水中联苯胺分析方法研究进展

对水中联苯胺的萃取方法及检测方法进行了综述。水中联苯胺的萃取方法主要为液–液萃取法和固相萃取法,检测方法主要有分光光度法、流动注射分析法、离子色谱法、气相色谱–质谱法、高效液相色谱法和高效液相色谱–质谱法等,对这些检测方法的优缺点进行了比较。对水中联苯胺的萃取技术及检测方法发展前景进行了展望。     

畜产品中激素残留检测方法的进展

目前畜产品中依然存在激素残留的严重现象,因此,对畜产品激素残留的检测有着重要的意义。本文讨论了检测畜产品中激素残留的前处理方法,并针对畜产品中激素残留检测技术如气相色谱法、高效液相色谱法、液质联用法、气质联用法、毛细管电泳技术、超临界流体色谱联用技术、放射免疫分析法等进行论述。     

药物中磺酸酯类基因毒性杂质测定方法研究进展

介绍磺酸酯类基因毒性杂质的分析方法,包括高效液相色谱法、液相色谱-质谱联用法、气相色谱法和气相色谱-质谱联用法等。高效液相色谱法操作简单,应用广泛,能实现绝大多数化合物的分离、分析;液相色谱-质谱联用法具有灵敏度高、准度高、特异性高等特点;气相色谱应用于易分离气体和易挥发的成分的检测,灵敏度高,专属性强;气相色谱-质谱联用法具有分析速度快、分离效能好、灵敏度高、选择性强的特点。开发通用、简便、灵敏度高的分析检测方法,为更好地监测磺酸酯类基因毒性杂质提供理论参考。     

单糖和二糖的定量分析的研究进展

综述了单糖和二糖的常用定量分析方法,如重量法、滴定法、旋光法、比色法,薄层扫描法、近红外光谱法、拉曼光谱法、气相色谱法、气相色谱-质谱联用法、液相色谱法、液相色谱-质谱联用法、离子色谱法和毛细管电泳法等,详细介绍了各方法的特点、应用及最新研究进展,并对其发展前景进行了展望。     

环境中手性污染物对映体分析方法的研究进展

手性污染物对映体尽管具有相似的物理化学性质,但在环境中的吸附、转移、降解等过程往往存在一定差异。生态安全问题与人类健康密切相关,因此,对手性环境污染物进行对映体水平上的分离分析是十分重要的研究课题。目前,国内外对环境中的手性污染物已开展了相关研究,然而全面评述相关分析测定方法的新进展鲜有报道。本文主要对环境中手性污染物的种类以及近5年环境中手性污染物的分析检测技术如液相色谱-质谱联用法、气相色谱-质谱联用法、毛细管电泳法、超临界流体色谱-质谱联用法等进行了归纳、综述和展望,为后续手性污染物的分析检测提供依据和参考。     

食品中角鲨烯样品前处理与检测方法研究进展

角鲨烯是一种存在于动物、植物、微生物体内的小分子功能活性脂质,由于具有抗氧化、防癌抗癌、抗辐射、携氧、皮肤保湿和抑制微生物生长等多种生物活性功能,被广泛应用于功能食品、医药产品和化妆品的开发。因此,不同食品中角鲨烯含量的分析技术一直是国内外学者研究的热点与重点。该文综述了不同食品中角鲨烯的样品前处理方法,包括超临界二氧化碳萃取法、固相萃取法、固相微萃取法、皂化法、有机溶剂提取法和分步结晶法等以及气相色谱法、液相色谱法和气相色谱-质谱联用法等检测方法在角鲨烯分析中的应用,并对其发展趋势进行了展望,为食品中角鲨烯的分析提供参考与借鉴。     

水杨酸在羟基自由基检测中的应用

对近二十年来国内外有关水杨酸为捕捉剂的羟基自由基的测定方法,包括高效液相色谱法及其联用法、比色法、气相色谱法、气相色谱-质谱法、液相色谱-质谱法等进行了综述,引用文献25篇。     

水中有机农药分析方法研究进展

随着我国农、林、牧及养殖业的发展,有机农药的使用量显著增加。自然水体中有机农药污染程度日益严重,已对水生生态和人类健康造成严重影响和潜在威胁。为深入了解水中有机农药污染物的检测方法,该文全面系统地对水中有机农药分析方法(预处理方法和检测方法)的原理及优缺点进行了综述,并对其发展方向及趋势进行了展望。通过总结和对比分析,气相色谱和液相色谱法被认为是目前检测水中有机农药残留最有效的方法。该文可为水中有机农药污染物的检测方法选择提供重要参考。     

