快速溶剂萃取-凝胶渗透色谱净化-气相色谱-串联质谱分析猪肉中109种农药残留

目的建立一种同时分析猪肉中109种农药残留的气相色谱-串联质谱(GC-MS/MS)方法。方法样品经快速溶剂萃取仪提取,凝胶渗透色谱仪净化,加入内标环氧七氯,采用GC-MS/MS在多反应监测模式(MRM)下分析,内标法定量。结果 109种农药在10~500μg/L的浓度范围内线性关系良好,相关系数(r~2)大于0.99。各农药的检出限(S/N=3)为0.09~1.57μg/kg,各农药的定量限(S/N=10)为0.31~4.78μg/kg,在10.0、20.0和50.0μg/kg 3个水平的添加浓度下,回收率在68.3%~112.8%之间,相对标准偏差小于14.2%(n=6)。结论该方法准确可靠、灵敏度高,可用于猪肉中109种农药残留的同时检测。     

气相色谱-三重四级杆串联质谱法同时测定西红柿中47种农药残留

目的建立气相色谱-三重四级杆串联质谱(gas chromatography-triple quadrupole mass spectrometry,GC-MS/MS)同时测定西红柿基质中47种农药残留的方法。方法西红柿样品经乙腈提取,QuEChERS方法净化,加入内标环氧七氯,采用GC-MS/MS法在多反应监测模式(multiple reaction monitor,MRM)下分析。结果 47种农药在20~1500 ng/mL浓度范围内呈现良好的线性关系,相关系数(r~2)大于0.99,各农药检出限(S/N=3)为0.07~3.12μg/kg,47种农药在3个浓度添加水平(16、32、160μg/kg)时,回收率在57.5%~124.5%之间,相对标准偏差(relative standard deviation,RSD)为0.74%~19.07%。结论该方法快速、灵敏、准确、高通量,可用于西红柿中47种农药残留的快速测定和确证。     

QuEChERS-气相色谱-三重四极杆质谱法同时测定枸杞中46种农药残留

建立了QuEChERS结合气相色谱-三重四极杆质谱法(GC-MS/MS)同时检测枸杞中46种农药残留的方法。样品经乙腈提取后,使用无水硫酸镁、N-丙基乙二胺(N-propyl ethylenediamine,PSA)进行净化,以HP-5MS色谱柱分离待测物,GC-MS/MS采用多反应监测(multiple reaction monitoring mode,MRM)模式检测,基质匹配外标法定量。结果表明,46种农药在0.01~0.20 μg/mL范围内线性关系良好,相关系数r>0.99。方法检出限(S/N=3)在0.02~3.90 μg/kg的范围内,方法定量限(S/N=10)在0.05~12.99 μg/kg的范围内;在10、50、100 μg/kg的加标水平下,46种化合物平均加标回收率达71.5%~99.8%,相对标准偏差为0.7%~8.9%。10批次枸杞样品中4批次检出农药残留,含量范围为19.4~262 μg/kg。该方法快速、灵敏、准确,适用于枸杞中多种农药残留的检测。     

QuEChERS-气相色谱-三重四级杆质谱法检测韭菜中6种农药残留

目的建立QuEChERS-气相色谱-三重四级杆质谱法(gas chromatography-triple quadrupole mass spectrometry,GC-MS/MS)检测韭菜中氧乐果、甲拌磷、毒死蜱、氟虫腈、腐霉利及溴氰菊酯6种农药。方法结合QuEChERS的前处理,分别比较了石墨化炭黑柱、C_(18)柱、PSA柱对样品的净化效果,利用GC-MS/MS进行检测,外标法进行定量。结果 6种农药在相应的范围内线性关系均良好,相关系数均在0.99以上,方法检出限(S/N=3)在0.05~0.85μg/kg的范围内,方法定量限(S/N=10)在0.25~2.83μg/kg的范围内,在0.05、0.1、0.2、0.5 mg/kg的加标水平下,6种农药的回收率为87.3%~112.8%,相对标准偏差为7.6%~16.8%。结论该方法灵敏、高效、准确度高,适合韭菜中多数农药残留的快速检测。     

