远红外烤制对烤鱼品质及多环芳烃含量的影响

为了改善烤鱼的质构特性等食用品质,减少多环芳烃的形成,以草鱼为对象,研究传统炭烤和远红外烤制方式对烤鱼质构特性及多环芳烃含量的影响。结果表明：传统炭烤和远红外烤制对烤鱼的食用品质有不同影响,与传统炭烤鱼肉相比,远红外烤制鱼肉硬度显著降低（P＜0.05）,且剪切力均显著低于传统炭烤组（P＜0.05）,能够显著改善烤制鱼肉的嫩度;相对而言,远红外烤制鱼肉具有更优的质构特性;远红外烤制能显著降低烤鱼肉中PAH4（苯并(a)蒽、?、苯并(k)荧蒽、苯并(a)芘）和PAH16（萘、苊烯、苊、芴、菲、蒽、荧蒽、芘、苯并(a)蒽、?、苯并(b)荧蒽、苯并(k)荧蒽、苯并(a)芘、茚苯(1,2,3-c,d)芘、二苯并(a,h)蒽、苯并(g,h,i)芘）的生成量（P＜0.05）,与传统炭烤鱼肉相比,PAH4和PAH16总生成量分别下降39.07%和44.07%。     

高效液相色谱-荧光检测法检测植物性食品中14种欧盟优控多环芳烃

目的 建立准确测定蔬菜、水果及粮食中多环芳烃含量,了解河北省内上述食品中14种欧盟优控多环芳烃(苯并(c)芴、苯并(a)蒽、?、5-甲基?、苯并(j)荧蒽、苯并(b)荧蒽、苯并(k)荧蒽、苯并(a)芘、二苯并(a,l)芘、二苯并(a, h)蒽、苯并(g,h,i)苝、茚并(1,2,3-cd)(a)芘、二苯并(a,e)芘、二苯并(a,i)芘、二苯并(a,h)芘)的实际污染状况。方法 样品经环己烷：乙酸乙酯(1:1, V:V)溶液超声提取后,浓缩至近干,经正己烷复溶后通过多环芳烃专用固相萃取柱进行净化处理,洗脱液经浓缩后用乙腈定容,采用液相色谱-荧光检测法进行检测。结果 14种化合物的线性范围为1.00~18.0μg/kg;方法回收率为60.9%~125.4%,相对标准偏差为2.2%~7.6%;苯并(c)芴、苯并(a)蒽、?、5-甲基-1,2-苯并菲、苯并(j)荧蒽、苯并(b)荧蒽、苯并(k)荧蒽、苯并(a)芘、二苯并(a,e)芘、二苯并(a,i)芘、二苯并(a,h)芘检出限为0.15μg/kg;二苯并(a,l)芘、二苯并(a, h)蒽、苯并(g,h,i)苝、茚并(1,2,3-cd)芘检出限为0.3μg/kg。市售的96份样品中, 检出不同种类不同含量的多环芳烃类化合物, 检出率为51.0%。结论 本方法重现性好,检测灵敏度高,可用于水果、蔬菜及粮食中14种多环芳烃的检测。     

水蒸气蒸馏脱臭对食用油中多环芳烃脱除效果的研究

以花生油为原料,研究水蒸气蒸馏脱臭过程以及脱臭条件对油脂中多环芳烃脱除效果的影响。结果表明:脱臭对油脂中多环芳烃的脱除具有一定的作用,脱臭温度越高、脱臭时间越长,多环芳烃的脱除效果越好。在脱臭温度270℃、脱臭时间120 min、脱臭残压80 Pa、直接蒸汽用量固定的条件下,花生油中Bap、PAH4、LPAHs、HPAHs及PAH16含量分别从24.00、129.2、667.44、96.50和763.94μg/kg降低至14.21、74.64、344.46、55.34及399.80μg/kg,脱除率分别为40.79%、42.23%、48.39%、42.65%及47.67%。油脂脱臭过程中多环芳烃各组分的脱除率有所不同,其中萘、苊、苊烯和芴4种轻质多环芳烃的脱除率达到70%以上,其他轻质多环芳烃组分的脱除率不足60%。重质多环芳烃中二苯并(a,h)蒽的脱除率最高,为61.65%,茚并(1,2,3-c,d)芘的脱除率最低,为37.59%。     

