高效液相色谱法测定食品中的几种重要金属元素

研究了用2－（2－喹啉偶氮）－5－二乙氨基酚（QADEAP）为柱前衍生试剂，甲醇（内含0．2％醋酸）和pH4.0醋酸－醋酸钠缓冲溶液梯度洗脱为流动相，Waters Nova-Pak-C18液相色谱柱为固定相，二极管矩阵检测器检测，高效液相色谱法分离测定食品中铁、钴、镍、铜、锌和锰的方法。根据信噪比（S／N＝3）各金属离子的检测限分别为：铁3．2μg/L，钴4．1μg/L，镍2．6μg/L，铜4．4μg/L，锌5．0μg/L，锰8．0μg/L，方法相对标准偏差在1．6％－3．5％之间，标准回收率在93％－107％，方法用于食品样品中痕量铁、钴、镍、铜、锌、锰的测定，结果令人满意。     

乳粉中叶黄素的测定方法及稳定性的影响

建立一种测定配方奶粉中叶黄素质量分数的高效液相色谱方法，采用YMCTM色谱柱（5μm，250mm ×4．6mm），流动相为甲醇-甲基叔丁基醚（85∶15），等度洗脱，流速为1．0ml/min，检测波长445nm，该方法在0．3～6．0mg/L的质量范围内线性良好（ R＝0．99993），基质加标水平为0．30μg/g、0．60μg/g、3．0μg/g时，回收率分别介于96．52％～98．10％之间，相对标准偏差介于1．31％～4．66％之间，方法检出限为0．05μg/g，说明该方法可行。同时，研究一定的温度、加热时间及光照等条件对乳粉中叶黄素稳定性的影响，得出随着温度提高、加热时间及光照时间的延长，叶黄素含量呈递减趋势，且变化显著（ P＜0．05）。     

高效液相色谱-串联四极杆质谱联席测定饼干中丙烯酰胺残留量

建立饼干中丙烯酰胺残留的高效液相色谱-串联四极杆质谱联用测定方法。该方法经纯水提取样品,以ZORBAXSB-Aq柱（4．6×150mm,5μm）分离,流动相为0．1％甲酸水溶液和乙腈（体积比为97：3）,电喷雾正离子MRM模式检测。该方法的检出限0．3μg／L,方法定量下限3．0μg/kg,线性范围0．3μg,/L-100．0μg/L,加标回收率91．5％～99．5％．相对标准偏差为4．44％。     

HPLC-MS联用测定果冻等食品中的3种甜味剂和苯甲酸

建立食品中糖精钠、甜蜜素、安赛蜜和苯甲酸的高效液相色谱-质谱（HPLC-MS）检测方法。色谱柱为Spherigel C18（5μm,4．6×200Mm）,流动相为：（A）甲醇-（B）甲酸-三乙胺缓冲盐,梯度洗脱;电喷雾负离子（ESI^-）采集模式,流速为1．0mL／min,进样量为10μL;以华法林钠为内标,质谱定性定量;安赛蜜、糖精钠、甜蜜素、苯甲酸的线性范围分别为：5．4～135,5．4～135,7．4～111,10～150μg／mL,加样回收率为93．19％～100．90％,RSD为1．05％～2．04％．该方法具有选择性好、分析时间短、定性定量准确等优点,可用于果冻等食品中的4种目标物定性定量检测。     

四-（对甲基苯基）-卟啉柱前衍生，高效液柱色谱法测定食品中痕量铅、镉、汞

研究了用四-(对甲基苯基)-卟啉柱前衍生，高效液相色谱法测定食品中痕量铅、镉、汞的方法。食品样品用湿法消化后，消化液中的铅、镉、汞用四-(对甲基苯基)-卟啉(T4MPP)柱前衍生，然后用甲醇(内含0．01mol／L四氢吡咯-醋酸缓冲盐)和四氢呋喃(内含0．01mol／L四氢吡咯-醋酸缓冲盐)为流动相梯度洗脱，Waters Xterra^TMRP18(3．9150mm，5μm)色谱柱为固定相分离铅、镉、汞的T4MPP络合物，用二极管矩阵检测器检测，铅、镉、汞含量在0．01～3mg／L范围内与峰面积成线性关系，根据信噪比(S／N=3)，方法检测限为：铅2．3μg／L、镉1．8μg／L和汞2.5μg／L，方法相对标准偏差为2．1％～3．5％，标准回收率为93％～106％，该方法用于测定食品中的铅、镉、汞，结果令人满意。     

