分子印迹固相萃取-气相色谱-质谱法测定猪尿中4种β-受体激动剂

建立了分子印迹固相萃取结合气相色谱-质谱测定猪尿中β-受体激动剂氯丙那林、马步特罗、克伦特罗、莱克多巴胺的方法.应用分子印迹柱富集并净化猪尿液中4种β-受体激动剂,比较了分子印迹固相萃取与常规固相萃取的净化效果.通过BSTFA-1％ TMS硅烷化衍生,氘代克伦特罗和氘代莱克多巴胺为校正内标,气相色谱-质谱测定.在优化条...     

亚临界水萃取-固相萃取联用技术对沉积物中有机氯农药的萃取研究

研究了用亚临界水萃取-固相萃取(SBwE-SPE)联用技术萃取湖泊沉积物中的有机氯农药。以活性炭纤维作为固相萃取剂,对亚临界水萃取物进行净化处理。在125℃下亚临界水萃取40min,对六氯环己烷(HCH)的四种异构体：(α-HCH,β-HCH,γ-δHCH,-HCH)和六氯代苯(HCB)的萃取回收率在70％～95％之间。该方法具有简单、快捷、只使用少量有机溶剂等优点。     

石墨烯复合材料固相微萃取涂层的制备及其对水样中六六六残留的测定

该文制备了石墨烯复合材料并将其包覆于铜丝上作为萃取纤维,利用固相微萃取／气相色谱-电子捕获检测器(GC-ECD)技术,建立了环境水样中有机氯农药六六六残留的直接测定方法.优化了萃取时间、萃取温度、pH值及离子强度等固相微萃取条件在优化的实验条件下,所制备的纤维对α-六六六、β-六六六、γ-六六六与δ-六六六的加标回收率...     

氟固相萃取辅助的生物分子质谱分析新方法

氟固相萃取(Fluorous solid-phase extraction,FSPE)是一种基于全氟化合物之间氟-氟相互作用的固相萃取技术,通过在目标分子上进行氟标签衍生,利用高氟化固相吸附剂实现特异性的分离纯化.这一技术在有机合成、催化,以及化学和生物分离分析等诸多领域应用广泛.近年来,由于氟固相萃取和生物质谱技术之间良好的兼容性,两者联用结合的分析方法受到了研究者的广泛关注.本文在简要介绍氟固相萃取技术原理的基础之上,重点综述了其在生物质谱分析领域中的应用,并对其发展前景进行了展望.     

分子印迹固相萃取技术检测江水、尿液及牛奶中雌激素残留

以β-雌二醇和炔雌醇的分子印迹聚合物为填料制备固相萃取小柱,选择60%(V/V)甲醇-水溶液作为雌激素的淋洗液,甲醇-乙酸(9:1,V/V)为洗脱液,洗脱两次可彻底洗脱固相萃取小柱中目标分子.以建立的萃取条件对上海黄浦江水、尿液、牛奶中雌激素进行富集,结合高效液相色谱法,建立了基于分子印迹固相萃取技术检测上述实际样品中...     

HPLC法分析烟叶中的β-D-吡喃葡萄糖苯乙醇苷

结合制备型HPLC分离纯化技术和分析型HPLC分析测定技术,建立一种直接分析测定烟叶中β-D-吡喃葡萄糖苯乙醇苷的新方法.在超声波辅助条件下,用甲醇-水溶液萃取烟叶中的β-D-吡喃葡萄糖苯乙醇苷,并优化了萃取条件;萃取液中的β-D-吡喃葡萄糖苯乙醇苷用制备型HPLC进行分离纯化,并用分析型HPLC对其含量进行测定.结果...     

同时亚临界水萃取与固相萃取从河流沉积物中分离有机氯化合物

静态亚临界水萃取中加入固相萃取剂对河流沉积物中4种有机氯化合物(2-氯酚、2,4,6-三氯酚、五氯酚、六氯苯)进行了同时萃取。与离线亚临界水萃取-固相萃取方法相比,分析物的萃取回收率均有提高,且受亚临界水萃取罐冷却程度的影响较小。以活性炭纤维(ACF)为固相萃取剂,在160℃时,0.050 g的ACF和4.0 mL水对0.500 g的加标沉积物样品中的2-氯酚(2-CP),2,4,6-三氯酚(246-TCP),五氯酚(PCP)和六氯苯(HCB)的萃取效率比离线亚临界水萃取-固相萃取的回收率均有所提高,萃取回收率受萃取罐冷却温度影响较小。方法特别适合于高含量的沉积物样品萃取。该方法与气相色谱检测联用,分析了长江镇江段沉积物中4种有机氯化合物的含量,结果与美国环保署(USEPA)标准方法所得的结果吻合。     

