A novel solid-phase microextraction (SPME) fiber was prepared by coating an HPLC β-cyclodextrin bonded silica stationary phase (CDS) on the surface of a fused-silica fiber. The fiber was evaluated for the determination of five phenol compounds (phenol, 2,4-dimethylphenol, 4-nitrophenol, 3-chlorophenol, 4-methylphenol). Compared with commercially available polymer coatings, the CDS coating showed high sensitivity and fast velocity of mass transfer for phenol compounds because of its porous structure and a unique molecular structure of β-cyclodextrin. In addition, the CDS coating was proved to be very stable at a relatively high temperature (up to 300℃). The method was suitable for the determination of phenol compounds in aqueous samples. The determination of 4-nitrophenol in soil by microwaveassisted extraction (MAE) coupled to solid-phase microextraction was also investigated.

用反向C固相萃取小柱对葡萄酒进行了预处理，然后用BSTFA硅烷化试剂对萃取物进行了衍生化处理，用气相色谱/质谱对葡萄酒中顺式、反式白藜芦醇进行了同时测定，建立了定量分析方法。对方法的精密度和回收率进行了测定，方法的相对标准偏差分别为4.48%（顺式）和5.23%（反式）。顺式、反式白藜芦醇的平均回收率分别为94.4%和97.6%。并对10种国产葡萄酒和两种进口葡萄酒样品进行了测定。对白藜芦醇的生理活性也进行了实验，初步探讨了白藜芦醇对大鼠血管平滑肌细胞（VSMC）、大肠癌细胞株Lovo细胞和小鼠成纤维株3T3细胞的生长生殖活性的影响，观察了其形态变化。

首次报道了应用聚二甲基硅氧烷纤维作为固相微萃取的萃取头，色-质联用法快速测定海水中角鲨烯的方法。研究了萃取平衡时间、搅拌速度、介质离子强度、pH值、以及解吸温度、解吸时间等条件对测定效果的影响。该方法具有简便、快速、灵敏度高、不使用有毒有机溶剂的优点，其检测限为0.005μg/L，相对标偏差介于4.9%～6.2%，回收率在92.0%～95.0%之间，能有效地应用于海水中角鲨烯的测定。海水中角鲨烯浓度的变化，可能作为赤潮预报的一个指标，通过对其变化的监测，为海洋赤潮的预报、防治提供科学依据。

介绍了微波辅助萃取技术的特点和装置，综述了近年来微波辅助萃取技术在环境分析和药物提取中的应用，并展望了微波辅助萃取技术的应用前景和发展方向。引用文献74篇。

A new method for the trace analysis of trans-resveratrol in wine was studied by developing a silylation on the fibre coating following solid-phase microextraction (SPME) combined with GC/MS. The silylation was performed directly by placing the fibre into the headspace of silylating reagent. The method is rapid and sensitive without going through laborious sample preparation. The effects of fibre selection, extraction and desorption times as well as the extraction temperature were studied. The optimum conditions of derivatization time and temperature were also studied. The derivatization was carried out at room temperature without damaging the fibre coating. A linear response of trans-resveratrol over a concentration range of 10ng l-1-1 mg l-1 with a correlation coefficient of 0.9997 and detection limit 5ng l-1 (3s criteria) were obtained. The analytical recoveries in wine ranged from 84 to 106% with precision below 10% relative standard deviation (R.S.D.).

有机氯农药（Ops）严重干扰多氯联苯（PcBs）的测定，本文采用微波加热技术将Ops碱解，在优化的实验条件下能完全消除六六六（HCH）、双对氯苯基三氯乙烷（DDT）、二氯二苯二氯乙烷（DDD）的干扰，二氯二苯二氯乙烯（DDEE）、艾试剂（A1drin）、狄试剂（Dieldrin）也有一定数量的减少，狄试剂经浓硫酸处理后其干扰完全消除。通过对合成土壤样品的处理，表明该法能有效地碱解Ops，消除其对测定PcBs的干扰；并能在碱解Ops的同时萃取PcBs，PcBs回收率为84.1%，相对标准偏差为2.7%。本方法快速、高效，减少了有机溶剂的使用量。

本文在有效地控制和消除基体干扰的基础上，探讨了Ag，As，Au，Bi，Cd，Co，Cr，Cu，Fe，Ga，Hg，Mn，Mo，Ni，Sb，Pb和V元素的理论原子化效率与原子化温度的关系。研究表明：元素的理论原子化效率是原子化温度的函数，在一定的原子化温度范围内，理论原子化效率与原子化温度呈线性递增关系，对研究的十八个元素其线性的相关系数在0.9940～0.9993之间，且斜率大部分在0.06～0.07之间，说明在一定的原子化温度范围内，理论原子化效率随原子化温度变化的斜率是相近的。

An efficient and noninvasive method consisting of an original sampling device, solid phase microextraction (SPME) and gas chromatography–mass spectrometry (GC-MS) was developed to analyze volatile organic emanations from the skin of human arms. The emanations were sampled by SPME connected with the active sampling device for 30 min and transferred into GC-MS immediately for the consequent analysis. The sampling projects for 15 candidates were scheduled in both winter and spring with the same optimized conditions. Thirty-five compounds were finally identified according to various degrees of certainty. Different emission behaviors specified with principal component analysis (PCA) and similar fingerprint characteristics were observed clearly by comparisons of chromatograms of different seasons. Top ten emanations contributing to characteristics in different seasons were attempted to be described using comparisons based on common model strategy. The large amounts of experimental data were all handled by the corresponding chemometrics strategies with the homemade chromatographic data processing system. The results suggest that the analysis based on fingerprint characteristics of human skin emanations could provide useful and important clues to reveal biomarkers among the mixture of human skin emanations.

A novel poly(dimethylsiloxane)/β-cyclodextrin (PDMS/β-CD) coating was prepared for solid-phase microextraction (SPME) in the form of membrane instead of fiber. The surface of the membrane was uniform and has not gel cracking after dipped into methanol, acetonitrile and acetone. Non-polar polycyclic aromatic hydrocarbons (PAHs) and polar phenolic compounds were used to evaluate the character of the PDMS/β-CD solid-phase microextraction membrane by direct extraction and solvent desorption, followed by GC-MS analysis. Parameters that affect the membrane extraction process were investigated, which included the matrix of sample, extraction time, desorption solvent and time. For PAHs, the linearitywas from 0.10 to 1000μg1-1. The limit of detection (LOD)was in the range of 0.01-0.2μg1-1. The repeatability was in the range of 5.4-9.3%. For phenolic compounds, the linearity was from 0.10 to 5000μg1-1 and LOD varied from 0.02 to 1.5μg1-1. Compared with the SPME fiber, the SPME membrane has a large extraction capacity, low cost of preparation. The sensitivity can be further increased by developing large-volume-injection or thermal desorption technique.

采用微波消解技术处理样品，用石墨炉原子吸收光谱法测定，对消解试剂和微波消解条件进行了筛选和优化，研究了石墨炉原子吸收的测定条件。研究表明，以HNO3+HClO4+H2O2作为微波消解试剂最佳，在基体改进剂NH4H2PO4存在下，可有效地消除基体的影响，建立了微波溶样2原子吸收光谱法测定中药石蒜中Cd，Cr和Pb的方法，其Cd，Cr和Pb的测定检出限分别为0.0667，1.22和0.810μg•L-1。将该法应用于石蒜样品中Cd，Cr和Pb的测定，结果令人满意，RSD小于3.1%，回收率在83.8%～1.8%之间。