3种固相萃取新技术在食品检测前处理中的应用

固相萃取技术是样品前处理中常用的方法,具有试剂用量少、环境污染少、无乳化、操作简单等优点。本研究介绍了固相微萃取、基质分散固相萃取和在线固相萃取等3种固相萃取新技术在食品检测领域中的应用,并对各技术的优缺点进行了分析,同时阐述了各技术在食品检测领域的发展局限性及发展趋势,以期为这3种技术的应用提供参考依据。     

固相微萃取在食品农药残留检测中应用

该文综述食品农药残留分析样品前处理技术—固相微萃取技术,对固相微萃取方法在食品农药残留检测中应用进行总结,并对固相微萃取在食品农药残留分析中发展进行讨论。     

固相微萃取技术在食品安全检测中的应用研究

作为一种新型的分析技术,固相微萃取技术经常会应用到样品的前处理环节。与之前使用的前处理技术相比,固相微萃取技术具备高效、快捷、简单的优势,所以在食品检测过程中应用非常广泛。随着科学技术水平的不断发展,使用固相微萃取技术对食品进行检测也已经取得了极大的进展。基于此,在本文中就结合固相微萃取技术的应用原理及操作步骤,探讨了其在食品安全检测中的具体应用,最后总结了固相微萃取技术的发展趋势。     

固相微萃取技术在食品安全检验中的应用研究

固相微萃取技术（SPME技术）是一种新型的样品前处理技术，也是一种新的分析技术。该技术与传统的样品前处理技术相比，具有简单、快速、高效等特点，目前已广泛应用于食品安全领域。近年来，随着我国科学技术的不断发展，食品安全检验领域中固相微萃取技术也有了较大的发展。本文首先介绍了固相微萃取技术的原理，然后对该技术在食品安全检验中的应用进行了研究，希望可以为今后该领域的研究提供一些参考。     

固相微萃取技术在食品安全检测中的应用研究

固相微萃取（SPME）是一种简便、快速、高效、环保的样品前处理方法，被广泛应用于食品安全检验领域。本文分析了固相微萃取技术的原理、常用的固相微萃取材料和方法，重点探讨了其在食品安全检测中的应用，包括农药残留、兽药、重金属和生物毒素等方面。     

分子印迹材料萃取与高效液相色谱联用技术

与传统固相萃取材料相比,分子印迹聚合物(MIPs)具有高选择性、稳定性好、可重复使用等优点,可以在复杂的样品中作为富集分离的一种前处理技术。分子印迹用于固相萃取(SPE)和固相微萃取(SPME)与高效液相色谱(HPLC)联用,可以用于检测复杂样品中的目标物。     

固相微萃取技术及其在N-亚硝胺分析中的应用

固相微萃取技术(SPME)是在固相萃取基础上发展起来的一种无溶剂的样品前处理技术,集采样、萃取、浓缩、进样于一体。该技术有着操作简单迅速、低耗费、安全、易解析、高灵敏度及无有机溶剂的优点。本文介绍了固相微萃取技术的原理、萃取装置、萃取方式、操作过程,并综述了固相微萃取技术在N-亚硝胺分析中的研究进展及应用前景。     

纺织品致癌芳香胺前处理萃取方法研究进展

针对纺织品中致癌芳香胺前处理的传统方法液液萃取、固相萃取存在使用试剂量大、过程繁琐、溶剂易挥发等问题。文章综合研究了近年来纺织品中致癌芳香胺检测前处理的方法,包括常规液液萃取、分散液液微萃取、漩涡辅助液液微萃取、单滴液液微萃取、双水相萃取、溶剂诱导相变微萃取、传统固相萃取、直接固相微萃取、加膜固相微萃取、加速溶剂萃取等方法。通过比较发现,液液微萃取、加膜固相微萃取使用有机量少,均低于1 mL,操作过程简单,适用纺织品致癌芳香胺前处理萃取发展方向,但需要加大研究增加致癌芳香胺加膜固相微萃取萃取头,以及纺织品成分、加工工艺对加膜固相微萃取、液液微萃取在萃取过程中的影响,以最终建立适合纺织品中致癌芳香胺的萃取方法。     

