顶空气相色谱-质谱联用技术的应用进展

顶空分析作为一种无有机溶剂萃取的样品处理技术,通常与气相色谱-质谱（GC-MS）技术结合用来分析复杂基质中的挥发性有机物。顶空气相色谱-质谱（HS-GC-MS）技术具有快速、高效、环保、灵敏度高等特点,在常规分析中发挥着重要作用。该文简要概述了静态顶空、动态顶空、顶空固相微萃取分析以及GC-MS联用技术,并介绍了整个顶空分析系统的影响因素和优化过程。根据基质类型的分类,综述了HS-GC-MS在食品和饮料、环境、生物等样品中的应用实例。HS-GC-MS的研究非常活跃,不断出现新应用,在分析挥发性有机物方面具有广阔前景。     

顶空-气相色谱法快速测定化工固体废物中16种挥发性有机物

采用顶空-气相色谱法快速测定化工固体废物中16种挥发性有机物的含量。顶空加热平衡温度为80℃,顶空加热平衡时间为30min。用HP-FFAP色谱柱(30m×0.32mm,0.25μm)分离,氢火焰离子化检测器检测。16种挥发性有机物的的质量浓度在一定范围内与其对应的峰高呈线性关系,方法的检出限为0.001～0.009mg·L~(-1)。方法用于化工固体废物样品的分析,加标回收率为82.5%～115%,测定总量的相对标准偏差(n=6)为1.9%～9.1%。     

顶空/气相色谱-质谱法分析方便面印刷包装材料中挥发性有机物

利用顶空/气相色谱-质谱(HS/GC-MS)联用法对袋装方便面印刷包装材料中7种挥发性有机物(异丙醇、乙酸乙酯、苯、乙酸丁酯、乙苯、间/对二甲苯、邻二甲苯)进行了检测分析.优化的实验参数为:平衡温度80℃,平衡时间40 min.本方法线性关系良好,7种挥发性有机物的相关系数均大于0.9991,检出限为0.004～0.0...     

基于准确质量测定和保留指数的GC-MS分析薄荷挥发性成分

采用顶空-气相色谱-四极质谱法和顶空-气相色谱-飞行时间质谱法对薄荷挥发性成分进行了检测, 分别从薄荷茎和叶中鉴定出39种和64种挥发性组分, 其中以酮类和萜烯类化合物为主. 本定性分析策略在复杂样品挥发性成分的定性分析中具有良好的应用前景.     

顶空气相色谱法测定水中挥发性有机物的精密度控制

试验证明在顶空采样-气相色谱法测定水中挥发性有机物时出现的分析结果重现性差的原因在于所采用HP 7694E型顶空自动进样器加热方法的设计缺陷,对此提出了改进措施。通过用水浴预加热使整批样品温度达到与检测室温度（25±2）℃接近,并选择顶空采样条件为55℃及15min。按此条件对三氯甲烷、一溴二氯甲烷、二溴一氯甲烷及三溴...     

静态顶空与顶空-SPME-气质联用法在烟用香料分析中的比较

对静态顶空和顶空-SPME-气相色谱-质谱联用法在烟用香料分析中的应用进行了比较。通过比较发现顶空-SPME法更适合于挥发性成分含量较低的香料的研究和质量控制。     

顶空-气相色谱-质谱法测定卫生巾中55种挥发性有机物的含量

提出了顶空-气相色谱-质谱法(HS-GC-MS)测定卫生巾中55种挥发性有机物含量的方法。将卫生巾样品剪碎,采用自动顶空进样方式,于110℃下低速振荡15 min,用DB-624色谱柱(60 m×0.25 mm, 1.40μm)分离和质谱检测样品中55种挥发性有机物,外标法定量。结果表明,55种挥发性有机物的质量分数均在0.080～2.000μg·g^-1内与其对应的峰面积呈线性关系,测定下限(10S/N)为0.000 3～0.031 0μg·g^-1。按照标准加入法进行回收试验,回收率为81.3%～119%,测定值的相对标准偏差(n=6)均小于9.0%。方法用于实际卫生巾样品的分析,结果显示多种挥发性有机物被检出,1,3,5-三甲苯的检出率高达89.3%,氯甲烷检出量高达10.688μg·g^-1。     

