Rapid determination of benzo(a)pyrene in processed meat and fish samples by second-derivative constant-energy synchronous fluorescence spectrometry

A simple, rapid and cost-effective method has been established for the determination of the quantity of benzo(a)pyrene (BaP), one of the most carcinogenic polycyclic aromatic hydrocarbons (PAHs), in roasted, smoked and charcoal grilled foods. Second-derivative constant-energy synchronous fluorescence spectrometry (DCESFS) improves the spectral resolution and selectivity of the fluorescence method. By using this method, processed meat, fish and some other food samples were analysed without resorting to complex pre-separation and purification procedures. The method was found to have a recovery of 97.7% ± 4.3%. The limit of detection (LOD) for BaP was 0.14 μg kg?1, far below the regulatory limit (1.0 μg kg?1) for BaP in food samples specified by the European Union. A certified reference material (Coconut oil, BCR?-458) was used to confirm the validity of the proposed method. The results suggest that the measurements are in a good agreement with the certified BaP concentrations (5.4% deviation). The results obtained by the proposed method for analysing BaP in food samples correlated well with those obtained by GC/MS.     

多维气相色谱/质谱法快速测定卷烟烟气中的苯并(a)芘

自行组装了一套具有全自动和在线富集功能的大孔径-毛细柱多维气相色谱(MDGC)系统。应用该系统,开发了一种简便快速且准确的检测卷烟烟气苯并(a)芘的方法。收集在剑桥滤片上的烟气冷凝物用环己烷提取和浓缩后,不需要任何净化,可直接进行MDGC-MS-SIM分析。方法的重现性、回收率和检测限均令人满意。对不同配方和过滤嘴的卷烟样品进行了定量测定,对样品的测定结果进行了比较。      

Aluminium content of some processed foods,raw materials and food additives in China by inductively coupled plasma–mass spectrometry

The level of aluminium in 178 processed food samples from Shenzhen city in China was evaluated using inductively coupled plasma–mass spectrometry. Some processed foods contained a concentration of up to 1226?mg/kg, which is about 12 times the Chinese food standard. To establish the main source in these foods, Al levels in the raw materials were determined. However, aluminium concentrations in raw materials were low (0.10–451.5?mg/kg). Therefore, aluminium levels in food additives used in these foods was determined and it was found that some food additives contained a high concentration of aluminium (0.005–57.4?g/kg). The results suggested that, in the interest of public health, food additives containing high concentrations of aluminium should be replaced by those containing less. This study has provided new information on aluminium levels in Chinese processed foods, raw materials and a selection of food additives.     

测定食品中苯并[a]芘的恒能量同步荧光光谱法研究

研究用恒能量同步荧光光谱法测定食品中的苯并[a]芘的含量,该方法与常规的荧光分光光度法比较具有可操作性强、准确度高和避免实验人员长时间受紫外线的照射等特点,可以定量测定苯并[a]芘的含量。并对特性基本相同的各种样品进行了加标回收检验,其回收率在85%以上,相关系数>0.9995,相对标准偏差为0.86%。     

A novel method for the rapid detection of benzo(a)pyrene in liquid milk by dimethyl sulfoxide selectively enhanced synchronous fluorescence spectrometry

Based on the high solubility efficiency and strong fluorescence response of benzo(a)pyrene (BaP) in dimethyl sulfoxide in combination with the high-performance derivative constant-energy synchronous fluorescence spectroscopic (DCESFS) technique, a simple, sensitive and economic method was developed for the determination of BaP in liquid milk. This method comprises ultrasound-assisted solvent extraction, solvent replacement and DCESFS detection. No saponification or other tedious clean-up procedures were needed. The recoveries of BaP in different milk samples were greater than 82%. Detection limits in full- and low-fat milk were 0.03 and 0.04 μg kg^–1, respectively.     