QuEChERS-气相色谱-串联质谱法同时测定高粱中16种农药残留

摘 要：目的 建立了三重四极杆气质联用仪GC-MS/MS 结合改良的 QuEChERS 方法同时检测高粱中16种农药多残留的分析方法。方法 高粱粉末加水浸润后,加入WondaPak QuEChERS提取盐试剂包Ⅱ均质提取,取上清液加入WondaPak QuEChERS 净化管Ⅲ净化,氮吹近干,定容至1mL,基质内标法定量。结果 在质量浓度为0.05~1.00μg/mL范围内,各农药的线性关系良好,线性回归方程的相关系数（R2）均大于0.998,方法检出限为0.00124μg/kg ~0.654μg/kg。分别向阴性高粱样品中添加16种农药标准品浓度为0.01mg/kg、0.10mg/kg和0.50mg/kg的3个水平,其加标平均回收率为78.54%~102.22%,相对标准偏差RSD%（n=6）为1.23%~9.52%。结论 与其他农药残留检测方法比,该方法具有前处理操作简单,重复性好,灵敏度高,简化样品前处理过程,降低分析成本等优势,适用于高粱样品中常用农药的高灵敏度快速检测。     

气液微萃取仪联用气相色谱-质谱仪检测果蔬中农药残留量

目的建立气液微萃取仪(gas-liquid microextraction,GLME)与气相色谱质谱联用仪(gas chromatographymass spectrography,GC-MS)测定食品中农药残留。方法称取0.1 g匀浆样品直接加入GLME中进行萃取净化,定容至100μL,结合内标法通过GC-MS检测分析。结果 30种农药在0.001~1 mg/kg浓度范围内线性良好,相关系数在0.9951~0.9999,检出限为0.001~0.021 mg/kg,定量限为0.003~0.070 mg/kg,平均回收率为67%~119%(n=3),相对标准偏差在1%~26%之间。结论该方法快速、准确,能满足果蔬类中多种农药残留的定性定量分析。     

气相色谱-串联质谱法测定茶叶茶汤中多种农药残留量

目的采用Qu ECh ERS方法和气相色谱-串联质谱(gas chromatography-tandem mass spectrometry,GC-MS/MS)分析技术,建立茶叶茶汤中65种不同极性农药残留量的快速检测方法。方法利用乙腈(含1%乙酸)提取茶叶茶汤样品,分散固相萃取法净化样品,GC-MS/MS检测采用选择反应监测模式(selective reactions monitoring,SRM),灵敏度最高的离子对用作定量。结果 65种农药在3个浓度添加水平上的加标回收率范围是76%~134.6%,相对标准偏差(RSD,n=6)范围为1.0%~18.41%,茶叶样品定量限是0.15~3.0μg/kg,茶汤样品定量限是0.1~1.5μg/kg。结论该方法灵敏度高,准确性好,快速简便,适用于绿茶、乌龙茶、白茶和红茶中多种农药残留量的检测。     

QuEChERS结合气相色谱-三重四级杆串联质谱法测定动植物混合型食品中多种农药残留

建立了气相色谱串联质谱(GC-MS/MS)定量和定性检测动植物混合型食品中7种农药残留量的方法。样品中的待测农药组分经乙腈-乙酸乙酯混合溶剂(85∶15,v/v)提取,采用改进的Qu ECh ERS法为净化方法,以外标法进行定量,以气相色谱-三重四级杆串联质谱(GC-MS/MS)多反应监测模式(MRM)检测。在动植物混合性食品基质中,以该方法检测的大部分农药的线性范围为0.01μg/L~0.50μg/L,检测低限最低可以达到1.0μg/kg,添加回收率为67.2%~118.6%,相对标准偏差(RSD)为5.2%~16.3%(n=6)。该方法的准确性高、重复性好、操作简便,适用于动植物混合型食品中多种农药残留同时测定。     

QuEChERS-GC-MS/MS法同时测定稻草中的106种农药残留

建立了一种稻草中106种农药残留的气相色谱-三重四极杆串联质谱检测方法。样品经QuEChERS技术提取和净化后,采用GC-MS/MS在选择反应监测模式(SRM)下定性定量。结果表明,(1)106种农药在稻草中的定量限(LOQ)为1.1~49.2μg/kg;(2)在4~492μg/L范围内,线性相关系数为0.9905~0.9999;(3)在稻草样品中添加浓度在36.5~1255.0μg/kg之间时,平均回收率在65.2%~124.1%之间,RSD在0.6%~19.4%之间;(4)该方法农药种类覆盖广、前处理简便、溶剂用量少,可应用于稻草中106种农药残留的快速筛查与定量分析。     