我国主产区油茶持久性有机污染物分布特征及相关性研究

为了明确油茶中持久性有机污染物(POPs)的污染分布特征,利用气相色谱-三重四极杆串联质谱(GC-MS/MS)对我国主产区45个采样点135批次油茶果不同部位及对应油茶林土壤进行16种多环芳烃(PAHs)、18种多氯联苯(PCBs)和21种有机氯(OCPs)污染水平分析。同时分析油茶籽仁和油茶林土壤中主要POPs之间相关性。结果表明:油茶果各部位及油茶林土壤PAHs污染以萘、苊烯、苊萘嵌戊烷、荧蒽等低环PAHs污染较为明显;PCBs污染程度很轻,含量均在1μg/kg以下;OCPs污染主要为狄氏剂、毒杀芬、α-六六六、硫丹、异狄氏剂和艾氏剂。油茶籽仁中荧蒽与菲具有强正相关(R~2=0.90);油茶林土壤中芴与菲,■与苯并(a)蒽、苯并(b)荧蒽、苯并(k)荧蒽、苯并(a)芘和苯并(a)蒽,PCB138与茚并(1,2,3-cd)芘,PCB180与苯并(g,h,i)苝,p,p′-DDE与o,p′-DDT、p,p′-DDD之间均具有较强相关性(R~2=0.81～0.98)。     

冷冻除脂-气相色谱-串联质谱法检测食用植物油中30 种多环芳烃

建立冷冻除脂--气相色谱-串联质谱检测食用植物油中30?种多环芳烃（polycyclic aromatic hydrocarbons,PAH）的方法。选用6?种氘标记PAH为内标,样品经乙腈--丙酮溶液（4∶1,V/V）于离心管中涡旋提取,10?000?r/min离心5?min,－80?℃对油脂冷冻固化,倾出提取液,再经减压浓缩和氮气吹干,以二氯甲烷复溶,气相色谱--串联质谱多反应监测方式进行检测。结果表明,在相应质量浓度范围内30?种PAH均有良好线性（R2＞0.998）,检出限为0.10～1.83?μg/kg,定量限为0.35～6.11?μg/kg,在5、20?μg/kg和50?μg/kg添加水平下的回收率为67.77%～119.28%,相对标准偏差为1.18%～12.47%。采用本方法对市售11?类38?个食用植物油样品的检测显示,萘、1-甲基萘、2--甲基萘、联苯、2,6--二甲基萘、苊烯、苊、2,3,6--三甲基萘、芴、二苯并噻吩、菲、蒽、1-甲基菲、荧蒽、芘、环戊烯[c,d]芘、苯并[a]蒽、屈、苯并[b]荧蒽、苯并[k]荧蒽、苯并[e]芘和苯并[a]芘的检出率均为100%;5--甲基屈、苝、茚并[1,2,3--c,d]芘、二苯并[a,h]蒽、苯并[g,h,i]苝和二苯并[a,l]芘的检出率分别为86.84%、63.16%、81.58%、21.05%、81.58%和26.32%;二苯并[a,e]芘和二苯并[a,h]芘未检出;PAH总量为92.56～905.16?μg/kg,其中苯并[a]芘含量为1.94～7.40?μg/kg,依据食品安全标准限量,PAH处于较安全水平。     

