绵白糖中糖类化合物的电喷雾质谱研究

使用电喷雾质谱检测了在不同溶剂条件下的绵白糖溶液。实验结果表明不同绵白糖溶液在电喷雾质谱检测中表现出不同的特点,如在碱性条件下有利于负离子的形成,在甲醇溶液中能观察到单糖的质谱峰等。尽管绵白糖的成分比较简单,但是在质谱中表现十分复杂。采用串联质谱技术分析了这些溶液中化合物的碎裂规律,通过其碎裂方式确定了其质谱峰的归属。所建立的电喷雾质谱方法,灵敏度高,定性能力强,操作简便快速,可以作为糖产品的重要检测方法之一。     

碰撞反应池-电感耦合等离子体质谱法(ICP-MS)测定膨化食品中的铝

采用密闭高压消解技术对样品进行前处理,建立了膨化食品中铝的电感耦合等离子体质谱测定方法。完善样品前处理条件,优化仪器工作参数,并以45Sc为内标元素消除非质谱干扰,以氦气为碰撞反应气消除质谱干扰。在优化的实验条件下,方法的检出限为13.61μg/L,标准曲线的回归系数为0.999 9。同时采用国家标准方法——分光光度法和原子吸收光谱法验证了方法的准确度,三种方法的测定结果没有显著性差异。实验结果表明,方法简单、快速、准确,适用于食品中铝含量的测定。     

气相色谱-质谱检测饮用水中二氯乙酸、三氯乙酸方法论述

介绍了使用液液萃取衍生化、气相色谱-质谱联用测定饮用水中二氯乙酸、三氯乙酸的方法。该方法使用甲基叔丁基醚萃取,酸化甲醇酯化,使用气相色谱-质谱进行分离定性,内标法定量。     

电感耦合等离子体质谱在饮用水检测中的应用

结合电感耦合等离子体质谱原理,采用该方法对饮用水及水源水中26种元素进行了测定,得出了相关结论,验证了电感耦合等离子体质谱测定方法精密度好,准确性高,快速,灵敏,适用于饮用水及水源水中多元素同时测定。     

水环境监测中色谱-质谱技术的运用

从事水质有机物质监测分析的实验室几乎都把质谱分析作为最主要的定性确认手段之一,在很多情况下也用于定量分析。质谱技术的应用常和气相、液相、电感耦合等联用,成为现代水环境监测的重要仪器。本文浅析了,气相色谱-质谱联用,液相色谱-质谱联用,电感耦合质谱联用技术在水质监测中应用。     

电感耦合等离子体质谱(ICP-MS)法测定钒银矿中硒

提出了电感耦合等离子体质谱(ICP-MS)法测定钒银矿中硒的含量。样品经逆王水加高氯酸溶解,并采用内标法消除了可能存在的质谱干扰。实验结果表明,方法检出限为0.066ng/mL,加标回收率为94%~104%,测定值的相对标准偏差(n=7)均小于5.0%。方法简单、快速、准确,适用于钒银矿中硒含量的测定。     

气相色谱法在食品及饲料有害物质分析中的应用

气相色谱法、气相色谱-质谱联用法、毛细管柱气相色谱-质谱联用法等方法提高了检测的效率与灵敏度,检测结果基本能达到国际标准,为食品及饲料中有害物质的分析提供了技术条件,有利于卫生部门对饲料及食品安全进行质量监督。文章论述了气相色谱法在食品及饲料中有害物质检测中的应用。     

水中10种挥发性有机物的快速检测

采用吹扫捕集与快速气相色谱 飞行时间质谱联用,建立测定水中10种石化行业常见挥发性有机物（VOCs）的吹扫捕集-快速气相色谱-飞行时间质谱的分析方法。通过质谱定性,选定目标物的特征离子,运用内标法定量,采用DN-624（20 m×0.18 mm×1 μm）快速毛细管色谱柱,在10 min内完成对水中10种VOCs的分析,在保证各目标物灵敏度和分辨率不受影响的同时,分析时间从标准方法的17 min降至10 min。该方法的线性、精密度与检出限满足标准方法HJ639—2012《水质挥发性有机物的测定吹扫捕集／     