猪肉、猪肝中 17 种全氟烷基化合物的HPLC-MS/MS 测定

目的建立猪肉、猪肝中17种全氟烷基化合物(perflurorinated alkylated substances,PFASs)的高效液相色谱-串联质谱(HPLC-MS/MS)检测方法。方法样品经酸化乙腈提取、混合吸附剂纯化后,应用HPLC-MS/MS技术检测,以Poroshell 120 EC-C18为色谱柱,甲醇-5 mmol/L乙酸铵水溶液梯度洗脱,多反应监测负离子模式扫描,同位素内标法定量,内标物为经13C或者18O标记的相应外标物。结果应用该方法检测猪肉样品中17种全氟烷基化合物的检出限(LOD,S/N=3)为0.009~0.047μg/kg,在猪肝样品中的检出限(LOD,S/N=3)为0.003~0.031μg/kg;在0.5μg/kg、1.0μg/kg、1.5μg/kg三个加标浓度下,该方法的平均加标回收率约为80%~110%,平均相对标准偏差(RSD)小于10%。结论该方法可有效应用于猪肉、猪肝中17种全氟烷基化合物的检测。     

Reliable identification of grapevine rootstock varieties using RAPD PCR on woody samples

Since grapevine ( Vitis spp .) rootstock material is being traded increasingly as disbudded woody material a lack of distinctive morphological features on such material necessitates an alternative and reliable means of identification. Methods described here were developed for rapid and efficient extraction of DNA from woody samples rich in phenolic compounds and polysaccharides, and for subsequent identification of varieties by RAPD PCR. Using these methods, and with the application of only one selected RAPD primer, we were able to differentiate sixteen rootstock varieties, including the seven varieties most commonly used in Germany. Problems commonly encountered with reproducibility of RAPD patterns were avoided by choosing primers with a dinucleotide sequence and a high G/C content that allowed a rather high annealing temperature of 45°C. Methods described here should also be useful for other horticultural crops, especially those with woody tissues rich in phenolic compounds and polysaccharides.     

Chlorohydrins of bisphenol A diglycidyl ether (BADGE) and of bisphenol F diglycidyl ether (BFDGE) in canned foods and ready-to-drink coffees from the Japanese market

BADGE.2HCl and BFDGE.2HCl were determined in 28 samples of ready-to-drink canned coffee and 18 samples of canned vegetables (10 corn, 5 tomatoes and 3 others), all from the Japanese market. HPLC was used as the principal analytical method and GCMS for confirmation of relevant LC fractions. BADGE.2HCl was found to be present in one canned coffee and five samples of corn, BFDGE.2HCl in four samples of canned tomatoes and in one canned corn. No sample was found which exceeded the 1mg/kg limit of the EU for the BADGE chlorohydrins. However the highest concentration was found for the sum of BFDGE.2HCl and BFDGE.HCl.H₂O at a level of 1.5mg/kg. A Beilstein test confirmed that all cans containing foods contaminated with BADGE.2HCl or BFDGE.2HCl had at lest one part coated with a PVC organosol.     

Aroma characterization of various apricot varieties using headspace–solid phase microextraction combined with gas chromatography–mass spectrometry and gas chromatography–olfactometry

The characterization of the aromatic profile of several apricot cultivars with molecular tracers in order to obtain objective data concerning the aromatic quality of this fruit was undertaken using headspace–solid phase microextraction (HS–SPME). Six apricot cultivars were selected according to their organoleptic characteristics: Iranien, Orangered, Goldrich, Hargrand, Rouge du Roussillon and A4025. The aromatic intensity of these varieties measured by HS–SPME–Olfactometry were defined and classified according to the presence and the intensity of grassy, fruity and apricot like notes. In the six varieties, 23 common volatile compounds were identified by HS–SPME–GC–MS. Finally, 10 compounds, ethyl acetate, hexyl acetate, limonene, β-cyclocitral, γ-decalactone, 6-methyl-5-hepten-2-one, linalool, β-ionone, menthone and (E)-hexen-2-al were recognized by HS–SPME–GC–O as responsible of the aromatic notes involved in apricot aroma and considered as molecular tracers of apricot aromatic quality which could be utilized to discriminate apricot varieties.     

European priorities for research to support legislation in the area of food contact materials and articles

A strong science base is required to underpin the planning and decision-making process involved in determining future European community legislation on materials and articles in contact with food. Significant progress has been made in the past 5 years in European funded work in this area, with many developments contributing to a much better understanding of the migration process, and better and simpler approaches to food control. In this paper this progress is reviewed against previously identified work-areas (identified in 1994) and conclusions are reached about future requirements for R&D to support legislation on food contact materials and articles over the next 5 or so years.     

Textural Properties of Cold-set Gels Induced from Heat-denatured Whey Protein Isolates

A 9% whey protein (WP) isolate solution at pH 7.0 was heat-denatured at 80°C for 30 min. Size-exclusion HPLC showed that native WP formed soluble aggregates after heat-treatment. Additions of CaCl2 (10–40 mM), NaCl (50–400 mM) or glucono-delta-lactone (GDL, 0.4–2.0%, w/v) or hydrolysis by a protease from Bacillus licheniformis caused gelation of the denatured solution at 45°C. Textural parameters, hardness, adhesiveness, and cohesiveness of the gels so formed changed markedly with concentration of added salts or pH by added GDL. Maximum gel hardness occurred at 200 mM NaCl or pH 4.7. Increasing CaCl2 concentration continuously increased gel hardness. Generally, GDL-induced gels were harder than salt-induced gels, and much harder than the protease-induced gel.     