油脂煎炸过程中多环芳烃含量的变化

对大豆油、米糠油和棕榈油进行油条煎炸试验,之后对不同煎炸时间油脂中多环芳烃含量进行检测分析,研究煎炸时间对油脂中多环芳烃含量的影响。结果表明:随着煎炸时间的延长,3种油脂中Bap、PAH4、PAH16的含量都呈现明显上升趋势。在32 h的煎炸过程中,大豆油Bap、PAH4、PAH16的含量(μg/kg)分别从原油的1.58、6.88、18.73增加至3.93、10.35;56.10,米糠油Bap、PAH4、PAH16的含量分别从原油的2.52、6.50、25.53增加至3.10、10.34、100.71;棕榈油Bap、PAH4、PAH16的含量分别从原油的1.67、8.60、25.23增加至2.26、10.95、59.98。在高温煎炸过程中,多环芳烃各组分含量的增幅是不同的。大豆油中增幅最大的组分是苊,增幅最小的是苯并(b)荧蒽;米糠油中增幅最大的也是苊,增幅最小的是苯并(g,h,i)苝;棕榈油中增幅最大的是芴,增幅最小的是苯并(a)蒽;3种油脂中轻质多环芳烃含量及增幅都要远多于重质多环芳烃。     

GC-MS法测定多种食用油中的多环芳烃

多环芳烃是一类常见的环境有机污染物,随着人们对其毒性研究逐步深入,各国相继制定限量要求。随机选取市面上不同种类的食用油,采用GC-MS法进行多环芳烃的测定,评估其食品安全风险。结果表明, 15种食用油中苯并[a]芘含量在0.00～9.20μg/kg之间,苯并[a]芘、苯并[a]蒽、苯并[b]荧蒽和苯并菲的含量之和在0.00～28.74μg/kg之间, 16种多环芳烃总量在0.00～72.47μg/kg之间。对随机网上购买食品安全风险较高的10份芝麻油进行测定,苯并[a]芘含量在0.00～6.76μg/kg之间,苯并[a]芘、苯并[a]蒽、苯并[b]荧蒽和苯并菲的总量在0.00～9.64μg/kg之间,16种多环芳烃总量在0.00～16.18μg/kg之间。植物油中多环芳烃含量水平相差较大,部分存在一定的食品安全风险,出口企业还应关注苯并[a]芘、苯并[a]蒽、苯并[b]荧蒽和苯并菲含量的水平。     

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。     

三种光敏剂介导的光动力对水体中8种多环芳烃的降解作用

为了探究不同光敏剂(姜黄素、核黄素、金丝桃素)介导的光动力对水体中多环芳烃的降解作用,以含有8种多环芳烃的水体为研究对象,在光敏剂浓度为10μM,光照时间为15 min的条件下,采用光动力方法处理并通过同步荧光法测定水体中的各种多环芳烃。结果表明,姜黄素介导的光动力对多环芳烃的降解效果明显优于核黄素和金丝桃素介导的光动力组。经姜黄素光动力处理后,水体中的8种多环芳烃均发生一定程度的降解,其中,荧蒽和菲的降解率分别为77.07%和78.31%,苯并[k]荧蒽和?的降解率分别为80.10%和85.95%,苯并[a]芘、萘、苯并[a]蒽和蒽的降解率达到95%以上。以上研究表明,与其他两种光敏剂相比,姜黄素介导的光动力对水溶液中的8种多环芳烃均具有显著的降解效果,为该技术在生活用水以及养殖水体污染治理方面的推广应用提供理论依据。     

烟熏液对卤煮牛肉中12种多环芳烃含量的影响

采用固相微萃取-高效液相色谱(荧光检测器)检测法,研究添加不同质量分数烟熏液(0.05%~1.0%)对卤煮牛肉中12种多环芳烃含量的影响。结果表明:12种多环芳烃中10种在卤煮牛肉中被检测出,总量为355.76 ng/g,其中萘(naphthalene,NA)含量最多,达到302.14 ng/g。添加烟熏液后,多环芳烃的总量显著降低(P<0.01),并随着烟熏液质量分数的增加,总量呈现明显降低趋势。在添加烟熏液质量分数为1%时,多环芳烃的总量由对照组355.76 ng/g降低到12.17 ng/g,其中苊(acenaphthene,AC)、苯并[k]荧蒽(benzo(k)fluoranthene,Bk FA)和苯并[a]芘(benzo(a)pyrene,Ba P)甚至检测不到。因此,烟熏液对卤煮牛肉中多环芳烃的形成具有良好的抑制作用,这种作用可能与其抗氧化性有关。     

