10年我国植物对重金属耐性/积累的文献研究分析[期刊论文]-农业图书情报学刊 2010(12)3.李有志.罗佳.张灿明.刘庆.郭丹丹湘潭锰矿区植物资源调查及超富集植物筛选[期刊论文]-生态学杂志 2012(1)4.李东旭.文雅超积累植物在重金属污染土壤修复中的应用[期刊论文]-科技情报开发与经济 2011(1)本文链接：/Periodical_schj200802020.aspx。
气相色谱-质谱法测定土壤中的磷脂脂肪酸张丽萍;王川;周巧红;王亚芬;吴振斌【摘要】采用气相色谱-质谱法测定土壤中的磷脂脂肪酸.土壤样品加入氢氧化钾的甲醇溶液中,其中的磷脂脂肪酸经甲酯化后,用正已烷萃取.萃取液采用Agilent DB-5MS色谱柱分离,质谱分析中选用全扫描和选择离子监测模式.26种脂肪酸甲酯的质量浓度在一定范围内与峰面积呈线性关系,检出限(3S/N)在0.001 2～0.295 9 mg·L-1之间.加标回收率在108％～115％之间,测定值的相对标准偏差(n=7)在3.2％～6.4％之间.【期刊名称】《理化检验-化学分册》【年(卷),期】2015(051)010【总页数】5页(P1353-1357)【关键词】气相色谱-质谱法;磷脂脂肪酸;土壤【作者】张丽萍;王川;周巧红;王亚芬;吴振斌【作者单位】中国科学院水生生物研究所,淡水生态与生物技术国家重点实验室,武汉430072;中国科学院水生生物研究所,淡水生态与生物技术国家重点实验室,武汉430072;中国科学院大学,北京100049;中国科学院水生生物研究所,淡水生态与生物技术国家重点实验室,武汉430072;中国科学院水生生物研究所,淡水生态与生物技术国家重点实验室,武汉430072;中国科学院水生生物研究所,淡水生态与生物技术国家重点实验室,武汉430072【正文语种】中文【中图分类】O657.63磷脂脂肪酸(PLFA)是构成活体细胞膜的重要组分,存在于所有生物细胞膜中。
在细胞死亡后,PLFA很快被降解,可以代表微生物群落中“存活”的群体。
不同种类的微生物群落之间体内PLFA的组成和含量有显著的差异,可以用来评价微生物的生物量及群落结构[1]。
磷脂脂肪酸生物标记法[2-4]近年被广泛地应用于土壤微生物多样性研究,并作为土壤微生物种群变化的监测指标。
土壤微生物多样性,既代表着土壤的生物活性,也反映了土壤生态胁迫机制对其微生物群落的影响[5-6],其研究对于探索自然生命机制、开发超常生物资源、应对全球气候变化、治理各类环境污染、维持生态服务功能及促进土壤持续利用等方面具有重要意义[7]。
应用固相微萃取技术分析番茄与天竺葵活体植株的挥发物*魏 明 邓晓军 胡文利 魏洪义 杜家纬**(中国科学院上海生命科学研究院植物生理生态研究所,上海200032)摘 要 应用固相微萃取技术(SPM E)和自行设计的挥发物收集装置对番茄和天竺葵的活体植株所释放的挥发性有机物(BV OCs)进行了色谱分析。
鉴定出番茄植株挥发物主要组成物质为A -蒎烯、A -萜品烯、水芹烯和桧烯等,天竺葵挥发物主要组成物质为A -蒎烯、莰烯、B -蒎烯、B -香叶烯、苎烯、石竹烯和A -草烯等。
而作为对照的常规通气吸附法则由于背景噪声复杂而未能有效鉴别出这两种植物活体植株的挥发物组成。
实验表明,本研究中建立的技术和装置能直接检测芳香植物活体所释放的挥发物的成分,并具有操作简便,无有机溶剂,重复性好等优点,适用于活体植物挥发性次生代谢物的相关研究。
关键词 固相微萃取,挥发物,收集装置,活体,色谱分析,通气吸附中图分类号 Q 949 文献标识码 A 文章编号 1000-4890(2004)04-0184-04Analysis of volatile chemicals em itted from living tomato and geranium samples with SPME tech -nique.W EI M ing ,DENG Xiaojun,HU Wenli,W EI Hong yi,DU Jiaw ei (Shanghai I ns titute of Plant Physiology and Ecology ,S hanghai I nstitutes f or Biological Sciences ,Chinese A cademy of Sciences ,Shanghai 200032,China).Chinese Journal of Ecology ,2004,23(4):184~187.So lid phase micro ex tract ion(SPM E)technique was applied to collect the biog enic volatile or ganic compounds(BV OCs)emitted from liv ing samples of tomato and geranium.A set of collecting devices desig ned by the authors was used in these experiments too.A nd t hen,the BV OCs collected were sent to be analyzed by the chromatogr am analysis system.T he major components in the BVOCs from tomato samples were identified as A -pinene,A -ter pinene,phellandrene,sabinene and some unknow n chemicals.And A -pinene,camphene,B -pinene,B -myrcene,limonene,caryophyllene and A -humulene were found in t he BVO Cs from geranium samples.In contrast,the control ex periments which em -ployed t he co nventional aerating abso rption system could not tell the certain volatile chemicals of tomato and g eranium because of the complex background.T hese exper iments indicated that t he tech -nique and dev ices established in this research were effective to ident ify the BVO Cs emitted fr om the liv ing aromatic plants directly,w ith the advant ag es such as clean -backg round,convenience,g ood re -peatability and solv ent -free.So this system can be a valuable method to study the volatile second metabolic chemicals in living plants.Key words Solid phase microex traction,V olatile compounds,Collecting devices,L iving samples,Chromatogram analysis,Aerated adsorption.*中国科学院知识创新工程项目(KSCX2-2-02)和2002年上海市科学技术委员会资助项目(023912004)。