气相色谱质谱联用法测定韭菜和姜等复杂蔬菜基质中嘧菌酯残留

【目的】建立韭菜、姜等复杂蔬菜基质中嘧菌酯的残留量的气相色谱质谱联用测定法。【方法】以乙腈为提取溶剂,经分散固相萃取净化,采用气相色谱质谱联用法测定残留量。【结果】结果表明,嘧菌酯在0.02~1mg/kg范围内呈线性关系,相关系数大于0.995。高中低档标准添加回收率为110%~130%,相对标准偏差(RSD)<12%,方法检出限为0.0067 mg/kg。该方法简便快捷,可作为复杂蔬菜基质中嘧菌酯的检测方法。     

Pure＆Trap、GC—MS测定水中挥发性有机物

吹扫/捕集、气相色谱-质谱联用分析技术是能同步进行定性定量检测经处理的饮用水、水源水或水处理工艺中任何阶段的水中可吹扫的VOCs测定通用分析方法，其中包括四种三卤甲烷-消毒剂副产物。针对这些化合物具有高挥发性和低水溶性，可用吹扫脯集的方法把他们有效地从水样中转移出来，采用气相色谱-质谱进行分离定性定量。本文采用吹扫脯集、气相色谱-质谱联用方法对水中60种VOCs进行了测试，结果表明，该方法是快速分析水中VOCs的有效手段。     

手持X射线荧光光谱法在矿山生产中的应用

通过手持X射线荧光光谱法与化学分析容量法的对比研究,显示手持X射线荧光分析仪具有较好的准确性。该仪器可用于铜品位3%,锌品位8%的样品分析,在日常工作中使用手持X射线荧光光谱法测量样品是一种快捷、简便、经济和有效的工作方法。     

Identification and determination of trace organic substances in tap water by computerized gas chromatography-mass spectrometry and mass fragmentography

Tap water was examined for the presence of trace organic substances by using the Amberlite XAD-2 resin adsorption method, computerized gas chromatography-mass spectrometry, high resolution mass spectrometry, and mass fragmentography. Chemical ionization and field desorption mass spectrometry were used for the analysis of high polar compounds. By these methods, a large number of alkylbenzenes, odorous components (menthol, acetophenone and its derivatives, and benzaldehyde), and several plasticizers (dimethyl phthalate, diethyl phthalate, dibutyl phthalate, di(2-ethylhexyl) phthalate, di(2-ethylhexyl) adiptate, and tributyl phosphate) were found in a concentration of 1–240 parts per thousand million.     

Component analysis of rigid polyurethane foams

A procedure is described for the analysis of the component parts of a rigid polyurethane foam. The technique can be used to identify the polyol, isocyanate, fire retardant, and blowing agent used in foam manufacture when less than 0.5 g of material is available. Techniques of pyrolysis/gas chromatography/mass spectrometry (Py-GC-MS), electron impact (EI) and chemical ionization/mass spectrometry (CI-MS), and high pressure liquid chromatography (HPLC) were essential for component characterization and identification. Foam samples were base-hydrolyzed and the resulting polyols and amines were identified by EI and CI-MS, and HPLC. A combination of CI-MS, Py-GC-MS, and halogen and phosphorus-sensitive chromatographic detectors were used for qualitative and quantitative analysis of the fire retardant. The blowing agent was determined by Py-GC-MS. The composition of the foam was confirmed by the synthesis and characterization of a chemically identical foam using known starting materials.     

Analysis of chlorinated styrenes in environmental samples using negative ion chemical ionization mass spectrometry

A method for the separation and identification of chlorinated styrene isomers with fully chlorinated aromatic nuclei in environmental samples is presented. Gas chromatography combined with negative ion chemical ionization mass spectrometry is used. The method has been applied to a combined fish liver and filét extract. All the possible chlorostyrenes with fully chlorinated aromatic nuclei were detected in the sample.     

Colorimetric flow-injection analysis of dissolved iron in high DOC waters

An iron flow-injection analysis system has been optimized for the analysis of iron in waters high in dissolved organic carbon. The method detects either dissolved iron(II) or total dissolved iron with a detection limit of 10 nM, precision of 0.65% at 1 microM, and a dynamic range of four orders of magnitude. There are minimal interferences (< 1%) from other metals at environmental concentrations. The iron(II) method measures iron(II) in the presence of excess iron(III) with less than 1% interference. When used with pre-acidified samples, the total dissolved iron method agrees well with electrothermal atomic absorption spectrometry for a variety of natural waters with a range of dissolved organic carbon (3-36 mg C/L) and iron (1-28 microM) concentrations. When used with samples at their ambient pH, the total dissolved iron method detects dissolved iron, but not colloidal iron (size fraction 0.05-0.45 micron).     