高效液相色谱-二极管阵列检测器-荧光检测器法测定植物油中的18 种多环芳烃

建立凝胶渗透色谱法净化样品、高效液相色谱-二极管阵列串联荧光检测器法同时测定植物油中18 种多环芳烃的检测方法。样品经环己烷-乙酸乙酯（1∶1,v/v）溶解,利用凝胶渗透色谱法去除油脂大分子,PAH C18柱分离,乙腈和水作流动相进行梯度洗脱,设置荧光检测程序,以2 个发射波长通道同时采集数据,测定油样中的17 种多环芳烃,以二极管阵列检测器测定苊烯。结果表明：方法检出限为0.5～4 ng/mL,样品回收率在78.65%～103.4%之间,相对标准偏差小于5%。本方法满足德国标准对18 种多环芳烃的同步检测新要求。     

Simultaneous formation of polycyclic aromatic hydrocarbons (PAHs) and heterocyclic aromatic amines (HCAs) in gas-grilled beef satay at different temperatures

This study investigated the simultaneous formation of polycyclic aromatic hydrocarbons (PAHs) and heterocyclic aromatic amines (HCAs) in gas-grilled beef satay at different temperatures (150, 200, 250, 300, and 350°C). Solid-phase extraction (SPE) was used for sample clean-up. Fifteen PAHs were determined using high performance liquid chromatography with fluorescence detection (HPLC-FLD) and nine HCAs were quantified using liquid chromatography tandem-mass spectrometry (LC-MS/MS) with a gradient programme. The lowest significantly concentrations of PAHs and HCAs were generated at 150°C; the formation of PAHs and HCAs simultaneously increased with temperatures. Benzo[a]pyrene was detected in all samples and increased markedly at 300 and 350°C. The sums of 4 PAHs (PAH4) in marinated beef satay at 300 and 350°C exceeded the maximum level in Commission Regulation (EU) 2015/1125. Significant reductions of polar and non-polar HCAs (except PhIP) were found in marinated beef satay across all temperatures. Overall, PAHs and HCAs showed opposite trends of formation in beef satay with marination.     

Optimization and validation of an extraction method for the analysis of polycyclic aromatic hydrocarbons in chocolate candies

Abstract: Chocolate is a key ingredient in many foods such as milk shakes, candies, bars, cookies, and cereals. Chocolate candies are often consumed by mankind of all age groups. The presence of polycyclic aromatic hydrocarbons (PAHs) in chocolate candies may result in health risk to people. A rapid, precise, and economic extraction method was optimized and validated for the simultaneous determination of polycyclic aromatic hydrocarbons in chocolate candy by high‐performance liquid chromatography (HPLC) and gas chromatography‐mass spectrometry (GS‐MS) as a confirmatory technique. The method was optimized by using different solvents for liquid–liquid extraction, varying volume of de‐emulsifying agent, and quantity of silica gel used for purification. The HPLC separation of 16 PAHs was carried out by C‐18 column with mobile phase composed of acetonitrile : water (70 : 30) in isocratic mode with runtime of 20 min. Limit of detection, limit of quantification (LOQ), and correlation coefficients were found in the range of 0.3 to 4ng g^?1, 0.9 to 12ng g^?1, and 0.9109 to 0.9952, respectively. The exploration of 25 local chocolate candy samples for the presence of PAHs showed the mean content of benzo[a]pyrene as 1.62 ng g^?1, which representing the need to evaluate effective measures to prevent more severe PAHs contamination in chocolate candies in future. Practical Application: Chocolate is one of the most favorite food items among people, especially children. Chocolate candies are often consumed by mankind of all age groups. Chocolate candies are often consumed by children in large quantities. The presence PAHs in chocolate candies may result in health risk to people. In the present study, a precise and cost effective rapid method was employed for the determination of PAHs, which can be employed for daily routine analysis of PAHs in chocolate products.     

