食用油中多环芳烃检测的前处理方法研究进展

近年来,食用油中多环芳烃的检出多有报道,其安全问题备受社会关注。多环芳烃作为一类复杂的高亲脂性有机污染物,具有致畸致癌性,易在食用油的生产加工贮存过程中残留,对人体健康造成危害。因此,开发快速准确的分析方法检测食用油中的多环芳烃对于认识和应对食用油中多环芳烃的危害有着重要的理论和实践价值,其中分析检测过程的关键环节是选择合适的前处理方法。本文首先对食用油脂中多环芳烃进行概述,同时重点综述了近年来检测食用油中多环芳烃的常用样品前处理方法,并比较了不同前处理方法的优缺点,最后对未来多环芳烃检测方法的发展方向进行了展望,以期为开发更高效的油脂中多环芳烃检测的前处理方法提供参考。     

肉制品中多环芳烃前处理技术研究进展

多环芳烃是肉制品中常见的污染物,具有强致癌性。肉制品中多环芳烃含量极低,所以,一个好的前处理方法直接关系到检测的准确度。本文综述了肉制品中多环芳烃的前处理方法,对食品中多环芳烃的检测具有重要意义。     

肉制品中多环芳烃前处理技术的研究进展

综述了索氏提取、超声波萃取、固相萃取、加速溶剂萃取等前处理技术，在肉制品中多环芳烃前处理技术中的应用进展，并对肉制品中多环芳烃前处理技术的发展趋势进行了展望。     

食用油中多环芳烃的研究进展

多环芳烃(PAHs)是一类普遍存在的食品污染物,是国内外公认的高毒性物质。部分PAHs具有致癌性和遗传毒性,没有致癌性的PAHs也可能作为促癌剂。食用油由于其亲脂性更易遭受PAHs的污染,含有PAHs的油脂将加剧其在肠道中的吸收,从而严重威胁人类健康。综述了食用油中PAHs的来源途径、控制措施、前处理技术和检测方法,旨在为解决其污染问题提供参考。     

液相色谱-串联质谱法检测食用油脂中多环芳烃

建立了有机溶剂萃取、硅胶固相萃取柱净化、液相色谱-串联质谱法(LC-MS/MS法)测定食用油脂中EPA 16种多环芳烃的检测方法。EPA 16种多环芳烃的定量限分别为0.02~0.43μg/kg,回收率为86.5%~104.6%,日内精密度小于6%,日间精密度小于5%。在40个受测油脂样品中,EPA 16种多环芳烃的含量范围为11.68~146.06μg/kg。对照我国GB 2716规定,所有受测样品中苯并(a)芘含量均不超过≤10μg/kg的限量标准。然而,8个油样的苯并(a)芘含量超过了欧盟≤2μg/kg的限量标准,10个油样的PAH4含量超过了欧盟≤10μg/kg的限量标准。     

食用油中多环芳烃的研究进展

多环芳烃(PAHs)是指2个或2个以上苯环以稠环形式相连的一类化合物,具有基因毒性和致癌性.对食用油中PAHs的来源、检测方法及控制和脱除方法进行了详尽的阐述,并指出PAHs前处理方法和控制、脱除方法是未来的研究方向.     

肉制品中多环芳烃检测方法研究进展

多环芳烃作为一种挥发性芳香族烷烃化合物,具有致畸性、致癌性、致突变性以及遗传毒性,被认定为影响人类健康的主要有机污染物。肉制品因含有大量脂肪、蛋白质等营养成分,在加工过程中易产生多环芳烃,对人体健康存在潜在威胁。近年来随着多环芳烃相关毒性的研究,由其引起的食品安全问题得到越来越多的关注,因此本文论述了近年来肉制品中多环芳烃的前处理方法及其检测方法,同时对多环芳烃检测分析的研究方向进行了展望,以期为开发准确、快速、高效和绿色的检测分析方法提供参考。     