固相微萃取及其在水产品风味分析中的应用

固相微萃取(SPME)是一种无溶剂萃取技术,它克服了传统样品前处理技术的缺陷,集采样、萃取、浓缩、进样于一体,具有简单、快速、高效、能直接与其他分析仪器联用等优点,已被广泛应用于风味成分的研究。水产品因其独特的风味深受人们的喜爱,研究水产品风味对于评价水产品的新鲜度、生产加工及品质控制等方面具有重要意义。文中主要介绍了固相微萃取技术及其发展,综述了该技术在水产品风味分析中的研究现状,并对SPME在水产品中的应用前景进行了展望。     

固相微萃取-气相色谱-质谱法测定食品塑料包装袋中6 种酞酸酯类化合物

建立固相微萃取-气相色谱-质谱同时测定食品塑料包装袋中6 种酞酸酯类化合物的分析方法,并对固相微萃取方式、萃取溶剂、萃取头涂层、萃取温度等参数进行优化。采用85 μm PA固相微萃取纤维头、正己烷为萃取溶剂,90 ℃平衡5 min后萃取吸附30 min,在250 ℃进样口解吸5 min后供气相色谱-质谱分析。结果表明：该方法的线性范围为0.25～50 mg/L,方法检出限为0.049～0.920 mg/L,回收率为82.2%～109.0%,相对标准偏差（n=6）为4.0%～12.0%,该方法能很好地富集基体中的目标化合物,满足食品塑料包装袋中多种酞酸酯类化合物的分析要求。     

Phthalate Sample Preparation Methods and Analysis in Food and Food Packaging: a Review

A review on phthalate esters or phthalic acid esters (PAEs), chemicals of concern since a few decades ago that are widely used as plasticizers in food processing and packaging, is presented taking into account the background of such compounds, the metabolism, human exposure to PAEs, the sources and occurrence in food as well as the toxicological aspects and human health effects. In addition, 45 novel research articles that were published between 2002 and 2017 were identified and their results were tabulated showing the PAEs analysed, food matrix of PAEs, methods of sample preparation/extraction, methods of instrumental analysis and quantitation, percentage recovery and limit of detection (LOD) of the instrument for ease of comparison and referencing. In general, it was found that in the last 15 years, the number of PAEs analysed has increased from the commonly analysed 8 PAEs, namely dimethyl phthalate (DMP), diethyl phthalate (DEP), diisobutyl phthalate (DIBP), di-n-butyl phthalate (DBP), butyl benzyl phthalate (BBP), dicyclohexyl phthalate (DCHP), di-n-octyl phthalate (DNOP) and di-(2-ethylhexyl) phthalate (DEHP) to as many as 23 PAEs. The methods of sample preparation have also progressed from the simple liquid-liquid extraction using organic solvents to solid-phase microextraction techniques to the more recent head-space or direct immersion solid-phase microextraction methods. Whereas for the analysis of PAEs, gas chromatography and liquid chromatography are still the preferred methods with improved LOD of analysis ranging from approximately 10 ppm for fatty foods to 1–60 ppt for water, juices and cooking oil samples.     

Phthalates in Beverages and Plastic Bottles: Sample Preparation and Determination