动态微波辅助顶空固相微萃取-气相色谱-质谱法测定芹菜叶中的化学成分

采用动态微波辅助顶空固相微萃取结合气相色谱-质谱法测定芹菜叶中的挥发性和半挥发性化学成分。对水蒸气蒸馏、顶空固相微萃取、微波辅助顶空固相微萃取、动态微波辅助顶空固相微萃取等4种不同的前处理方法进行了比较,通过气相色谱-质谱分析,分别鉴定出20,17,36,41种化学成分,主要化合物为α-月桂烯、柠檬烯、β-顺式罗勒烯、β-芹子烯和(Z)-3-己烯-1-醇等。结果表明:动态微波辅助顶空固相微萃取是一种简单、快速、易操作,无需净化步骤,消耗样品量少,对于沸点较高的半挥发性物质的萃取效果优于微波辅助顶空固相微萃取的方法,可用于分析各类植物中的挥发性和半挥发性化学成分。     

顶空固相微萃取-气相色谱-质谱联用分析麦冬中有机挥发物

采用顶空固相微萃取-气相色谱-质谱联用(HS-SPME-GC-MS)分析麦冬中挥发性成分,对萃取温度、时间、脱附时间及样品用量等条件进行了优化,方法所得结果与同时蒸馏萃取-气相色谱-质谱联用(SDE-GC-MS)方法比较,相对含量较高的成分基本一致.固相微萃取方法可应用于麦冬中有机挥发性成分的快速分析.     

顶空液相微萃取/气相色谱-质谱对中药枳壳中有机挥发物的快速分析

建立了顶空液相微萃取/气相色谱-质谱联用测定中药枳壳中有机挥发物的方法.在顶空液相微萃取实验条件优化的基础上,确定了最佳实验条件:以正辛烷作为有机萃取剂,体积为2 μL,样品用量为0.3 g,液滴距离样品表面0.8 cm处,萃取8 min后直接进样.与固相微萃取/气相色谱-质谱法相比,顶空液相微萃取法定性了30种成分,固相微萃取法定性了24种成分,顶空液相微萃取法操作简单、快速,实验结果灵敏度更高,且萃取效率高,重复性好,可用于中药枳壳中有机挥发物的快速分析.     

A New Cell for Single Sided Headspace Sampling and Evaluation of Barrier Function in Laminated Paperboard

A new cell for single sided headspace sampling has been developed for the analysis of volatile organic compounds from food packaging paperboard and laminated paperboard. The cell, which samples the volatile organic compounds over a selected surface, is useful for determining the barrier function of laminated paperboards with respect to volatile compounds. The analysis of volatile organic compounds is carried out by purge and trap capillary gas chromatography in combination with mass spectrometric detection and compound identification. The new sampling cell was constructed to facilitate specific analysis of organic compounds from only one side of a laminated paperboard. The construction and the operating principles of the new sampling device are described. The repeatability of the single sided headspace procedure was found to be quite good. Relative standard deviations of about 5–7% were obtained for the major compounds quantified in replicate headspace analyses of a laminated paperboard. The volatile compounds released from the inner side of a food packaging paperboard sample with different surface composition on the two sides were determined. The barrier function against volatile organic compounds of some laminated paperboards was investigated employing the new headspace cell.     

Isolation and preconcentration of volatile organic compounds from water

Methods for the isolation and/or concentration of volatile organic compounds from water samples for trace organic analysis by gas chromatography are reviewed. The following basic groups of methods are discussed: liquid-liquid extraction, adsorption on solid sorbents, extraction with gas (gas stripping and static and dynamic headspace techniques) and membrane processes. The theoretical bases of these methods are discussed. Experimental arrangements for the isolation and/or concentration of volatile compounds from water are presented and discussed with respect to their efficiency. The applicability of the described methods to the isolation and/or concentration of various organic compounds from waters of various origins is discussed.     

Sampling volatile organic compounds using a modified solid phase microextraction device

Headspace solid phase microextraction (headspace SPME) has been demonstrated to be an excellent solvent-free sampling method. One of the major factors contributing to the success of headspace SPME is the concentrating effect of the fiber coating toward organic compounds. The affinity of the fiber coating toward very volatile analytes, such as chloromethane, may, however, not be large enough for detection at the parts per trillion concentration level. Static headspace analysis, on the other hand, is very effective for these very volatile compounds. As analyte volatility decreases, the sensitivity of static headspace analysis drops. The complementary nature of these two sampling methods can be exploited by combining the SPME device with a gastight syringe. The sensitivity of the new sampling device is better than that of SPME for very volatile compounds or that of static headspace analysis for less volatile compounds. This new method can sample a wide range of compounds from chloromethane (b.p. −24°C) to bromoform (b.p. 149°C) with estimated limits of detection at the low parts per trillion level.     