食用油脂多环芳烃污染研究进展

食用油脂多环芳烃污染问题近期引起广泛关注。该文探讨食用油脂中多环芳烃污染现状、产生原因、脱除方法、分析方法等,并提出监控食用油脂多环芳烃措施。     

SPE净化-同位素稀释-GC-MS法检测食用油脂中16种多环芳烃

研究建立了乙腈超声提取、硅胶SPE柱净化、DB–5MS毛细管柱分离、同位素稀释法定量检测食用油中16种多环芳烃的气质联用(GC–MS)方法。油脂样品采用乙腈提取、硅胶SPE柱净化,减少了有机溶剂的消耗,再采用16种同位素内标法定量,定量结果更加准确。结果表明:16种多环芳烃在1~100μg/kg范围内线性关系良好,线性相关系数为0.998 9~0.999 9,检出限为0.06~0.17μg/kg,定量限为0.18~0.56μg/kg。16种目标物在2、5、10μg/kg加标水平下的各组分回收率在84.36%~114.35%之间,相对标准偏差在0.12%~10.36%之间(n=6)。21个受测样品中16种多环芳烃的总含量为30.83±0.66~793.13±16.96μg/kg。除全部浓香型油脂及1个花生油外,所有受试油样中Ba P和PAH4含量均达到欧盟限量指标(Ba P≤2μg/kg,PAH4≤10μg/kg),浓香型油脂样中PAHs的污染情况较为严重。从油脂品类来看,低温制油和浸出精炼成品油的多环芳烃的风险低于浓香型油脂。     

纳米多孔材料在食品中多环芳烃分析样品前处理的应用研究进展

多环芳烃（PAHs）作为在食品中广泛存在的一种持久性污染物,因其具有致癌性、致畸性和毒性备受重视。因此,如何快速、高效地检测食品中的PAHs是研究的热点,在食品分析检测过程中,样品前处理是分析来自不同基质的PAHs的至关重要的一环。当前用于分析PAHs的传统前处理技术通常耗时长、灵敏度低、消耗大量有害有机溶剂且易丢失分析物,而基于纳米多孔材料的固体萃取法是一类高效、绿色、经济的前处理技术。本综述讨论了近年来纳米多孔材料对食品中多环芳烃分析前处理的研究进展,对比了不同样品前处理技术的优缺点,旨在为检测食品中的PAHs提供高效、便捷的前处理技术借鉴。     

Survey of polycyclic aromatic hydrocarbons of vegetable oils and oilseeds by GC-MS in China

There is a lack of information regarding the occurrence and content of contamination of polycyclic aromatic hydrocarbon (PAH) in edible vegetable oils and oilseeds used for oil production in China. By combining the advantages of ultrasound-assisted extraction, low temperature separation and silica SPE purification, a method for the determination of the USEPA, 16 PAHs was developed based on GC-MS to fill this gap. The method recoveries for oils and oilseeds were 84.4–113.8% and 84.3–115.3%, respectively. The LODs and LOQs for 16 PAHs were ranged from 0.06–0.17 and 0.19–0.56 μg kg^–1, respectively. Based on the established method, PAH concentrations in 21 edible oils and 17 oilseeds were determined. Almost all the PAHs were found in all the samples tested, especially the light PAHs (LPAHs). Three oil samples exceeded the maximum level of 10 μg kg^–1 for BaP set by China. However, five and six oil samples, respectively, exceeded the maximum limits of 2 and 10 μg kg^–1 set for BaP and PAH4 by the European Union. The concentrations of PAH16 in oilseed samples were 1.5 times higher than corresponding oil samples. The relationships between PAH4 and PAH8, PAH4 and PAH16 as well as PAH8 and PAH16 indicates that PAH4 is a sufficient surrogate for the contamination level of PAHs in edible oils when compared with PAH8.     