肉制品中3,4-苯并(a)芘的残留与检测

3,4-苯并(a)芘是肉制品在烟熏、烧烤过程中产生的一种多环芳烃化合物,是一种强致癌物质和诱变剂,对人类健康造成潜在的威胁。肉制品中3,4-苯并(a)芘的残留是影响肉制品安全及出口的主要因素。本文主要对肉制品中3,4-苯并(a)芘的产生途径及其影响因素、检测方法进行了详细的阐述。     

烟熏食品中苯并(a)芘的产生机理及防止方法

本文主要从当前备受关注的烟熏食品的安全问题出发,简述了烟熏食品中的有害物质--苯并(a)芘(benzo(a)pyrene)的产生机理、毒害、检测及防止方法,为今后更好的研究苯并(a)芘,控制其在烟熏食品中的含量提供一定的理论基础.     

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.     

食用油中苯并(a)芘的快速检测研究

采用间接免疫法结合显色反应快速检测食用油中苯并(a)芘,在抗体与磁珠上苯并(a)芘抗原结合的基础上,通过辣根过氧化酶连接苯并(a)芘二抗进行间接免疫反应。结果表明:优化的免疫磁珠反应条件为苯并(a)芘抗体用量4μg,辣根过氧化酶用量100μg,免疫反应温育时间60min;方法的线性范围为0. 5 pg/m L～500 ng/m L,检出限为0. 12μg/kg,定量限为0. 5μg/kg,加标回收率为89. 3%～100. 1%。方法具有良好的特异性和稳定性,符合食品污染物现场快速检测的基本要求。     

Determination of pesticides and their metabolites in processed cereal samples

Fifteen pesticides including some of their metabolites (disulfoton sulfoxide, ethoprophos, cadusafos, dimethoate, terbufos, disulfoton, chlorpyrifos-methyl, malaoxon, fenitrothion, pirimiphos-methyl, malathion, chlorpyrifos, terbufos sulfone, disulfoton sulfone and fensulfothion) were analysed in milled toasted wheat and maize as well as in wheat flour and baby cereals. The QuEChERS (quick, easy, cheap, effective, rugged and safe) methodology was used and its dispersive solid-phase extraction procedure was optimised by means of an experimental design with the aim of reducing the amount of co-extracted lipids and obtaining a clean extract. Gas chromatography with nitrogen phosphorus detection were used as the separation and detection techniques, respectively. The method was validated in terms of selectivity, recoveries, calibration, precision and accuracy as well as matrix effects. Limits of detection were between 0.07 and 34.8?µg?kg^?1 with recoveries in the range of 71–110% (relative standard deviations were below 9%). A total of 40 samples of different origin were analysed. Residues of pirimiphos-methyl were found in six of the samples at concentrations in the range 0.08–0.47?mg?kg^?1, which were below the MRLs established for this pesticide in cereal grains. Tandem mass spectrometry confirmation was also carried out in order to identify unequivocally the presence of this pesticide.     

QuEChERS-气相色谱-串联质谱法测定熟肉制品中9种N-亚硝胺类化合物

目的建立同时测定熟肉制品中9种N-亚硝胺类化合物的气相色谱-串联质谱分析方法。方法样品采用快速基质分散净化(QuEChERS)法处理后,用HP-INNOWax石英毛细管色谱柱(30 m×0.25 mm,0.25μm)分离,经气相色谱-串联质谱多反应监测技术进行定性及定量分析。结果 9种N-亚硝胺类化合物在0.20～50.00μg/kg范围内线性关系良好,相关系数均0.997,方法检出限为0.02～0.1μg/kg。3个加标水平的平均回收率为78%～120%,相对标准偏差为3.42%～15.24%。结论本方法准确、快速、灵敏度高,可用于熟肉制品中9种N-亚硝胺类化合物的检测。     

Changes of benzo(a)pyrene contents in smoked fish during storage

The paper refers to the determination of benzo(a)pyrene (BaP) contents in smoked fish by an HPLC method. Samples were analyzed after saponification and purification on Florisil and Separon SGX C-18, using selective fluorescence detection for the determination of BaP in smoked fish as well as in the model system, which was kept at the same conditions.

