GC-MS/MS法测定马铃薯中多农药残留含量

本文建立了三重四极杆气质联用仪GC-MS/MS同时测定马铃薯中多农药残留分析方法.在1—100μg·L~(-1)浓度范围内,各农药的相关系数均在0.996以上.对10μg·L~(-1)的标准溶液连续6针进样,峰面积的RSD%均小于10%.当样品称样量为5 g时,绝大数农药的最低检出限(LOD)在1. 0μg·kg~(-1)以下.在0.05 mg·kg~(-1)的加标浓度下,大部分农药的加标回收率在70.0%—130.0%之间,完全满足日常检测对薯类中农药残留分析的要求.     

方波阳极溶出伏安法同时测定煤矸石和粉煤灰中的锌、镉、铅

采用铋膜修饰玻碳电极,建立了用方波阳极溶出伏安法同时测定煤矸石和粉煤灰中锌、镉、铅元素的分析方法.优化了扫描方式、电解液及p H值、铋离子浓度、富集电位、富集时间等实验参数.在最佳实验条件下,锌、镉、铅分别在1—90μg·L-1、20—120μg·L-1和1—120μg·L-1浓度范围内呈现良好的线性关系,3种元素的检出限分别为0.04、0.03、0.02μg·L-1.该法用于实际煤矸石、粉煤灰样品中锌、镉、铅的测定,准确度和精密度良好.     

气相色谱-质谱法检测运动场地塑胶面层中的18种多环芳烃

本文建立了气相色谱-质谱法(GCMS)检测运动场地塑胶面层中18种多环芳烃的方法.样品经乙酸乙酯超声萃取60 min,取上清液,加入内标混合溶液(萘-D8、蒽-D10和苝-D12等3种内标),用GCMS分离和检测.结果表明,多环芳烃在5—200μg·L~(-1)浓度范围内标准曲线线性良好,相关系数均在0.999以上.在5.0μg·L~(-1)浓度下,连续6次进样,峰面积RSD值均小于10.0%,精密度良好.以3倍信噪比(peak to peak)计算18种多环芳烃的检出限,以10倍信噪比(peak to peak)计算18种多环芳烃的定量限,各组分的检出限为0.09—0.8μg·kg~(-1),定量限为0.27—2.4μg·kg~(-1).在1.0 mg·kg~(-1)的加标浓度下,样品加标回收率为83.2%—129.7%.该方法简单方便,能够有效的监测运动场地塑胶面层中多环芳烃的含量.     

采用安捷伦5977B GC-MS测定土壤中有机氯农药含量

本文采用安捷伦7890B_5977B GC-MS测定土壤样品中的有机氯农药含量.本文中所涉及的样品前处理方法以及仪器分析方法完全参考环境标准《土壤和沉积物有机氯农药的测定气相色谱-质谱法》环境报批稿以及土壤样品前处理标准HJ783-2016规定的样品前处理要求和仪器分析条件.采用加压快速溶剂萃取的提取方法,结合弗罗里硅土净化法,对土壤样品进行提取与净化,建立了详细的前处理标准操作步骤和方法分析流程.此方法成功应用于土壤中26种有机氯农药的分析测定,样品加标回收率达到了73.0%—116.2%(标准要求40%—150%),仪器最低检出限为0.07—0.39μg·kg~(-1)(标准0.02—0.09 mg·kg~(-1)),方法检出限为0.01—0.08μg·kg~(-1)(标准0.08—0.36 mg·kg~(-1)).     

ICP-MS法测定电子电器材料中的有害元素铅、镉、砷、铬

建立了电感耦合等离子体质谱测定不同基体的电子电器材料中铅、镉、铬、砷四种有害元素的方法.对仪器的参数、测试稳定性等作了系统研究,优化了对不同基体样品中铅、镉、铬、砷元素分析的前处理条件,探讨了各种材料中基体元素与其它共存元素对待测元素的影响.方法检出限为0.0024-0.46μg·g-1,对标准物质的测定值与参考值相符,相对准偏差为0.6%-5.8%.     