Using solid-phase microextraction combined with gas chromatography-mass spectrometry for the study of the volatile products of biosynthesis released by plants and microorganisms

Published data on the methods and results of study of profiles of volatile biologically active compounds are summarized and discussed. The leading role of gas chromatography-mass spectrometry combined with headspace solid-phase microextraction as an optimum analytical method for determining the qualitative and quantitative composition of volatile organic compounds in in vivo experiments is substantiated. The results of investigation of volatile organic compounds produced by micromycetes of the genus Fusarium are reviewed.     

Dynamic headspace analysis of solid waste materials

A dynamic headspace stripping technique for the extraction of volatile organic compounds has been applied to a variety of solid and semisolid waste materials. A simple glass apparatus accommodates a wide range of sample sizes and allows for the volatiles to be stripped at elevated temperatures. Concentration on Tenax, followed by thermal desorption and analysis by fused silica capillary gas chromatography provides detailed information on the volatile content of waste samples of widely differing matrix composition.     

Analysis of organic compounds in environmental samples by headspace solid phase microextraction

The analysis of samples contaminated by organic compounds is an important aspect of environmental monitoring. Because of the complex nature of these samples, isolating target organic compounds from their matrices is a major challenge. A new isolation technique, solid phase microextraction, or SPME, has recently been developed in our laboratory. This technique combines the extraction and concentration processes into one step; a fused silica fiber coated with a polymer is used to extract analytes and transfer them into a GC injector for thermal desorption and analysis. It is simple, rapid, inexpensive, completely solvent-free, and easily automated. To minimize matrix interferences in environmental samples, SPME can be used to extract analytes from the headspace above the sample. The combination of headspace sampling with SPME separates volatile and semi-volatile analytes from non-volatile compounds, thus greatly reducing the interferences from non-target compounds. This paper reports the use of headspace SPME to isolate volatile organic compounds from various matrices such as water, sand, clay, and sludge. By use of the technique, benzene, toluene, ethyl-benzene, and xylene isomers (commonly known as BTEX), and volatile chlorinated compounds can be efficiently isolated from various matrices with good precision and low limits of detection. This study has found that the sensitivity of the method can be greatly improved by the addition of salt to water samples, water to soil samples, or by heating. Headspace SPME can also be used to sample semi-volatile compounds, such as PAHs, from complex matrices.     

Improved sensitivity of headspace gas chromatography for organic aromatic compounds

Summary The effect of adding an electrolyte and increasing the temperature on the preconcentration of volatile compounds in headspace analysis has been investigated. Quantification of the interactive effects of temperature and addition of salt on the vapor concentration is of interest for the determination of trace organic impurities in pharmaceutical base materials. This study was undertaken to investigate the quantitative effects of the addition of salts alcohols, and acetone, and of increasing the temperature on the vapor concentrations and distribution coefficients of volatile aromatic compounds (benzene, toluene, ando-xylene). It was found that the concentration of aromatic compound residues in the headspace could be increased by adding an inert salt to the water, but this effect was not very significant because of the low orginal solubility of the aromatic compounds in water. The reverse effect can be achieved by use of polar organic additives; this can be explained by the high polarizability of aromatic compounds and their greater solubility in the presence of these solvents. Presented at Balaton Symposium on High-Performance Separation Methods, Siófok, Hungary, September 1–3, 1999.     

固相微萃取-气相色谱/同位素质谱法测定水中挥发性有机物单体碳同位素

建立了采用75μm碳分子筛/聚二甲基硅氧烷(CAR-PDMS)纤维的固相微萃取-气相色谱/同位素质谱联用方法测定水中挥发性有机污染物碳同位素。使用浸入式固相微萃取和顶空固相微萃取方法进行实验确定在低浓度条件下最佳δ13C测试方法。通过使用顶空固相微萃取前处理技术进行单体同位素分析分析灵敏度更高,应用CSIA技术对1,2-二氯乙烯,三氯乙烯,四氯化碳进行单体同位素分析,方法的检出限为70μg/L,与样本的标准偏差小于0.3‰。该法适用于水体中微量挥发性有机污染物的同位素组成测定。     

顶空气相色谱法测定化妆品中15种挥发性有机溶剂残留

建立了化妆品中15种挥发性有机溶剂残留的顶空气相色谱测定方法。样品经60 ℃、30 min静态顶空后,采用气相色谱-氢火焰离子化检测器进行检测,外标法定量。加标回收试验结果表明: 15种挥发性有机溶剂残留平均回收率为62.8%～116%,相对标准偏差均小于5%。方法的检出限为0.09～0.68 mg/kg。该方法可有效克服基体干扰,一次进样可同时分离和测定化妆品中15种挥发性有机溶剂,准确灵敏,简单快速,适用于化妆品中挥发性有机溶剂残留的检测。