In the model system, the BaP degradation was found to be directly proportional to the duration of influence of environmental physicochemical factors with a clearly linear BaP decay line.

On the other hand, in the case of smoked fish the BaP contents were changed in dependence on diffusion into the internal product layers where their amount was relatively stabilized due to the absence of both light and oxygen.

Measurements have shown that BaP contents cannot be considered as a constant but that a gradual decrease is taking place as a result of various factors influencing the degradation process, which in itself can attain different velocities depending on the changing properties of the meat products as well as on environmental conditions.     

Survey of furan in heat processed foods by headspace gas chromatography/mass spectrometry and estimated adult exposure

Furan is a suspected human carcinogen that is formed in some processed foods at low ng per g levels. Recent improvements in analytical methodology and scientific instrumentation have made it possible to accurately measure the amount of furan in a wide variety of foods. Results from analysis of more than 300 processed foods are presented. Furan was found at levels ranging from non-detectable (LOD, 0.2–0.9 ng g^?1) to over 100 ng g^?1. Exposure estimates for several adult food types were calculated, with brewed coffee being the major source of furan in the adult diet (0.15 µg kg^?1 body weight day^?1). Estimates of mean exposure to furan for different subpopulations were calculated. For consumers 2 years and older, the intake is estimated to be about 0.2 µg kg^?1 body weight day^?1.     

Survey of furan in heat processed foods by headspace gas chromatography/mass spectrometry and estimated adult exposure

Furan is a suspected human carcinogen that is formed in some processed foods at low ng per g levels. Recent improvements in analytical methodology and scientific instrumentation have made it possible to accurately measure the amount of furan in a wide variety of foods. Results from analysis of more than 300 processed foods are presented. Furan was found at levels ranging from non-detectable (LOD, 0.2-0.9 ng g^-1) to over 100 ng g^-1. Exposure estimates for several adult food types were calculated, with brewed coffee being the major source of furan in the adult diet (0.15 µg kg^-1 body weight day^-1). Estimates of mean exposure to furan for different subpopulations were calculated. For consumers 2 years and older, the intake is estimated to be about 0.2 µg kg^-1 body weight day^-1.     

食用油中苯并(a)芘检测技术研究进展

概述了食用油中苯并(a)芘残留现状,介绍了当前在食用油苯并(a)芘残留分析中应用的液液萃取法、微波辅助萃取法、超声波辅助提取法、固相萃取法、固相微萃取法和超临界流体萃取法等样品前处理技术和色谱法、光谱法等检测方法的应用进展。提出了我国食用油中苯并(a)芘检测技术今后研究的重点和方向。     

Studies on the occurrence and formation of 2-(hydroxymethyl)-N-nitrosothiazolidine-4-carboxylic acid (HMNTCA) and 2-(hydroxymethyl)-N-nitrosothiazolidine (HMNTHZ) in various cured smoked meats,fish and cheese

Abstract : Because of the carcinogenic nature of many N-nitroso compounds, there is concern about their presence in foods. This paper presents some data on the levels of two non-volatile compounds (2-(hydroxymethyl)-N-nitrosothiazolidine-4-carboxylic acid (HMNTCA) and 2-(hydroxymethyl)-N-nitrosothiazolidine (HMNTHZ)) in various smoked foods such as 25 cured meats, eight smoked fish and seafoods, 15 smoked poultry products, and 17 smoked cheeses. All samples were negative for HMNTHZ, but 11 of the cured meats, six poultry products and two smoked fish contained HMNTCA at levels of 10–260 μg kg^?1. Upon frying, appreciable levels of HMNTHZ were formed in only one of 10 samples of cured meat products. The smoked cheeses were all negative for HMNTCA.     