Tests of potential functional barriers for laminated multilayer food packages. Part I: Low molecular weight permeants

The advent of the functional barrier concept in food packaging has brought with it a requirement for fast tests of permeation through potential barrier materials. In such tests it would be convenient for both foodstuffs and materials below the functional barrier (sub-barrier materials) to be represented by standard simulants. By means of inverse gas chromatography, liquid paraffin spiked with appropriate permeants was considered as a potential simulant of sub-barrier materials based on polypropylene (PP) or similar polyolefins. Experiments were performed to characterize the kinetics of the permeation of low molecular weight model permeants (octene, toluene and isopropanol) from liquid paraffin, through a surrogate potential functional barrier (25 μm-thick oriented PP) into the food simulants olive oil and 3% (w/v) acetic acid. These permeation results were interpreted in terms of three permeation kinetic models regarding the solubility of a particular model permeant in the post-barrier medium (i.e. the food simulant). The results obtained justify the development and evaluation of liquid sub-barrier simulants that would allow flexible yet rigorous testing of new laminated multilayer packaging materials.     

Occurrence of bisphenol-F-diglycidyl ether (BFDGE) in fish canned in oil

The levels of bisphenol-F-diglycidyl ether (BFDGE) were quantified as part of a European survey on the migration of residues of epoxy resins into oil from canned fish. The contents of BFDGE in cans, lids and fish collected from all 15 Member States of the European Union and Switzerland were analysed in 382 samples. Cans and lids were separately extracted with acetonitrile. The extraction from fish was carried out with hexane followed by re-extraction with acetonitrile. The analysis was performed by reverse phase HPL C with fluorescence detection. BFDGE could be detected in 12% of the fish, 24% of the cans and 18% of the lids. Only 3% of the fish contained BFDGE in concentrations considerably above 1mg/kg. In addition to the presented data, a comparison was made with the levels of BADGE (bisphenol-A-diglycidyl ether)analysed in the same products in the context of a previous study.     

Contribution of European research to risk analysis

The European Commission's, Quality of Life Research Programme, Key Action 1—Health, Food & Nutrition is mission-oriented and aims, amongst other things, at providing a healthy, safe and high-quality food supply leading to reinforced consumer confidence in the safety of European food. Its objectives also include the enhancing of the competitiveness of the European food supply. Key Action 1 is currently supporting a number of different types of European collaborative projects in the area of risk analysis. The objectives of these projects range from the development and validation of prevention strategies including the reduction of consumers risks; development and validation of new modelling approaches; harmonization of risk assessment principles, methodologies, and terminology; standardization of methods and systems used for the safety evaluation of transgenic food; providing of tools for the evaluation of human viral contamination of shellfish and quality control; new methodologies for assessing the potential of unintended effects of genetically modified (genetically modified) foods; development of a risk assessment model for Cryptosporidium parvum related to the food and water industries; to the development of a communication platform for genetically modified organism, producers, retailers, regulatory authorities and consumer groups to improve safety assessment procedures, risk management strategies and risk communication; development and validation of new methods for safety testing of transgenic food; evaluation of the safety and efficacy of iron supplementation in pregnant women; evaluation of the potential cancer-preventing activity of pro- and pre-biotic ('synbiotic') combinations in human volunteers. An overview of these projects is presented here.     

Influence des ions sur le pouvoir hydratant de l'ure e: e tude sur peau de porc ex vivo

This study deals with the influence of ions (NaCl and MgSO4) in a W/O emulsion containing 10% urea. Moisturization kinetics are assessed by corneometry on pig skin ex vivo. The formula's influence on urea penetration is measured by infrared spectrometry with an ATR device and the stripping method. Corneometry and spectroscopy were chosen to record simultaneously the hydratation levels and urea localization into superficial cell layers. Urea crystallization after evaporation of emulsions and aqueous solutions is described. Results show that urea does not hydrate nor penetrate when applied to the skin through an aqueous gel. In a W/O emulsion, sodium chloride increases the ability of urea to moisturize without improving penetration. In vitro urea crystallization is disturbed by sodium chloride or magnesium sulphate for solutions and emulsions. This stabilization by ions is correlated with good moisturization values. The stabilization of urea in the solute state provided by ions increases its water epidermal binding capacity without enhancing penetration.