直接进样-离子色谱法测定饮用水中痕量溴酸盐

对直接测定饮用水中痕量溴酸盐的离子色谱方法进行了优化 .选用高容量的碳酸盐选择性离子色谱柱 ,以 7 2mmol·l- 1 Na2 CO3 2mmol·l- 1 NaOH为流动相 ,可消除样品中碳酸盐、次氯酸根和高浓度氯离子的干扰 ,直接进样测定饮用水中 2 μg·l- 1 溴酸盐 ,其检出限为 0 6μg·l- 1 .样品经微波浓缩后 ,对溴酸盐的检出限可降为 0 0 6μg·l- 1 .方法用于北京市饮用水中溴酸盐浓度的测定 ,结果满意     

微波消解-电感耦合等离子体质谱法测定8类化妆品中23种元素

建立了微波消解-电感耦合等离子体质谱,同时测定8类化妆品中23种元素的方法.根据化妆品不同基质,选用硝酸-双氧水或硝酸-双氧水-氢氟酸对样品进行微波消解,采用在线内标校正基体效应,外标法定量进行ICP-MS测定.方法检出限为0.03～6.2μg·kg-1,线性相关系数均大于0.999,RSD为1.3%～6.8%,加标回收率为88.6%～109.1%.实验结果表明,该方法简便、快速、灵敏度高、准确度好,适用于8类化妆品中23种元素的同时测定.     

采用安捷伦5977B GC-MS测定土壤中硝基苯类化合物含量

本文采用安捷伦7890B_5977B GC-MS测定土壤样品中的硝基苯类化合物含量.样品前处理方法以及仪器分析方法参考《GC-MS测定半挥发性有机物》(EPA method 8270D)和土壤样品前处理标准HJ 783—2016规定的样品前处理要求和仪器分析条件.分别采用两种加压快速溶剂萃取的提取方法,结合弗罗里硅土净化法,对土壤样品进行提取与净化,建立了详细的前处理步骤并对处理过程中的要点进行描述.此方法成功应用于土壤中14种硝基苯类化合物的分析测定,样品加标回收率达到了73%—104%(标准要求40%—150%),仪器最低检出限为1.3—2.3μg·kg~(-1),方法检出限为1.4—2.4μg·kg~(-1).     

高效液相色谱-串联质谱法同时测定人血清中的全氟辛烷磺酸及其前体物

本研究采用HPLC-MS/MS联用技术,建立了分析人血清样品中全氟辛酸(PFOA)、全氟辛烷磺酸(PFOS)及7种PFOS前体物的方法.以Fluoro Sep RP Octyl反相柱为色谱分离柱,甲醇和醋酸铵为梯度洗脱淋洗液,内标校正法进行定量分析.比较了3种不同萃取方法对目标全氟化合物的萃取性能,结果表明乙腈/乙酸乙酯(体积比60∶40)混合溶剂的萃取效率最高.提取液进质谱分析前,预先过石墨烯柱进一步净化以减轻基质效应和延长色谱柱寿命.9种目标全氟烷基化合物在0.50—50μg·L~(-1)浓度范围内线性相关系数r均大于0.995,检出限为0.013—0.083μg·L~(-1),定量限为0.043—0.28μg·L~(-1).在添加浓度为0.50、1.0、5.0μg·L~(-1)水平下,9种全氟烷基化合物的加标回收率为81.7%—108%,相对标准偏差均小于12%.本方法稳定性好、准确度高、且可同时分析不同种类的PFOS前体以及PFOA和PFOS的异构体,适用于实际人体血清样品的定量分析检测.对10份中国人体血清样品的分析结果表明,PFOA和PFOS的浓度分别为0.60—5.1μg·L~(-1)和1.2—63μg·L~(-1),总支链PFOA的含量比例为3.0%—12%,总支链PFOS的含量比例为32%—69%.N-Me FOSAA在一个血清样品中被检出,其浓度为0.92μg·L~(-1).2个血清样品中含有全氟辛烷磺酰胺(FOSA),其浓度为0.12μg·L~(-1)和0.17μg·L~(-1).     

超高效液相色谱/三重四极杆质谱-直接进样分析地表水中硝基酚类化合物

本文建立了一种使用岛津超高效液相色谱仪Nexera X2和三重四极杆质谱仪LCMS-8050联用直接进样分析水中硝基酚类化合物的方法.本方法可在5 min内完成3种硝基酚类化合物分析.采用内标法定量,方法线性范围为0.1—100.0μg·L~(-1),相关系数大于0.998,各浓度回读值准确度在85.8%—112.7%之间.3个浓度下保留时间和峰面积的相对标准偏差(RSD%)分别在0.10%—0.20%和0.85%—3.30%之间.进样2.0μL,方法检出限在0.022—0.034μg·L~(-1)之间,测定下限在0.088—0.136μg·L~(-1)之间.地表水3个不同浓度样品加标回收率在86.7%—94.5%之间.残留实验结果为阴性.     