食品中多环芳烃及卤代多环芳烃的研究进展

综述了多环芳烃及卤代多环芳烃的性质、毒性及国内外食品中的污染情况和研究现状,并对目前的分析测定方法进行了介绍,希望为我国开展食品领域内多环芳烃和卤代多环芳烃的研究提供参考。     

油茶籽油中多环芳烃残留检测高效预处理方法的建立

目的建立一种高效的油茶籽油中多环芳烃(PAHs)残留检测预处理方法—凝胶渗透色谱(GPC)净化浓缩法。方法对适量油茶籽油样品添加与不添加PAHs混合标准液处理,经GPC系统净化,并利用系统配置的荧光检测器,比较2个监测样品各组分分离时段图谱,从而获得PAHs的最佳搜集时段,辅以回收率验证。结果对GB/T 24893-2010检测方法进行了优化,并对无PAHs油茶籽油样品进行加标处理,经回收试验,该方法在10~50μg/kg范围内的加标回收率范围为78.21%~95.64%,标准偏差为1.39%~4.55%。结论该方法简化了油茶籽油样品预处理步骤、减少了人工耗时、提高了检测效率,适合实验室批量检测。     

HPLC determination of polycyclic aromatic hydrocarbons in olive oils

 In this paper, HPLC with spectrofluorimetric detection was applied to the determination of polycyclic aromatic hydrocarbons (PAHs) in olive oils. These compounds may sometimes contaminate vegetable oils because of their specific lipophilic characteristics, which are a significant problem for their extraction and purification from lipid matrices. Some improvements to previously published methods are introduced and satisfactory results for repeatability and recovery were obtained. Data on 51 authentic olive oil samples are reported and it was found that there is usually a limited presence of PAHs in extra virgin olive oils; furthermore, the analysis of some blends of refined and virgin oils shows that the distributions of light and heavy PAHs are different with the content of the former being lower in refined samples. As an example of this fact, two samples of lampante oil were followed throughout the refining step. Received: 23 September 1996 / Revised version: 17 December 1996     

食用植物油中多环芳烃含量水平调查分析

调查了8类、116个食用植物油样品中的苯并(a)蒽、■、苯并(b)荧蒽和苯并(a)芘的污染情况。采用简单的液-液萃取法进行前处理,GC-MS/MS测定。结果表明:不同品种食用植物油多环芳烃含量差异较大;苯并(a)芘的检出率为85.34%,检出结果范围为0.59~9.75μg/kg;4种多环芳烃总量的检出率为100%,检出结果范围为0.88~59.17μg/kg;苯并(a)芘含量与4种多环芳烃总量成线性关系。     

Single-laboratory validation of a saponification method for the determination of four polycyclic aromatic hydrocarbons in edible oils by HPLC-fluorescence detection

An analytical method is reported for the determination of four polycyclic aromatic hydrocarbons (benzo[a]pyrene (BaP), benz[a]anthracene (BaA), benzo[b]fluoranthene (BbF) and chrysene (CHR)) in edible oils (sesame, maize, sunflower and olive oil) by high-performance liquid chromatography. Sample preparation is based on three steps including saponification, liquid–liquid partitioning and, finally, clean-up by solid phase extraction on 2 g of silica. Guidance on single-laboratory validation of the proposed analysis method was taken from the second edition of the Eurachem guide on method validation. The lower level of the working range of the method was determined by the limits of quantification of the individual analytes, and the upper level was equal to 5.0 µg kg^?1. The limits of detection and quantification of the four PAHs ranged from 0.06 to 0.12 µg kg^?1 and from 0.13 to 0.24 µg kg^?1. Recoveries of more than 84.8% were achieved for all four PAHs at two concentration levels (2.5 and 5.0 µg kg^?1), and expanded relative measurement uncertainties were below 20%. The performance of the validated method was in all aspects compliant with provisions set in European Union legislation for the performance of analytical methods employed in the official control of food. The applicability of the method to routine samples was evaluated based on a limited number of commercial edible oil samples.     