Several compounds of the phthalate family are widely applied as additives for polymers as polyvinyl chloride (PVC) and polyethylene terephthalate (PET). These compounds are not part of the polymer chains, and therefore, they can be released easily from products and migrate into beverages that come into direct contact causing environmental and human health impacts. Because of this, certain phthalates (PAEs) have been identified as priority pollutants by the European Union (EU), US Environmental Protection Agency (EPA) and other international organizations. Due to that the concentration of these compounds in beverages is found at very low level, a pretreatment step prior to their analysis is necessary; thus, several sample preparation methods have been described, such as liquid–liquid extraction (LLE), solid-phase extraction (SPE), solid-phase microextraction (SPME), and liquid-phase microextraction (LPME). Chromatographic techniques such as gas chromatography (GC) coupled to mass spectrometry (MS) or liquid chromatography (LC) with UV detector, diode array detector (DAD), and MS have been used to analyze PAEs. Additionally, non-chromatographic techniques such as electrochemical sensors and immunoassay-based techniques have been described for PAE analysis in beverages. This review provides an overview of the different analytical techniques for PAE quantification in beverages and their plastic containers, focused in the last 10 years published works, covering the sample preparation and determination, as well as the legislation and the evaluation of main factors that could promote the migration of these plasticizers from polymers into beverages.     

气相色谱-质谱联用法直接测定植物油料中邻苯二甲酸酯类塑化剂

建立有机溶剂萃取、N-正丙基乙二胺（N-(n-propyl) ethylenediamine,PSA）玻璃固相萃取柱净化、内标法定量、气相色谱-质谱法直接测定植物油料中邻苯二甲酸二甲酯（dimethyl phthalate,DMP）、邻苯二甲酸二乙酯（diethyl phthalate,DEP）、邻苯二甲酸二异丁酯（di-iso-butyl phthalate,DIBP）、邻苯二甲酸二丁酯（dibutylphthalate,DBP）、邻苯二甲酸丁基苄基酯（butyl benzyl phthalate,BBP）、邻苯二甲酸二（2-乙基）己酯（di(2-ethtlhexyl) phthalate,DEHP）和邻苯二甲酸正辛酯（di-n-octyl phthalate,DNOP）7 种邻苯二甲酸酯的方法。该方法在0.01～2.0 mg/L范围内具有良好的线性关系,相关系数R2在0.999 8～1.000 0之间,仪器检出限（RSN=3）为0.01～0.02 μg/L,定量限（RSN=10）为0.03～0.06 μg/L。7 种目标物在0.1、0.5、1.0 mg/kg的加标水平下平均回收率为77.2%～98.8%,相对标准偏差为0.62%～9.37%（n=6）。采用本方法对不同种类、不同产地的76 个植物油料样品中7 种邻苯二甲酸酯类塑化剂含量进行测定。结果表明：所有受检植物油料样品中均检出DBP和DEHP,范围分别为（0.015±0.002）～（0.584±0.012） mg/kg和（0.085±0.006）～（2.334±0.016） mg/kg,检出率均为100%（76/76）;DIBP、DEP、DMP、BBP、DNOP检出率分别为98.7%（75/76）、64.5%（49/76）、63.2%（48/76）、32.9%（25/76）、5.3%（4/76）。17 个油料样品中DBP含量超出国家标准限量（≤0.3 mg/kg）,超标率为22.4%;1 个油料样品中DEHP含量超出国家标准限量（≤1.5 mg/kg）,超标率为1.3%。     

Rapid analysis of phthalates in beverage and alcoholic samples by multi-walled carbon nanotubes/silica reinforced hollow fibre-solid phase microextraction

A novel procedure based on multi-walled carbon nanotubes (MWCNTs)/silica reinforced hollow fibre solid-phase microextraction combined with gas chromatography–mass spectrometry has been developed to analyse trace phthalate acid esters in beverage and alcoholic samples. Because of their excellent adsorption capability towards hydrophobic compounds, functionalized MWCNTs, acting as solid-phase sorbent, were co-deposited with silica particles in the pores of polypropylene hollow fibre through a layer-by-layer self-assembly technique. The parameters influencing the extraction efficiency, such as pH values and ionic strength of sample solution, extraction time, temperature and desorption solvent were optimised. Recoveries for phthalates at spiking levels in different matrices were satisfactory (between 68% and 115%). Moreover, the results were further confirmed by comparing them with those obtained using a solvent extraction method according to the national standard of China.     