Assessment of total uncertainty in cocaine and benzoylecgonine wastewater load measurements

To check the effectiveness of campaigns preventing drug abuse or indicating local effects of efforts against drug trafficking, it is beneficial to know consumed amounts of substances in a high spatial and temporal resolution. The analysis of drugs of abuse in wastewater (WW) has the potential to provide this information. In this study, the reliability of WW drug consumption estimates is assessed and a novel method presented to calculate the total uncertainty in observed WW cocaine (COC) and benzoylecgonine (BE) loads. Specifically, uncertainties resulting from discharge measurements, chemical analysis and the applied sampling scheme were addressed and three approaches presented. These consist of (i) a generic model-based procedure to investigate the influence of the sampling scheme on the uncertainty of observed or expected drug loads, (ii) a comparative analysis of two analytical methods (high performance liquid chromatography-tandem mass spectrometry and gas chromatography-mass spectrometry), including an extended cross-validation by influent profiling over several days, and (iii) monitoring COC and BE concentrations in WW of the largest Swiss sewage treatment plants. In addition, the COC and BE loads observed in the sewage treatment plant of the city of Berne were used to back-calculate the COC consumption. The estimated mean daily consumed amount was 107 ± 21 g of pure COC, corresponding to 321 g of street-grade COC.     

Combined application of high-pressure liquid chromatography and field desorption mass spectrometry for the determination of biocides of the phenylurea- and carbamate-type in surface water

A novel method for the indentification and determination of biocides in environmental samples is introduced. The combined application of high-pressure liquid chromatography and field-desorption mass spectrometry has been used for two years to monitor herbicides of the phenylurea-, carbamate- and thiocarbamate-type in Rhine river water. Water samples of 2 liter were used to identify and determine 10 to 150 ng of the biocides (ppt level concentrations). For the HPLC determination a precision of ± 5% and an accuracy of ± 10% was achieved. Although field-desorption mass spectrometry is a costly and somewhat complex analytical technique, the short analyses time (～10 min), the small sample consumption (～ng), the high selectivity obtained in multicomponent mixtures and he unmatched reliability for biocide identification are essential advantages.     

电感耦合等离子体质谱法测定模拟玻璃固化体中Cs2O的含量

建立了一种电感耦合等离子体质谱法（ICP-MS）测定玻璃固化体中铯含量的方法。该方法从ICP-MS的背景控制、内标物选择、质谱干扰等方面进行了优化。试验结果表明，该方法检出限为0.18mg/kg，相对标准偏差（n=12）为0.48%～4.11%，加标回收率为98%～102%，可用于玻璃固化体中铯含量的测定。     

Analysis of triclosan and 4n‐nonylphenol in Colombian reservoir water by gas chromatography‐mass spectrometry

In this work were determined triclosan and 4n‐nonylphenol in water from a reservoir that is used to provide water to a purification plant in an important city in Colombia. The analytical methodology was validated using solid‐phase extraction and analysis by gas chromatography‐mass spectrometry (GC‐MS). The analysis by GC‐MS showed good linearity in the range of 0.05–5 μg/L for both compounds. Recoveries from 79 to 109% and standard deviations of 2.5–7.7 for low concentrations and from 3.8 to 9.6 (n = 5) for high concentrations were obtained for both compounds. In Colombia, this is the first time that these compounds have been analysed in water supplying of a drinking water treatment plant. The validated method was applied to the analysis of 27 samples collected in August 2010 in 11 locations from the reservoir and in the influent and effluent of the drinking water treatment plant. In total, seven samples were found to contain triclosan.     

X射线荧光光谱法测定"芝麻白"成份的研究

采用玻璃熔融制样技术、X射线荧光光谱仪测定芝麻白花岗石的化学组成,可获高准确度和高精密度的分析结果,测定值与化学法及推荐值相符,重复10次测定主、次量纽分的RSD<0.64％。 方法简便快捷,分析时间仅为传统湿法化学分析的1/8,应用于花岗石的测定,结果满意。