Determination of nine preservatives in processed foods using a modified QuEChERS extraction and quantified by HPLC-PDA

ABSTRACT

In this study, a new method was developed for simultaneously determining nine preservatives, that is, benzoic acid (BA), sorbic acid (SOA), dehydroacetic acid (DHA) and PHBAs (methyl p-hydroxybenzoate [PHBA-me], ethyl p-hydroxybenzoate [PHBA-et], isopropyl p-hydroxybenzoate [PHBA-ipro], propyl p-hydroxybenzoate [PHBA-npro]), isobutyl p-hydroxybenzoate [PHBA-ibut] and butyl p-hydroxybenzoate [PHBA-nbut]), in processed foods, employing liquid chromatography (LC). This procedure accelerated sample preparation and improved efficiency by employing modified quick, easy, cheap, effective, rugged and safe (QuEChERS) extraction without clean-up. Samples were prepared with 20 mL of acetonitrile/water (1:1) with the assistance of a ceramic stone. The extract solutions were diluted 10 times or according to the detection amount and then injected into an LC-PDA. This method showed good linearity, and the LOQs were 10 mg/kg for BA, SOA and DHA and 5?mg/kg for the PHBAs. When validating this method, the recoveries of the nine preservatives were in the range 77.0–99.6%, RSD_r values were in the range 0.7–5.3% and those of RSD_wr were in the range 2.3–8.4%. These results suggest that this new method is highly reproducible.     

Rapid screening of illicit additives in weight loss dietary supplements with desorption corona beam ionisation (DCBI) mass spectrometry

Desorption corona beam ionisation (DCBI), the relatively novel ambient mass spectrometry (MS) technique, was utilised to screen for illicit additives in weight-loss food. The five usually abused chemicals – fenfluramine, N-di-desmethyl sibutramine, N-mono-desmethyl sibutramine, sibutramine and phenolphthalein – were detected with the proposed DCBI-MS method. Fast single-sample and high-throughput analysis was demonstrated. Semi-quantification was accomplished based on peak areas in the ion chromatograms. Four illicit additives were identified and semi-quantified in commercial samples. As there was no tedious sample pre-treatment compared with conventional HPLC methods, high-throughput analysis was achieved with DCBI. The results proved that DCBI-MS is a powerful tool for the rapid screening of illicit additives in weight-loss dietary supplements.     

液相色谱法测定食用油中苯并(a)芘含量结果的不确定度评定

摘 要: 目的：为了正确评估液相色谱法测定植物油中苯并(a)芘含量的准确性。方法：依据GB5009.27-2016《食品安全国家标准 食品中苯并(a)芘的测定》测定食用油中苯并(a)芘的含量，建立液相色谱-荧光检测器法测定食用油中苯并(a)芘的不确定度数学模型，通过分析其测定的过程，确定影响测定结果的不确定度主要分量来源，并计算出扩展不确定度。结果：称样量约为1g时，测量结果为：17.2μg/kg，扩展不确定度Up为1.3μg/kg，合成不确定度U C-rel 为3.9×10-2μg/kg，包含因子k=2。结论：该方法的建立可以有效评价食用油中苯并(a)芘的不确定度，为测量的准确性提供可靠的依据。     

Determination of PAHs in various smoked meat products and different samples by enzyme immunoassay

An enzyme immunoassay was used to determine benzo[a ]pyrene (BaP) in smoked meat products and other samples of food and environmental origin. The method used has a detection limit (3 σ) of 0.1 μg kg⁻¹ and a coefficient of variation less than 10%. The main aim of the study was to compare the possible influence of different smoking processes and packaging material on the amount of BaP deposited on smoked meat product, mainly different sausages. The lowest amount of BaP was found when smoke produced by steam in the indirect method smoking‐chamber was used. A slightly protective effect of polyamide casing was noted. © 1999 Society of Chemical Industry