近年国内固相萃取-色谱分析的进展

对近两年国内各个领域的学者在使用固相萃取做样品前处理的色谱分析方面的研究和应用作了综述, 这一综述包括10个部分: 1. 国内近两年有关固相萃取的综述报告;2. 固相萃取-色谱分析在水质分析中的应用;3. 固相萃取-色谱分析在奶制品和肉类食品分析中的应用;4. 固相萃取-色谱用于蔬菜和水果中有害物质分析的应用;5. 固相萃取-色谱用于粮食和其他食品中有害物质分析的应用;6. 固相萃取-色谱在血药浓度、体液及组织中有害物质分析中的应用;7. 固相萃取-色谱在药物分析中的应用;8. 固相萃取-色谱在其他使用色谱分析中的应用;9. 基质固相分散在色谱分析中的应用;10. 分子印迹SPE在样品前处理中的应用.     

固相微萃取涂层制备方法研究进展

涂层是固相微萃取技术的核心,近年来出现的各种新型涂层材料和制备技术,进一步拓宽了固相微萃取技术的应用范围.该文介绍了各种新型固相微萃取介质的发展,并综述了各种新型固相微萃取涂层的制备方法,包括直接制备、溶胶-凝胶技术、化学键合与聚合、分子印迹技术、树脂固载技术、电化学沉积等.     

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。     

β-Cyclodextrin-polyurethane polymer as solid phase extraction material for the analysis of carcinogenic aromatic amines

β-Cyclodextrin-polyurethane (β-CDPU) polymer was synthesized by the reaction of β-cyclodextrin with hexamethylene diisocyanate in dry dimethylformamide and used as a sorbent for the solid phase extraction (SPE) of carcinogenic aromatic amines from water. The polymers were characterized by Fourier transform infrared spectroscopy, thermogravimetric analysis, differential scanning calorimetry and particle size analysis. The separation and quantification was performed by Liquid chromatography with RP-C₁₈ column and diode array detection using standard arylamines for quantification. When compared with commercially available sorbents, β-CDPU gave better recovery for the aromatic amines. From the variation of pH of the extractant from 4.0 to 8.5 recovery was highest at pH 8.5. The breakthrough volume has been ascertained to be 100 ml for 200 mg of the resin. The new SPE material offers better recovery and estimation of banned arylamines.     

固相萃取新技术研究

固相萃取技术是一种用于样品分离、纯化、浓缩的重要的样品前处理手段。近年来,高分子材料合成技术、分子印迹技术等新技术与传统固相萃取技术相结合,衍生出众多技术改进和创新。主要对各种固相萃取新技术进行评述。     

碳纳米管在分离科学中的应用研究进展

碳纳米管(CNTs)作为一种新型纳米材料已在材料、催化、吸附分离等诸多领域得到了广泛的应用。本文对近年来CNTs在分离科学中的应用研究进展进行了简要评述,主要讨论了CNTs在固相萃取、固相微萃取、膜萃取、色谱固定相和毛细管电泳假固定相等方面的应用。     

利用分子印迹技术预处理生物样品中头孢药物的研究

优化了头孢硫脒分子印迹聚合物的合成条件,探讨了分子印迹技术和固相萃取联用对血浆中头孢硫脒的分离富集,发现用4-乙烯基吡啶作功能单体合成的分子印迹聚合物作为固相萃取填充料,能定量吸附血浆中的头孢硫脒,并初步研究了其吸附机理。     

3DG Functionalized Magnetic Solid Phase Extraction Materials for the Efficient Enrichment of Hexamethylenetetramine in Vermicelli

Solid phase extraction (SPE) is regarded as the most effective purification method for complex matrix samples owing to its simplicity of operator, time-saving, high accuracy, and environmental friendliness. SPE technology is still affected by the high cost of commercial SPE columns and poor adsorption selectivity. Hence, the development of low-cost and highly selective adsorbents is quite challenging and demanding in SPE. In this study, a novel 3DG functionalized magnetic solid phase extraction materials was prepared based on “thiol-ene” click chemistry. The structure, morphology, thermal stability, and magnetic properties of the magnetic composites were studied by Fourier transform infrared spectroscopy (FT-IR), scanning electron microscopy (SEM), energy dispersive spectroscopy (EDS), thermogravimetric analysis (TGA), and vibrating sample magnetometer (VSM). Then the adsorption performance of composite was determined by static adsorption experiments, which showed fast binding kinetics (100 min) and good adsorption performance (Q_e = 65.34 mg/g). Moreover, these magnetic nanoparticles were used as adsorbents for magnetic solid phase extraction (MSPE) and coupled with high-performance liquid chromatography (HPLC) for separation and detection of illegally added hexamethylenetetramine in vermicelli. As for practical application, the recoveries for the spiked samples in the concentration range of 8–40 μg/g were between 83.24–92.69%, and the RSD was between 0.20–2.07%.     