Vortex-Assisted Liquid–Liquid Microextraction Combined with HPLC for the Simultaneous Determination of Five Phthalate Esters in Liquor Samples

A vortex-assisted liquid–liquid microextraction (VALLME) method using hexanoic acid as extractant followed by high-performance liquid chromatography–diode array detection was developed for the extraction and determination of five phthalate esters (PAEs) including bis-methylglycol ester (DMEP), benzyl butyl phthalate (BBP), dicyclohexyl phthalate (DCHP), di-n-butyl phthalate (DBP), and di-n-octyl phthalate (DNOP) from liquor samples. In this method, hexanoic acid was employed as extraction solvent, because its density is lower than water. And vortex mixing was utilized as a mild emulsification procedure to reduce emulsification time and improve the effect of extraction. Under the studied conditions, five phthalate esters were successfully separated within 20 min and the limits of detection were 2.3 ng mL^?1 for DMEP, 1.1 ng mL^?1 for BBP, 1.9 ng mL^?1 for DCHP, 1.2 ng mL^?1 for DBP, and 1.5 ng mL^?1 for DNOP, respectively. Recoveries of the PAEs spiked into liquor samples were ranged from 89 to 93 %. The precisions of the proposed method were varied from 1.6 to 2.6 % (RSD). The VALLME method has been proved to have the potential to be applied to the preconcentration of the target analytes. Moreover, the method is simple, high sensitivity, consumes much less solvent than traditional methods and environmental friendly.     

基于体外消化模型的食品中邻苯二甲酸酯生物有效性的测定

目的 建立固相萃取-高压液相色谱法检测体外消化模型消化液及固相残渣中邻苯二甲酸酯(PAEs)的方法。 方法 食品经体外消化模型处理后离心分为固液两相, 分别经溶剂提取、固相萃取柱净化后采用HPLC检测两相中的PAEs含量, 通过计算得到生物有效性值。结果 该方法在0.1~20 mg/L范围内线性关系良好, 相关系数均大于0.998, 方法的回收率在70.38%~96.49%之间, 相对标准偏差均低于7%。结论 该方法操作简单, 灵敏度和重现性好, 抗干扰能力强, 可用于食品中PAEs生物有效性的测定, 同时为进一步进行PAEs暴露评估和健康风险评估奠定基础。     

采用顶空固相微萃取和搅拌棒吸附萃取技术分析古井贡酒中香气成分

采用顶空固相微萃取(headspace solid-phase microextraction,HS-SPME)和搅拌棒吸附萃取(stir bar sorptive extraction,SBSE)技术,结合气相色谱-质谱联用仪对古井贡酒酒样香气成分进行提取分析。通过优化样品酒精度、萃取温度、萃取时间等参数确定了最优萃取条件,两种方法的整体精密度和重复性均较好。在相同条件下,对比两种萃取方法,SBSE的灵敏度和回收率均高于HS-SPME。通过标准品、保留指数、NIST 14谱库比对,共定性出190种化合物,其中用标准品准确定性143种。在白酒中首次发现4种酯类化合物:3-甲基丁酸己酯、丁酸辛酯、癸酸丙酯、癸酸异丁酯。     

顶空固相微萃取-气质联用法结合自动解卷积技术分析葛根中的挥发性成分

建立顶空固相微萃取-气相色谱-质谱结合自动解卷积技术检测葛根中挥发性物质的分析方法,以总峰面积和峰数目为考察指标,通过单因素试验和正交试验对不同萃取条件进行优化。结果表明,萃取温度对峰数目和总峰面积的影响较大,较佳萃取条件为样品量3.0 g、50/30 μm DVB/CAR/PDMS萃取头、萃取温度90 ℃、平衡时间13 min、萃取时间50 min、解吸时间5 min;在此条件下,鉴定出葛根挥发性成分67 种,分别为酯类11 种、醛类22 种、醇类9 种、酮类5 种、萜烯类8 种和12 种其他类物质。