预浓缩/柱箱制冷GCMS/FID法测定大气中117种挥发性有机物

建立了罐采样、吸附剂辅助电子制冷预浓缩-柱箱制冷GCMS/FID同时测定大气中117种挥发性有机物(VOCs)的方法.样品经填充吸附剂的电子制冷预浓缩系统除水、除CO2、浓缩和热脱附后,采用柱箱制冷及GCMS/FID的多维切割单元,将5种C2-C3组分切到二维色谱柱进行分离并进入FID检测,甲醛及其他111种VOCs组...     

高效液相色谱-串联质谱法同时检测水体中26种药物及个人护理品

通过优化固相萃取条件和高效液相色谱-串联质谱参数,建立了可以同时检测地表水和地下水中26种典型药物及个人护理品(pharmaceuticals and personal care products,PPCPs),包括磺胺类、大环内酯类、喹诺酮类、酰胺醇类、精神类、消炎止痛类以及个人护理品的检测方法.通过将水样pH值调节至7,利用HLB固相萃取柱对水样中PPCPs进行富集,以甲醇和含0.005%甲酸的水溶液作为正离子模式流动相,甲醇和含0.5 mmol·L^-1乙酸铵的水溶液作为负离子模式流动相进行梯度洗脱,采用多反应监测的质谱扫描模式(MRM)分析测定.26种PPCPs的检出限为0.007—1.78 ng·L^-1,定量限为0.02—5.68 ng·L^-1,回收率为52.28%—115.24%.利用该方法检测北京潮白河地表水和地下水中PPCPs的浓度,结果表明,地表水中PPCPs的含量普遍高于地下水,磺胺甲恶唑、舒必利、咖啡因、卡马西平和布洛芬在地表水和地下水中的含量相对较高,检测浓度分别高达147.83、52.48、78.35、166.58、30.63 ng·L^-1.     

Whole pictures of halogenated disinfection byproducts in tap water from China’s cities

When bromide/iodide is present in source water, hypobromous acid/hypoiodous acid will be formed with addition of chlorine, chloramine, or other disinfectants. Hypobromous acid/hypoiodous acid undergoes reactions with natural organic matter in source water to form numerous brominated/iodinated disinfection byproducts (DBPs). In this study, tap water samples were collected from eight cities in China. With the aid of electrospray ionization-triple quadrupole mass spectrometry by setting precursor ion scans of m/z 35, m/z 81, and m/z 126.9, whole pictures of polar chlorinated, brominated, and iodinated DBPs in the tap water samples were revealed for the first time. Numerous polar halogenated DBPs were detected, including haloacetic acids, newly identified halogenated phenols, and many new/unknown halogenated compounds. Total organic chlorine, total organic bromine, and total organic iodine were also measured to indicate the total levels of all chlorinated, brominated, and iodinated DBPs in the tap water samples. The total organic chlorine concentrations ranged from 26.8 to 194.0 μg·L^–1 as Cl, with an average of 109.2 μg·L^–1 as Cl; the total organic bromine concentrations ranged from below detection limit to 113.3 μg·L^–1 as Br, with an average of 34.7 μg·L^–1 as Br; the total organic iodine concentrations ranged from below detection limit to 16.4 μg·L^–1 as I, with an average of 9.1 μg·L^–1 as I; the total organic halogen concentrations ranged from 31.3 to 220.4 μg·L^–1 as Cl, with an average of 127.2 μg·L^–1 as Cl.     

Dilution sampling and analysis of particulate matter in biomass-derived syngas

Thermochemical biomass gasification, followed by conversion of the produced syngas to fuels and electrical power, is a promising energy alternative. Real-world characterization of particulate matter (PM) and other contaminants in the syngas is important to minimize damage and ensure efficient operation of the engines it powers and the fuels created from it. A dilution sampling system is demonstrated to quantify PM in syngas generated from two gasification plants utilizing different biomass feedstocks: a BioMax^?15 Biopower System that uses raw and torrefied woodchips as feedstocks, and an integrated biorefinery (IBR) that uses rice hulls and woodchips as feedstocks. PM_2.5 mass concentrations in syngas from the IBR downstream of the purification system were 12.8–13.7 μg·m^-3, which were significantly lower than the maximum level for catalyst protection (500 μg·m^-3) and were 2–3 orders of magnitude lower than those in BioMax^?15 syngas (2247–4835 μg·m^-3). Ultrafine particle number concentration and PM_2.5 chemical constituents were also much lower in the IBR syngas than in the BioMax^?15. The dilution sampling system enabled reliable measurements over a wide range of concentrations: the use of high sensitivity instruments allowed measurement at very low concentrations (~1 μg·m^-3), while the flexibility of dilution minimized sampling problems that are commonly encountered due to high levels of tars in raw syngas (~1 g·m^-3).     