煎炸油中多环芳烃污染情况及其健康风险评估

目的 了解煎炸油中多环芳烃(PAHs)污染水平,并评估其对人群造成的健康风险。方法 利用2015年和2017年PAHs专项监测中158份煎炸油样品的8种PAHs污染水平数据,以及其中76份样品14种PAHs污染水平数据,结合我国普通人群植物油消费量,采用暴露情景假设的方法,计算膳食暴露量和暴露限值(MOE),评估其健康风险。结果 煎炸油样品中14种PAHs化合物的检出率范围为0.0%～100.0%,其中苯并(a)芘的检出率为83.5%(132/158)。二苯并(a,h)蒽污染水平最高,均值为3.33 μg/kg,其次分别为苯并(a)蒽、艹屈、苯并(a)芘,均值分别为2.25、2.21、1.91 μg/kg。艹屈 是14种PAHs中最主要的化合物,占14种PAHs的比例为18.6%。经煎炸油摄入的苯并(a)芘、苯并(a)芘+艹屈 、苯并(a)芘+艹屈 +苯并(a)蒽+苯并(b)荧蒽、苯并(a)芘+艹屈 +苯并(a)蒽+苯并(b)荧蒽+苯并(k)荧蒽+二苯并(a,h)蒽+苯并(g,h,i)芘+茚并(1,2,3-cd)芘的平均暴露量分别为0.99、2.13、4.36、7.90 ng/kg BW,其MOE值分别为70 707、79 812、77 982、62 025,均远大于10 000。结论 基于当前监测的煎炸油中PAHs污染水平,我国普通人群经煎炸油摄入PAHs的健康风险在极端暴露的情况下较低。     

Gas chromatography-mass spectrometry (GC-MS) method for the determination of 16 European priority polycyclic aromatic hydrocarbons in smoked meat products and edible oils

A gas chromatography-mass spectrometry (GC-MS) method was developed for the analysis of 15 polycyclic aromatic hydrocarbons (PAHs) highlighted as carcinogenic by the Scientific Committee on Food (SCF) plus benzo[c]fluorine (recommended to be analysed by the Joint FAO/WHO Expert Committee on Food Additives (JECFA)) in fat-containing foods such as edible oils and smoked meat products. This method includes accelerated solvent extraction (ASE) and the highly automated clean-up steps gel permeation chromatography (GPC) and solid-phase extraction (SPE). Using a VF-17ms GC column, a good separation of benzo[b]fluoranthene, benzo[j]fluoranthene and benzo[k]fluoranthene was achieved. Furthermore, the six methylchrysene isomers and the PAH compounds with a molecular weight of 302 Daltons in fat-containing foods attained a better chromatographic separation in comparison with a 5-ms column. The reliability of the analytical method for edible oils was demonstrated by the results from a proficiency test. Measurements with GC-high-resolution mass spectroscopy (HRMS) and gas chromatography-mass selective detection (GC-MSD) led to comparable results. A survey of the 16 PAHs in 22 smoked meat products showed concentrations in the range <0.01–19 µg kg^?1. The median concentration for benzo[a]pyrene was below 0.15 µg kg^?1.     

油籽炒籽条件对油脂中多环芳烃含量影响的研究

以花生仁和芝麻籽为原料,研究了炒籽温度和炒籽时间对其油脂中16种多环芳烃含量的影响。结果表明,随着炒籽温度的提高及炒籽时间的延长,花生油和芝麻油中Bap、PAH4、PAH16的含量都呈明显上升趋势。对照GB2716及欧盟No 835/2011中对Bap、PAH4的限量规定,花生仁的合理炒籽温度为不超过160℃、炒籽时间不超过20 min,芝麻的合理炒籽温度为不超过180℃、炒籽时间不超过20 min。在优化的炒籽条件下,花生油中Bap、PAH4、PAH16含量(μg/kg)分别从原料中的0.31、4.60、16.69增加至1.07、11.98、48.86,芝麻油中Bap、PAH4、PAH16含量分别从原料中的0.63、5.23和21.84增加至0.93、8.28和47.95。