金属有机骨架复合材料在样品预处理中的研究进展

金属有机骨架（MOFs）材料是近几年涌现出的一类新型多功能多孔材料,以金属离子或金属簇为配位中心,与含氧或氮的有机配体通过配位作用形成多孔骨架结构。相比于其他传统无机多孔材料,MOFs具有比表面积高、孔隙率大、热稳定性好和结构与功能多样化的特点,因而被广泛用于气体存储、催化、吸附和分离等领域。MOFs复合材料在样品预处理方面的应用引起了研究者们的极大兴趣和广泛关注。由于MOFs材料和不同功能材料如高分子聚合物、碳基材料以及磁性材料组装复合,使MOFs复合材料的性能优于原来的MOFs材料。综述了近年MOFs复合材料在样品预处理的研究应用,尤其是在固相微萃取、固相萃取以及磁性固相萃取等方面的应用。     

无筛板型固相萃取柱的制备及其在食品中苯甲酸的测定研究

结合固相萃取(SPE)盘与含支撑物的SPE柱技术,制备了一种新型的无筛板型固相萃取柱.以C18填料为例,以话梅样品为介质对其中的苯甲酸进行分析,并用传统固相萃取小柱平行比较;将SPE与HPLC-UV结合,考察了填料对简单介质中苯甲酸的最大吸附量及洗脱曲线,研究了新型SPE柱在实际应用中的分离纯化效果.结果表明,新型SPE柱对样品的吸附效果更好,规格为200 mg/3 mL的SPE柱对苯甲酸的吸附量达到0.951 mg,超过了传统柱的吸附量0.908 mg;其洗脱曲线与传统柱几乎重合;苯甲酸在1～100 mg/L浓度范围内线性关系良好, r=0.9999,用此SPE柱纯化后的样品加标回收率和相对误差分别在88.4%～102.3%和1.4%～2.9%之间.     

Hyphenated gas chromatography-mass spectrometry analysis of 3-mercaptohexan-1-ol and 3-mercaptohexyl acetate in wine: Comparison with results of other sampling procedures via a robust regression

This work describes a new purge and trap gas chromatography electron impact mass spectrometry (PT-GC-EIMS) method for quantifying 3-mercaptohexan-1-ol (3-MH) and 3-mercaptohexyl acetate (3-MHA), two molecules able to characterize some wines with their tropical scents. Firstly the experimental conditions of the purge and trap extraction (sample temperature, extraction time, trap temperature, flow rate) following a multivariate approach were optimized. Then the method through the construction of the calibration curves and the establishment of the detection limits was validated. The purge and trap procedure appears faster and more sensitive than both the headspace solid phase microextraction (HS-SPME) and the solid phase extraction (SPE) procedures, reaching detection limits for the two thiols closer to their sensory thresholds. Evidence of similar performances of the three sampling methods considered was gained comparing the results relevant to same wine samples. The Theil's regression method was used for purpose of comparison.     

β-Cyclodextrin-cross-linked polymer as solid phase extraction material coupled with inductively coupled plasma mass spectrometry for the analysis of trace Co(II)

A sensitive method for the separation/analysis of Co(II) was described. The β-cyclodextrin cross-linked polymer (β-CDCP) was synthesized and used as solid phase extraction material (SPE) to separate/pre-concentrate trace cobalt coupled with inductively coupled plasma mass spectrometry (ICP-MS) for the analysis of Co(II). The method was based on α-pyridylazo-β-naphthol (PAN) as the complexing agent for Co(II)-PAN at neutral condition and the adsorption behavior of Co(II)-PAN on β-CDCP was studied. Further, p-octylpolyethylene-glycolphenyl ether (Triton X-100) as environment-friendly eluant was used. The linear range, detection limit (DL) and the relative standard deviation (R.S.D.) was 5.0-160.0 ng/mL, 5.84 ng/L and 2.27% (n = 3, c = 30.0 ng/mL) respectively. The enhancement factor was 10. Moreover, the β-CDCP could be used repeatedly and offered better recovery and estimation of standard samples.     

固相微萃取与色谱联用方法分析水中12种有机氯化合物

运用顶空固相微萃取与色谱闻用方法（ＨＳ－ＳＰＭＥ－ＧＣ）对水中的残留有机氯化合物进行了分析。对影响ＨＳ－ＳＰＭＥ－ＧＣ分析灵敏度的各种实验因素如涂层种类,萃取温度、平衡时间,离子浓度等进行了讨论并将该方法与固相萃取法（ＳＰＥ）,液液萃取法（ＬＬＥ）作了对比,同时考察了常见环境共存污染物直链烷基苯磺酸钠（ＬＡＳ）对几种方法的影响。