Haloacetic acids in swimming pool and spa water in the United States and China

The objective of this study is to investigate the occurrence of haloacetic acids （HAAs）, a group of disinfection byproducts, in swimming pool and spa water. The samples were collected from six indoor pools, six outdoor pools and three spas in Pennsylvania, the United States, and from five outdoor pools and nine indoor pools in Beijing, China. Five HAAs （HAA5）, including monochloroacetic acid, dichloroacetic acid, trichloroacetic acid, monobromoacetic acid, and dibromoacetic acid were analyzed. Total chlorine, pH and total organic carbon concentration were analyzed as well. Results indicated that the levels of HAA5 in swimming pools and spas in the United States ranged from 70 to 3980μg·L^-1, with an arithmetic average at 1440μg·L^-1 and a median level at 1150μg·L^-1. These levels are much higher than the levels reported in chlorinated drinking water and are likely due to organic matters released from swimmers＇ bodies. The levels of HAA5 in swimming pools in China ranged from 13 to 332μg·L^-1, with an arithmetic average at 117μg·L^-1 and a median level at 114μg·L^-1. The lower HAA levels in swimming pools in China were due to the lower chlorine residuals. Results from this study can help water professionals to better understand the formation and stability of HAAs in chlorinated water and assess risks associated with exposures to HAAs in swimming pools and spas.     

南京秋季大气PM2.5中类腐殖质的光学性质与来源分析

类腐殖质(humic-like substances, HULIS)是水溶性有机碳(WSOC)中具有吸光特性的重要组分,对空气质量、气候变化和人体健康均有重要影响.尽管目前对HULIS的研究很多,但不同方法分离机理不同,对于HULIS的分离与测定仍然缺乏统一的标准,针对HULIS分离方法的研究很少.固相萃取法(solid phase extraction, SPE)因其操作简单、分离效果较好而被广泛应用,但对于低浓度样品仍存在检出限较高、回收率较低的问题,且很少有人关注提纯过程中流程空白所包含的含碳组分及其吸光能力.本研究通过调整活化溶液(0.01 mol·L^-1 HCl溶液+甲醇+2%NH₃H₂O/MeOH)与洗脱溶液(2%NH₃H₂O/MeOH)用量的比例对提纯方法进行优化.结果表明,应用优化后的方法对流程空白进行测量时,检出限(MDL)降低到0.035 mg·L^-1以下,精密度RSD <5.41%(n=20),标准品回收率达到95%,在保证回收率的情况下减少了流程空白,提高了样品的精密度,使测定浓度较低的HULIS含量成为可能.为了探究生物质燃烧期间含碳组分的光学特性和来源特征,本研究对2017年10月6日至11月9日南京北郊秋季大气气溶胶样品进行采集.采样期间PM_2.5的浓度为(87.9±43.7)μg·m^-3,WSOC和类腐殖质碳(HULIS-C)的浓度分别为(4.2±2.3)μg·m^-3和(3.6±2.0)μg·m^-3,HULIS-C占WSOC的比例为47.3%,是WSOC中的重要组成部分.本研究还对HULIS在330—400 nm波段的吸光进行测定,使用Angstrom指数(absorption angstrom exponent,AAE)进行表征,得到采样期间AAE的值为2—7,说明HULIS污染主要来自二次转化.后向轨迹结果表明,重污染期间污染物来源为本地生物质燃烧和区域或者长距离气团的输送.     

Preparation of hapten-specific monoclonal antibody for cadmium and its ELISA application to aqueous samples

High-affinity and specific monoclonal antibodies against cadmium-ethylene diamine tetraacetic acid (EDTA) complex have been produced using the hybridoma technique. A hapten was synthesized and characterized by Fourier Transform Infrared Spectroscopy (FT-IR) and UV-Vis. Competitive enzyme-linked immunosorbent assay (ELISA) for quantitative detection of cadmium in aqueous sample was developed. The monoclonal antibody with high level of binding affinity for Cd-IEDTA-BSA and high specificity for soluble Cd-EDTA complex showed less than 0.99% cross-reactivity with other 11 metals. The limit of detection was 0.10 μg·L^-1, and the effective linear range was 10^-1–10³ μg·L^-1. The intra- and inter-assay coefficient variations were 1.5%–6.3% and 3.2%–7.4%, respectively. The spike recovery in different water samples were between 98.5% and 110.3%. The detection limit of this assay was well below the allowable concentration of cadmium (3 μg·L^-1), and the working range was wider than that of other methods which showed the range of 2.19–86.38 and 0–10³ μg·L^-1. The competitive ELISA established in this paper was sensitive and accurate in the screening of cadmium in aqueous samples. The results will lay a solid foundation for construction of an immunoassay kit for cadmium.     

