国内气相色谱-质谱联用分析技术在氨基甲酸乙酯检测中的应用

气相色谱-质谱法是测定发酵食品和酒精饮料中氨基甲酸乙酯非常重要的方法,相关的报道也非常多。为了适应不同基质样品的分析,需采用不同的样品前处理方法。文章介绍了液/液萃取(LLE)、固相萃取(SPE)、固相微萃取(SPME)等9种样品前处理方法结合气相色谱/气质联用技术在检测氨基甲酸乙酯中的应用。     

固相微萃取(SPME)的演变和现状

固相微萃取(SPME)是一种广泛使用的样品前处理技术,它是集萃取、浓缩、解吸、进样于一体的样品前处理新技术,它以固相萃取(SPE)为基础,保留了SPE的全部优点,排除了需要柱填充物和使用有机溶剂进行解吸的缺点.SPME是以涂渍在石英玻璃纤维上的固定相(高分子涂层或吸附剂)作为吸收(吸附)介质,对目标分析物进行萃取和浓缩,并在气相色谱仪进样口中进行分析,这一技术适合于很多技术领域的样品处理和分析.对SPME的演变和进展做了简要讨论.     

碳纳米固相微萃取纤维的制备及在水样分析中的应用

固相微萃取(SPME)是基于固相萃取(SPE)技术发展起来的一种集萃取、浓缩、解吸、进样等功能于一体的样品前处理方法。碳纳米管CNTs是一维碳基纳米材料,具有独特的管状结构、良好的化学稳定性、热稳定性和高比表面积。本文将碳纳米材料作为固相微萃取的纤维涂层材料,进而介绍了两种纤维涂层的制备方法—物理涂覆法和化学涂覆法,并对其在水样分析中的应用做一综述。     

固相微萃取技术模式的研究进展

样品前处理技术是分析化学的瓶颈,1987年提出固相微萃取(SPME)后样品前处理领域极大进步。近年出现的多种SPME涂层材料和制备技术,进一步拓宽了SPME在活体和现场分析中的应用。综述了固相微萃取技术相关模式,包括纤维固相微萃取、管内萃取和搅拌棒萃取等模式,并阐述了固相微萃取的发展趋势。     

固相萃取-液相色谱联用检测镍电解液中的有机磷萃取剂

建立了固相萃取(SPE)-高效液相色谱(HPLC)联用测定镍电解液中P204、P507和C272的分析方法。优化了萃取溶剂、SPE柱填料类型、SPE淋洗溶剂等前处理条件以及HPLC检测条件。采用C18填料的SPE柱进行固相萃取,检测方法的线性范围为0.1~100 mg/L;检出限为0.02 mg/L。加标样品回收率为68.6%~83.5%,RSD为5.5%~9.2%。该方法灵敏度高,重复性良好,操作简便快速,适用于镍电解液中3种有机磷萃取剂的检测。     

固相微萃取技术模式的研究进展

样品前处理技术是分析化学的瓶颈,1987年提出固相微萃取(SPME)后样品前处理领域极大进步。近年出现的多种SPME涂层材料和制备技术,进一步拓宽了SPME在活体和现场分析中的应用。综述了固相微萃取技术相关模式,包括纤维固相微萃取、管内萃取和搅拌棒萃取等模式,并阐述了固相微萃取的发展趋势。     

固相微萃取在食品安全检验中的应用

固相微萃取(SPME)技术是在固相萃取(SPE)的基础上发展出起来的一种新型样品前处理技术,它集采样、萃取、浓缩、进样于一体,可与GC、HPLC联用,检测简便、快速、无有机溶剂、选择性好、灵敏度高.本文介绍其装置、原理、SPME-GC联用技术、SPME-HPLC联用技术,及其在食品安全检验中的应用.     

MAE-SPME联合提取GC-MS检测草莓果实中的香气成分

分别采用溶剂萃取法(SE)、固相微萃取法(SPME)和微波辅助-固相微萃取(MAE-SPME)联用技术等前处理方法提取草莓果实中香气物质,通过气相色谱-质谱(GC-MS)联用仪对挥发性成分进行了分离鉴定。结果表明,不同的前处理方法所得结果相差甚远,MAE-SPME联用技术前处理方法提取后,可鉴定到85种化合物,其中酯类53种,其他依次是醛类、酮类、醇类、酸类、醚类、烯烃、芳香烃和杂环化合物等;而用SE法、SPME法提取,分别仅鉴定到26种和16种香气物质。说明微波辅助-固相微萃取两种技术联用,是一种能较好地提取果蔬中香气物质的样品前处理技术。     