A novel cloud-point extraction process for preconcentrating selected polycyclic aromatic hydrocarbons in aqueous solution

A novel but simple cloud-point extraction (CPE) process is developed to preconcentrate the trace of selected polycyclic aromatic hydrocarbons (PAHs) with the use of the readily biodegradable nonionic surfactant Tergitol 15-S-7 as extractant. The concentrations of PAHs, mixtures of naphthalene and phenanthrene as well as pyrene, in the spiked samples were determined with the new CPE process at ambient temperature (23 degrees C) followed by high performance liquid chromatography(HPLC) with fluorescence detection. More than 80% of phenanthrene and pyrene, respectively, and 96% of naphthalene initially present in the aqueous solutions with concentrations near or below their aqueous solubilities were recovered using this new CPE process. Importantly Tergitol 15-S-7 does not give any fluorometric signal to interfere with fluorescence detection of PAHs in the UV range. No special washing step is, thus, required to remove surfactant before HPLC analyses. Different experimental conditions were studied. The optimum conditions for the preconcentration and determination of these selected PAHs at ambient temperature have been established as the following: (1) 3 wt% surfactant; (2) addition of 0.5 M Na2SO4; (3) 10 min for equilibration time; and (4) 3000 rpm for centrifugal speed with duration of 10 min.     

多环芳烃分子印迹柱-高效液相色谱荧光检测法快速测定烤肉中15 种多环芳烃

建立一种高效液相色谱-荧光检测（high performance liquid chromatography-fluorescence detection,HPLC-FLD）法同时测定烤肉中15 种多环芳烃（polycyclic aromatic hydrocarbons,PAHs）的方法。样品经超声提取,多环芳烃分子印迹柱（molecular imprinting column of PAHs,MIP-PAHs）净化,通过HPLC分离,外标法定量。结果表明：15 种PAHs在质量浓度1～50 ng/mL范围内与色谱峰面积呈良好的线性关系,r＞0.999 5;在5.0、10.0、25.0 μg/kg 3 个加标水平下,平均回收率为71.1%～98.8%,相对标准偏差为1.0%～5.8%;方法检出限（RS/N=3）为0.33～3.30 μg/kg,定量限（RS/N=10）为1.0～10.0 μg/kg。     

Rapid determination of polycyclic aromatic hydrocarbons in natural tocopherols by high-performance liquid chromatography with fluorescence detection

A simple and rapid method has been developed and validated for the determination of seventeen polycyclic aromatic hydrocarbons (PAHs) in natural tocopherol products. Samples were dissolved in n-hexane, cleaned by an alumina column, and separated and determined by reversed-phase high-performance liquid chromatography (HPLC) with fluorescence detection. The recoveries were greater than 77.9%, except for the lowest molecular weight PAHs (Na, 1-Me, 2-Me, AC, F) which were between 15.9% and 75.8%. The limits of quantification were less than 0.38 ng/g for the heavy PAHs and less than 1.50 ng/g for the light PAHs. Good repeatabilities were achieved with RSD less than 10.7% for all the objective compounds. This method has been applied to evaluating PAHs contents in various natural tocopherol products and controlling natural tocopherol product quality.     