土壤和沉积物中多环芳烃分析技术研究进展

综述了近年来土壤和沉积物中多环芳烃分析技术的研究进展。重点阐述了索氏提取、超声波提取法、加速溶剂萃取法、微波辅助萃取法、超临界流体萃取法、固相微萃取法、柱层析法、固相萃取法、凝胶渗透色谱法等前处理技术和气相色谱-质谱法、高效液相色谱法和超高效液相色谱法等分析方法,并展望了未来发展的趋势(引用文献71篇)。     

液相色谱测定固体废物中丙烯酸含量

国标分析方法GB 5085.3附录I《固体废物有机磷化合物的测定气相色谱法》,用于分析固体废物中有机磷化合物,并不适用于丙烯酸.固体废物中丙烯酸含量检测因基质复杂等原因不适合气相色谱法、气质联用法及离子色谱法.开发了液相色谱检测方法,样品用试验用水超声提取,静置或离心,上清液经微孔滤膜过滤,经液相色谱检测,以保留时间定...     

固相微萃取在水样污染物检测中的应用

固相微萃取是一种具有高灵敏度、回收率和重复性等优点的前处理技术,广泛应用于水中痕量污染物的处理,本文从固相微萃取装置、基本原理及其在水样污染物检测的中应用展开介绍,并以固相微萃取作为主题检索词,利用ISI Web of Knowledge中Web of Science引文数据库,对1998年到2012年间的相关文献进行计量分析。结果表明,固相微萃取主要应用于水样前处理,杀虫剂是主要的富集对象,气相、液相色谱以及质谱是常使用的检测器。     

Recent methods for the determination of volatile and non-volatile organic compounds in natural and purified drinking water

Four analytical protocols for the extraction and preconcentration of organic residues in natural or purified drinking water were investigated and compared: closed loop stripping analysis; simultaneous extraction-distillation; purge and trap analysis; continuous liquid-liquid extraction. Organic extracts were submitted to a variety of separation and identification techniques. Volatiles were determined by conventional capillary column gas chromatography with tandem mass spectrometry, using triple-stage quadrupole instruments. Non-volatile and thermally labile molecules were investigated by several different techniques (high-temperature gas chromatography, capillary column supercritical fluid chromatography, pyrolysis gas chromatography-mass spectrometry, thermospray liquid chromatography with tandem mass spectrometry and conventional fast-atom bombardment with tandem mass spectrometry). Several samples recently examined in the laboratory provide examples of this multitechnique approach for a more complete knowledge of the organic carbon distribution in water-dissolved organic matter, taking into account organic substances with widely different volatilities, polarities and thermal stabilities.     

Determination of nalbuphine using high-performance liquid chromatography coupled to photodiode-array detection and gas chromatography coupled to mass spectrometry.

A procedure involving capillary column gas chromatography coupled to mass spectrometry and a method involving liquid chromatography coupled to a diode-array detector have been developed for the analysis of nalbuphine. The extraction step is the same for both techniques and involves extraction under alkaline conditions in chloroform-2-propanol-n-heptane (50:17:33, v/v/v) with levallorphan as the internal standard. After purification by acidic extraction and back alkaline extraction, drugs are derivatized with N,O-bis-(trimethylsilyl)trifluoroacetamide with 1% trimethylchlorosilane for gas chromatography-mass spectrometry and directly injected for high-performance liquid chromatography-diode-array detection. The limits of detection are 2.0 and 25.0 ng/mg, respectively.     

水体中硝基芳烃类有机污染物分析方法研究进展

硝基芳烃类有机物是一类重要的化工原料,也是性质相对稳定、难以降解的高毒污染物。其检测技术主要有分光光度法、电化学法、液相色谱法、气相色谱-电子捕获检测器法(GC/ECD)、气相色谱-质谱法(GC-MS)等。其中GC/ECD法和GC-MS法因测定准确、灵敏、适用范围广而得到广泛应用。该文从不同类型水体中硝基芳烃类有机物样品的采集、前处理以及检测分析技术的选择角度,对硝基芳烃类有机物检测技术的发展进行了简要评述,同时对其分析方法进行了展望。     

Chromatography as a reference technique for the determination of clinically important steroids

Chromatographic methods (paper chromatography, thin layer chromatography, high performance liquid chromatography, gas chromatography and gas chromatography-mass spectrometry) for the determination of clinically important steroids in biological specimens are reviewed. The emphasis is on the use of gas chromatography, gas chromatography-mass spectrometry and high performance liquid chromatography as reference rather than routine techniques. Chromatographic methods are compared with colorimetric, fluorimetric and radioimmunoassay procedures in terms of simplicity of operation, cost and ability to analyse large numbers of specimens. The importance of correct specimen collection and storage are discussed. Sample preparation techniques for the various analytical methods are described. These include extraction of free and conjugated steroids from serum, plasma, urine and saliva by solvent partition, with polymer-based resins such as Amberlite XAD-2, DEAE-Sephadex and Sephadex resins bonded with various other function groups and, more recently, with chemically bonded reversed-phase silicas.     