固相萃取净化-气相色谱-质谱法测定染料中7种指示性多氯联苯

本文建立了以固相萃取(SPE)前处理净化、结合气相色谱-质谱(GC-MS)测定染料中7种指示性多氯联苯的分析方法。该法将染料样品经溶剂萃取后,通过固相萃取(SPE)净化、浓缩,气相色谱-质谱采用选择离子监测模式(SIM)测定,以保留时间和特征离子定性,外标法定量。     

金属有机框架化合物(MOFs)在水、食品以及化妆品检测中的应用进展

样品前处理是整个分析检测过程的重要环节，开发高效、绿色化的前处理技术是目前的研究趋势。近年来，金属有机框架化合物(MOFs)凭借其优异的物理化学性质(高比表面积、均匀的孔腔、良好的热稳定性以及高孔隙率)作为固相萃取(SPE)吸附材料，在绿色化学检测(GAC)领域得到了广泛的应用。综述了近年来MOFs作为固相萃取吸附剂，检测水、食品以及化妆品中有害物质样品前处理研究进展，以期为这些领域相关的科研人员和检测人员提供新的思路。     

Application of Headspace Solid-Phase Microextraction and Gas Chromatography for the Analysis of Furfural in Crude Palm Oil

Processing of vegetative material containing pentoses has been shown to result in the formation of furfural. Furfural exhibits a spectrophotometric absorption peak at 518 nm when complexed with aniline acetate. Headspace solid-phase microextraction (HS-SPME) method has been successfully used to confirm the presence of furfural in crude palm oil (CPO). Solid phase microextraction (SPME) fiber composed of divinylbenzene/Carboxen/polydimethylsiloxane (DVB/PDMS/CAR) was used to absorb the volatiles in the headspace of the oil. The isolated compounds from the fiber was desorbed and separated on a capillary polar column of a gas chromatograph. Response surface methodology (RSM) was used to optimize the SPME fiber condition for maximum absorption of furfural from CPO. The optimized temperature and time for furfural extraction onto the SPME fiber are 70 °C for 40 min. Oils obtained from the mill were found to contain between 2 and 13% furfural.     

Solid‐phase microextraction (SPME) in polymer characterization—Long‐term properties and quality control of polymeric materials

Solid‐phase microextraction (SPME) in combination with GG‐MS was applied to quality control polyamide 6.6 collected for recycling and to study the long‐term properties and degradation of nitrile rubber, polyethylene, and polyamide 6.6. The migration of plasticizer and other additives reduces the service‐life and changes the properties of the material. It is also a possible health hazard, for example, legislation against the use of brominated flame retardants in plastic materials, is under discussion, and fast and reliable methods are required to detect such compounds in plastic materials collected for recycling. SPME rapidly and effectively extracted several brominated compounds from in‐plant collected polyamide 6.6. Migration of tris(2‐butoxyethyl)phosphate plasticizer and its degradation products from nitrile rubber during long‐term thermal ageing at 60 and 80°C was shown by SPME‐GC‐MS, while the plasticizer was not volatile enough to be detected by traditional HS‐GC‐MS. In accordance the number of degradation products extracted from thermo‐oxidized PE by HS‐SPME was three times larger than the number detected after HS‐GC‐MS analysis. SPME‐GC‐MS could also detect early signs of degradation in thermo‐oxidized virgin and in‐plant recycled polyamide 6.6 before any signs of degradation were observed by, for example, tensile testing or FTIR. © 2003 Wiley Periodicals, Inc. J Appl Polym Sci 89: 867–873, 2003     

固相微萃取技术及其应用

固相微萃取（solid phase microextraction,SPME)技术是近年来发展起来的一种样品分析预处理的新方法，与传统的溶剂萃取技术相比，该技术具有快速，高效 ，简便，园需溶剂，易于自动化操作等优点，目前已经被应用于环境分析和药品检测等许多领域，本文简介了固相微萃取技术的原理以及该技术在生产，生活领域上的应用。     

Rapid Separating and Enrichment of 4,4′-Dimethylsterols of Vegetable Oils by Solid-Phase Extraction