上海市公园绿地常见落叶树木叶片汞浓度时空特征及环境意义

植物叶片汞浓度与大气气态单质汞(GEM/Hg0)浓度的线性关系表明叶片汞浓度大小可用于指示植物生长区内GEM浓度的高低水平.通过分析上海市绿地公园(25座)中常见落叶树木樱花、水杉、法桐叶片汞浓度的时空变化特征,探究区域内GEM含量水平及分布特征.2017年5-10月对7座公园中这3种树木叶汞浓度进行连续监测,结果显示...     

A new procedure combining GC-MS with accelerated solvent extraction for the analysis of phthalic acid esters in contaminated soils

An optimized procedure based on gas chromatography-mass spectrometry (GC-MS) combined with accelerated solvent extraction (ASE) is developed for the analysis of six phthalic acid esters (PAEs), which are priority soil pollutants nominated by United States Environmental Protection Agency (USEPA). Quantification of PAEs in soil employs ultrasonic extraction (UE) (USEPA 3550) and ASE (USEPA 3545), followed by clean up procedures involving three different chromatography columns and two combined elution methods. GC-MS conditions under selected ion monitoring (SIM) mode are described and quality assurance and quality control (QA/QC) criteria with high accuracy and sensitivity for target analytes were achieved. Method reliability is assured with the use of an isotopically labeled PAE, di-n-butyl phthalate-d4 (DnBP-D4), as a surrogate, and benzyl benzoate (BB) as an internal standard, and with the analysis of certified reference materials (CRM). QA/QC for the developed procedure was tested in four PAE-spiked soils and one PAE-contaminated soil. The four spiked soils were originated from typical Chinese agricultural fields and the contaminated soil was obtained from an electronic waste dismantling area. Instrument detection limits (IDLs) for the six PAEs ranged 0.10–0.31 μg·L^-1 and method detection limits (MDLs) of the four spiked soils varied from a range of 20–70 μg·kg^-1 to a range of 90– 290 μg·kg^-1. Linearity of response between 20 μg·L^-1 and 2 mg·L^-1 was also established and the correlation coefficients (R) were all>0.998. Spiked soil matrix showed relative recovery rates between 75 and 120% for the six target compounds and about 93% for the surrogate substance. The developed procedure is anticipated to be highly applicable for field surveys of soil PAE pollution in China.     

Occurrence of estrogenic endocrine disrupting chemicals concern in sewage plant effluent

The purpose of this study was to give a worldwide overview of the concentrations of typical estrogenic endocrine disrupting chemicals （EDCs） in the effluent of sewage plants and then compare the concentra- tion distribution of the estrogenic EDCs in ten countries based on the survey data of the estrogenic EDCs research. The concentrations of three main categories （totally eight kinds） of estrogenic EDCs including steroidal estrogens （estrone （El）, estradiol （E2）, estriol （E3） and 17a- ethynylestradiol （EE2））, phenolic compounds （nonylphe- nol （NP） and bisphenol A （BPA）） and phthalate esters （dibutyl phthalate （DBP） and dibutyl phthalate （2- ethylhexyl） phthalate （DEHP）） in the effluents of sewage plants reported in major international journals over the past decade were collected. The statistics showed that the concentration distributions of eight kinds of EDCs were in the range of ng·L^-1 to μg·L^-1. The concentrations of steroidal estrogens mainly ranged within 50.00 ng. L-1, and the median concentrations of El, E2, E3 and EE2 were 11.00, 3.68, 4.90 and 1.00 ng·L^-1, respectively. Phenolic compounds and phthalate esters were found at pg. L-1 level （some individual values were at the high level of 40.00 μg·L^-1）. The median concentrations of BPA, NP, DBP and DEHP were 0.06, 0.55, 0.07 and 0.88 μg·L^-1, respectively. The concentrations of phenolic compounds and phthalate esters in the effluents were higher than that of steroids estrogens. The analysis of the concentration in various ten countries showed that steroids estrogens, phenolic compounds and phthalate esters in sewage plant effluents were detected with high concentration in Canada, Spain and China, respectively.