Study of several aspects of a general method for the determination of polycyclic aromatic hydrocarbons in liquid smoke flavourings by gas chromatography-mass spectrometry

The effectiveness of the steps of a general method, which includes alkaline treatment of the samples, extraction, clean-up and analysis, for the determination of polycyclic aromatic hydrocarbons in liquid smoke flavourings and smoked foods have been studied, by using mixtures of pure polycyclic aromatic hydrocarbons and of smoke flavouring compounds. All these products were applied to samples of liquid smoke flavourings in order to test the effectiveness of each step of the method, as well as to investigate its effect on real samples, and thus obtain a suitable procedure for the study of polycyclic aromatic hydrocarbons in liquid smoke flavourings. The alkaline treatment has been proved to be necessary because of its capability for removing some smoke components. Both cyclohexane and dichloromethane are able to extract polycyclic aromatic hydrocarbons with high recovery percentages; however, cyclohexane is more adequate due to its lower ability to extract other smoke flavourings components. It is important to note that the elution sequence of polycyclic aromatic hydrocarbons during the clean-up step is quite different depending on the solvent used to dissolve the extract, which determines the ability of this process to isolate polycyclic aromatic hydrocarbons for their accurate identification and quantification by gas chromatography-mass spectrometry in selected ion monitoring mode. Finally, the PAHs present in a liquid smoke flavouring and their concentrations were determined; it was observed that, despite the different extraction solvents and clean-up procedures used, the results were very similar.     

Removal of polycyclic aromatic hydrocarbons from water by migration into polyethylene

Water was spiked with three polycyclic aromatic hydrocarbons (PAHs) and filled into a steel diffusion chamber. Low-density polyethylene sheet combined of five polyethylene foils was used as a partition in the chamber. Depth of PAHs migration into the sheet was followed for 143 h, using high performance liquid chromatography with selective fluorimetric detection after extraction of PAHs from the foils peeled off. On the basis of the results obtained, the process of PAHs migration into PE was characterised as a one-dimensional diffusion into polyethylene bulk. The diffusion coefficients were calculated for individual compounds using the second Fick law. It was concluded that PAHs are primarily adsorbed on the polyethylene surface with subsequent migration into bulk polymer. Transportation of PAHs through the bulk can be described satisfactorily by Fickian laws of diffusion and is consistent with the theory of the depth adsorption of PAHs in polyethylene.     

Polycyclic aromatic hydrocarbons (PAHs) levels in propolis and propolis-based dietary supplements from the Italian market

Propolis and propolis-based extracts, attained from beekeepers and the local market, were analysed for the presence of 13 polycyclic aromatic hydrocarbons (PAHs), including eight high molecular weight PAHs (PAH8), recently indicated by the European Food Safety Authority (EFSA) as suitable indicators of the presence of carcinogenic and genotoxic PAH in foods. An analytical procedure based on microwave assisted saponification/extraction, high performance liquid chromatography (HPLC) and spectrofluorometric detection, has been developed. About half of the samples analysed presented benzo[a]pyrene (BaP) concentrations exceeding 2 μg/kg, which is proposed as a regulatory limit for dietary supplements. A product-by-product approach (based on maximum recommended dosage) was used to calculate PAH exposure. Even thought the majority of the samples gave low exposure levels when compared to exposure levels from other diet constituents, PAH intakes deriving from a daily consumption of some of the investigated products provided an important contribution to the total dietary intake and lead to margin of exposure (MOE) values which are of concern for human health.     

Determination of Polycyclic Aromatic Hydrocarbons in Seafood

The aim of this project is to determine polycyclic aromatic hydrocarbons (PAHs) in several seafood matrices, i.e., fish, and mussel, by the use of comprehensive two-dimensional gas chromatography-quadrupole mass spectrometry (GCXGC-MS). The procedure involves a simple extraction of PAHs, a filtration and concentration step followed by GCXGC-MS analysis. PAHs were determined in fish tissue samples by GCXGC-MS and by a standard high-pressure liquid chromatography fluorescence detector method. A Bland–Altman analysis of the two methods was performed. It indicated equivalence between the two methods. Analysis of mussel tissue (National Institute of Standards and Technology (NIST)-SRM 2974a) was performed. The results were in line with the official results of NIST.