猪肉中63种有机磷农药的气相色谱筛选与气质联用确证方法

建立了固相萃取-气相色谱筛选和气相色谱-质谱联用确证猪肉中63种有机磷农药的分析方法。样品用正己烷配合乙腈-水溶液均质提取,加入氯化钠继续均质,离心分层后取部分乙腈层经C18柱和PSA柱净化后供GC和GC-MS分析。气相色谱筛选采用火焰光度检测器（FPD）,气相色谱-质谱联用确证采用选择离子扫描方式（SIM）,外标法定量。该方法简便、快速,优化条件下测定方法的定量下限（S/N=10）为0.001～0.043 mg/kg,在加标水平为0.16 mg/kg时,回收率为70%～121%,相对标准偏差为4.1%～13.9%。     

Drug detection in hair by chromatographic procedures.

This article reviews the analysis of 31 drugs and drug metabolites in human hair by thin-layer chromatography, high-performance liquid chromatography, gas chromatography, gas chromatography-mass spectrometry and mass spectrometry. The most important detection method after chromatographic separation of the components is the mass spectrometry because of its sensitivity and specificity. Washing steps to exclude external contamination, extraction, derivatization, stationary phases, detection modes and detection limits of the mass spectrometric and gas chromatographic-mass spectrometric procedures are presented in five tables. Additionally, a method for a gas chromatographic-mass spectrometric screening procedure is presented.     

Methods for the determination of sulphonamides in meat.

Sulphonamides, due to their important antibacterial effects, are widely used in veterinary practice and animal husbandry. Residues arising from administration without observing withdrawal time sufficiently are normally the parent compounds and the N4-acetyl derivatives, the latter being hydrolyzed to the parent compounds only during extraction under acidic conditions. It is therefore quite conceivable that many authors concentrate on determining these metabolites. In the past decade, we have witnessed a considerable increase in new analytical techniques dealing with the determination of sulphonamides. Among these procedures, especially the so-called multimethods using high-performance liquid chromatography--though sometimes including toilsome clean-up steps--can be mentioned. However, current approaches also utilize gas chromatography, gas chromatography-mass spectrometry, liquid chromatography-mass spectrometry, supercritical fluid chromatography-mass spectrometry, thin-layer chromatography and immunological methods. For most of these techniques, a strong trend towards lowering the level of detectability (down to the sub-ppb range) and improving accuracy and reproducibility can be established.     

Characterization of Oil by Micro-Solid-Phase Extraction and Gas Chromatography–Mass Spectrometry

Micro-solid-phase extraction is reported for the preparation of Bohai crude oil for the determination of hydrocarbons by gas chromatography-mass spectrometry. The operational parameters were optimized. Micro-solid-phase extraction provided higher quantities of low-molecular weight components than conventional liquid chromatography. The concentrations of high-molecular weight n-alkanes, polycyclic aromatic hydrocarbons, and their alkylated homologs obtained were comparable by micro-solid-phase extraction and liquid chromatography. The diagnostic ratios also indicated that there were no significant differences between these methods. Therefore, micro-solid-phase extraction with gas chromatography–mass spectrometry is recommended for the characterization of spilled oil.     

食品及食品接触材料中烃类矿物油分析技术进展

食品和食品接触材料中矿物油的潜在危害性引起了国内外的普遍关注和深入研究。矿物油是石油提炼过程中的副产物,成分复杂,为分析检测带来了很大的挑战,也促使相关检测技术不断向前发展。目前,针对不同样品基质,已有多种提取、净化方法;国内外也先后建立起了固相萃取/气相色谱法、气相色谱-质谱法、液相色谱-气相色谱联用法、二维气相色谱法、核磁共振等测定方法。该文将对食品和食品接触材料中矿物油检测技术的应用及进展进行综述,并对新技术的发展进行展望,为后续的应用提供借鉴和参考。