Phytosterols are separated into three classes: 4-desmethylsterols, 4-monomethylsterols and 4,4′-dimethylsterols. 4,4′-Dimethylsterols are used to detect vegetable oil adulteration and some compounds from this class can have anti-inflammatory and anticancer properties. There are methods such as thin layer chromatography (TLC) and solid phase extraction (SPE) used to separate phytosterol classes from each other. However, in some cases, separation of all three classes is not required. In addition, TLC has some drawbacks such as low recovery and it is time consuming. An SPE method has previously been used, but it was necessary to use high volume of solvents with this method to avoid coelution of phytosterol classes. In this study, an SPE (silica, 1 g) method was developed to separate and enrich only 4,4′-dimethylsterols from unsaponifiables of vegetable oil samples using 25 mL n-hexane and diethyl ether (95:5, v:v). This method was applied to hazelnut and olive oils and results were compared with those of TLC and the previously developed SPE method. Recovery of 4,4′-dimethylsterols was two times higher with the new SPE method compared with the TLC method. The newly developed SPE method generally gave a similar recovery compared with the previously developed SPE method. Moreover, the SPE method developed in this study has the advantage of using a 3.5 times lower volume of solvent than previously developed SPE methods. Because the newly developed SPE method has a single step requiring a low volume of solvents, it is rapid and simple, and can easily be used to detect olive oil adulteration with hazelnut oil and to analyze and quantify effective nutritional compounds in the 4,4′-dimethylsterols class.     

固相萃取技术的应用与研究新进展

固相萃取技术(SPE)是近年来发展较快并得到广泛应用的一种新前处理方法,介绍了固相萃取技术的基本原理及方法。对固相萃取技术在食品、药品、和环境检测等领域的应用进行了综述,阐述了目前对固相萃取技术的研究开发和发展展望。     

Comparison of Sample Preparation and Analysis Using Solid-Phase Extraction and Solid-Phase Microextraction to Determine Monohydroxy PAH in Urine by GC/HRMS

Sample preparation techniques using solid-phase extraction (SPE) and solid-phase microextraction (SPME) are compared for the analysis of monohydroxy polycyclic aromatic hydrocarbons (OHPAH) in human urine. Urine samples spiked with five carbon-13 labeled internal standards are first enzymatically hydrolyzed. Sixteen OHPAH from eight parent compounds (naphthalene, fluorene, phenanthrene, fluoranthene, pyrene, chrysene, benzo[ c ]phenanthrene, and benz[ a ]anthracene) are then extracted along with the internal standards by these two different techniques. The analytes are derivatized by a silylating reagent before final analysis. Final separation and detection are performed by temperature-programmed capillary gas chromatography (GC) and high-resolution mass spectrometry (HRMS). The two extraction techniques are compared for sample preparation time, cost, throughput, reinjection possibility, frequency of outliers, matrix interference, signal linearity, and method detection limit. SPE demonstrates major advantages over SPME for most of these aspects.     

黑龙江产芜荽籽香气成分研究

研究了黑龙江产芫荽籽的香气成分.采用两种固相微萃取柱萃取芫荽籽香气成分,并用GC-MS分析,还与水蒸气蒸馏法获取的芫荽籽精油的成分进行了比较.用DVB/CAR on PDMS萃取柱时,检出24个成分,解析出占总成分的85.391%的17种物质,主要成分芳樟醇相对含量44.666%;用CAR on PDMS萃取柱时,检测出19种成分,解析出占总成分98.443%的18种成分,主要成分芳樟醇相对含量为32.578%;水蒸气蒸馏法获取的芫荽籽精油得油率为0.50%,检测出31个成分,解析出占精油总成分的99.727%的29种成分,芳樟醇相对含量为73.614%.     

固相萃取技术及其应用新进展

固相萃取(SPE)是近年来新开发出并得到广泛应用的一种新技术。本文拟通过固相萃取技术的原理、特点、分离模式和操作方法等以及在各个领域的应用和发展前景的介绍与阐述,以对这项新技术在我国的广泛应用起到推动作用。     

固相萃取技术在化妆品样品前处理中的应用研究

固相萃取是化妆品样品前处理的重要手段之一。以化妆品中生物碱的检测为例,研究了在化妆品的样品前处理中,固相萃取柱的选择以及影响净化效率的因素。研究表明,应根据目标化合物的性质选择合适的固相萃取柱,同时也要考察不同的上样溶液对保留能力的影响,根据不同的提取方式优化适宜的固相萃取条件。另外,固相萃取柱填料的粒度对净化效率和试验周期也有重要影响。     

Identification of rubber polymers in rubber blends

Abstract

Solid phase extraction (SPE) was used to separate pyrolysates of rubber blends. Then each rubber polymer in rubber blends was identified, based on interpreting infrared spectrum of separated pyrolysates. By using this method, nature–ethylene–propylene, ethylene–propylene–silicone, butyl–styrene–butadiene and ethylene–propylene–butadiene–acrylonitrile rubber blends were analysed. The analytical results show that each characteristic pyrolysate of polymer in rubber blend pyrolysate can be separated by SPE. The method for identification of rubber polymers in rubber blends by infrared coupled with SPE is flexible, rapid and low cost, compared with the method by pyrolysis gas chromatography coupled with infrared spectroscopy or mass spectroscopy.