固相微萃取-气相色谱在水中有机污染物测定中的应用

固相微萃取技术是一种新型的无溶剂的样品前处理方法,集取样、萃取、富集、进样于一体,具有无溶剂、可直接进样、操作简便快捷、灵敏的特点。简述了固相微萃取技术原理,综述了SPME与GC联用在水中有机污染物测定中的应用。具体介绍了该技术在苯系物、酚类化合物、多环芳烃、有机氯化物及其它有机污染物分析中的应用,并提出了该技术的发展趋势及应用展望。     

SPME-GC同时测定地表水环境质量标准特定项目中硝基苯类和氯苯类化合物

针对地表水特定项目有机物中硝基苯类和氯苯类的测定,采用固相微萃取(SPME)前处理技术,用毛细管色谱柱进行色谱分离,用ECD检测器进行测定。SPME富集效率达118~1352倍,检出限为0.00004~0.05μg/L,方法的线性相关系数为0.9963~0.9999,RSD为2.0%~11.0%,加标回收率为87.0%~108%,所有技术参数均可满足地表水环境质量标准。该方法简单、快捷、无污染且省时省力,具有较好的推广性。     

C_8-SBA-15新型介孔涂层SPME-HPLC联用测定水样中的芘

以辛基键合SBA-15为固相微萃取（SPME）的吸附涂层,考察了吸附和解吸时间、萃取温度、搅拌速率对SPME效率的影响。该方法的线性范围为3.0—320μg/L,检出限为0.5μg/L,依据此方法测定了环境水样中芘,具有灵敏度高和精密度好的特点。     

新型动态针捕集阱技术分析大气中低浓度的VOCs

本研究针对大气中挥发性有机物（VOCs）浓度低,难于分析等特点,以Carboxen 1000作为吸附剂,制作一种新型动态针捕集阱（needle trap）装置,可用于主动富集大气中低浓度VOCs.该装置与气相色谱-质谱（GC-MS）联用,操作简单、无需溶剂、容易定性定量.选择空气中苯系物（BTEX）为目标化合物,对needle trap装置从设计原理到实际应用进行了详细分析,将萃取条件与穿透体积等实验条件进行优化,建立了needle trap吸附提取空气中BTEX的最佳条件.结果表明,方法检出限低至0.05ng·mL-1,加标回收率为86.5%～110.5%,符合外场采样要求.     

新型固相微萃取头测定胶粘剂中苯及其同系物

结合分子印迹技术与溶胶-凝胶技术,自制新型联苯分子印迹溶胶-凝胶聚合物涂层固相微萃取头,结合顶空固相微萃取-气相色谱法(HS-SPME-GC),测定水溶液中的苯及其同系物。结果表明,该方法精密度良好(RSD<5%),线性范围超过2个数量级,最低检出限达到10ng/mL。运用该法对市售胶粘剂中苯及其同系物进行检测,结果令人满意。     

Solid-phase microextraction coupled with atomic emission spectroscopy--rapid screening for volatile chlorinated compounds

Solid-phase microextraction (SPME) coupled with atomic emission spectroscopy was evaluated as a rapid screening tool for volatile halogenated compounds in water samples. After extraction, the SPME fiber was introduced to the injector where the analytes were rapidly and efficiently desorbed. The analytes entered the detector over a short period of time and produced one well-defined analyte signal. Element selective responses were measured to confirm the presence and to roughly estimate the content of volatile compounds. The total time for extraction and detection was approximately 5 min, which makes this method a rapid and promising technique for determination of total amount of volatile halogenated compounds. The proposed technique may prove useful as a screening test in order to pinpoint the samples that need further assessment by capillary gas chromatography.     

固相微萃取技术及其应用现状综述

固相微萃取技术（SPME）在固相萃取（SPE）基础上发展而来。作为一种较新的样品前处理技术,固相微萃取技术具有操作简单、快速、集采样、萃取、浓缩和进样于一体等诸多优点,目前已被广泛应用。阐述了 SPME 的技术原理、操作流程、影响因素、应用领域和新的进展。着重指出 SPME 在环境有机污染物分析中具有广泛的应用前景。     

南极长城湾附近和台湾以南部分海域水样中丁基锡化合物分析

对南极长城站附近水域及中国台湾以南海域采集的水样进行了分析研究。应用顶空固相微萃取（SPME）技术富集丁基锡化合物，由气相色谱分离后，表面发射火焰光度检测器测定，在两个水域均未检出三丁基锡，但存在一定量的三丁基锡降解产物，即二丁基锡和一丁基锡。     

固相微萃取-毛细管气相色谱法快速分析水中酞酸酯

用固相微萃取富集水中酞酸酯，毛细管气相色谱分离分析，整个分析过程只需50min，检出限可达0.01-40.0μg／L，实验表明，固相微萃取是一种快速、简便、集萃取浓缩进样于一体的样品前处理技术，具有分析时间短、灵敏度高、无需有机溶剂的优点，已用于地面水源、海水、饮用水中酞酸酯含量的测定。     

Release of sex pheromone and its precursors in the pine sawfly Diprion pini (Hym., Diprionidae)

Summary. The first identification of a sex pheromone of a pine sawfly (Hymenoptera, Diprionidae) dates back almost thirty years. Since then, female-produced pheromones of over twenty diprionid species have been investigated by solvent extraction followed by separation and identification. However, no study has shown what the females actually release. Collection of airborne compounds using absorbtion on charcoal filter as well as solid phase microextraction (SPME) followed by analysis employing gas chromatography combined with mass spectrometry (GC-MS), revealed an unusual system in Diprion pini, in which the pheromone precursor alcohol, 3,7-dimethyl-2-tridecanol, is released together with acetic, propionic, butyric and isobutyric acids. The corresponding acetate, propionate and butyrate esters of 3,7-dimethyl-2-tridecanol were also found in the samples. All esters were electrophysiologically active, and the propionate and isobutyrate were attractive in trapping experiments. Based on these and earlier reported results, it seems that at least in part of its range, the pheromone response of D. pini is not very specific with regard to the functional group, as long as this is an ester.