高效液相色谱测定猪肉中醋酸美仑孕酮的残留

建立了高效液相色谱测定猪肉样品中新型兽药醋酸美仑孕酮残留的方法。样品用V（甲醇）：V（0．1％H3PO4）=70：30混合溶液提取,经离心后用PCX固相萃取小柱净化,以Symmetry C8色谱柱为分离柱,线性范围为10～500μg／kg,检出限为5．0μg／kg,平均回收率为93．1～105．5％,相对标准偏差为1．5～4．6％,批间相对标准偏差为1．8～5．6％,检测效果良好。     

酱油中Monacolin K的高效液相色谱分析

采用Polaris C18色谱柱（100×2．0mmid,3μm）,水（含0．5％H3PO4）、乙腈为流动相,梯度洗脱,流速0．20mL／min,柱N500c,测定波长（λ）237nm,分析了酱油中MonacolinK,结果显示,MonacolinK在0．2mg/L-5mg／L时显线性关系,加样平均回收率为90．7％,相对标准偏差0．93％-2．7％。     

高效液相色谱法测定糖蜜中的甜菜碱含量

建立了一种简单、快速测定甜菜糖蜜中甜菜碱的方法,即样品经去离子水提取,碱式醋酸铅脱色后,采用高效液相色谱-DAD检测器测定甜菜碱的含量。色谱柱为AgilentZorbaxNH2柱（Φ4．6mm×150mm,5Ixm）,流动相为0．05mol／L KH2PO4溶液（pH=4．53）,流速0．7mL／min,柱温30℃,检测波长195nm。试验结果表明：甜菜碱在0．1mg／mL～5．0mg／mL范围内线性良好,相关系数为0．998;加标回收率为99．5％～99．7％,相对标准偏差（RSD）为0．09％-1．06％（n=3）。     

RP-HPLC法测定桑叶中的芦丁和异槲皮苷含量

目的：建立HPLC法测定桑叶中芦丁、异槲皮苷含量的定量分析方法。方法：HPLC外标法。采用色谱柱：Agilent TC-C18柱（250mm×4．6mm,5μm）;流动相：乙腈．甲醇．水．磷酸（100：10：340：0．3,V／V）;检测波长365nm;流速1．0ml／min;进样量20u1;柱温：室温。结果：在上述色谱条件下,芦丁、异槲皮苷获良好分离,浓度分别在7．5～150μg／ml（R2=0．9995）、7．1～142μg／ml（R2=0．9998）范围内呈良好的线性关系,平均加样回收率为98．79％、99．01％,RSD分别为3．37％、2．43％,重复性实验RSD分别为0．0133％和0．0214％。结论：该方法分离度好,简便快速,为桑叶生药及其制剂的质量控制提供可借鉴的分析方法。     

液相色谱-串联质谱同时测定婴幼儿奶粉中5种四环素类抗生素残留

本文建立了婴幼儿配方奶粉中5种四环素类抗生素残留量的高效液相色谱-串联四极杆质谱联用测定方法。该方法用0．005mol／LNa2EDTA水溶液提取样品,以ZORBAX Aq-C18柱（2．1×150mm,5μm）分离,流动相为乙腈和0．1％甲酸水溶液（梯度洗脱）,电喷雾正离子MRM模式检测。该方法的检出限0．5ng／ml～1．0ng／ml,方法定量下限5．0μg／kg～10μg／kg,线性范围0．5ng／ml～20．0ng／ml,加标回收率84．2％～92．3％,相对标准偏差为2．20％～4．07％。     

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.     

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.     

低温带皮菜籽粕微粉的不同粒级部分的功能特性

为研究低温带皮菜籽粕微粉的不同粒级部分的功能特性,以经低温脱脂的带皮菜籽粕为原料,经微粉碎后筛分成212~425μm、150~212μm和106~150μm的3个不同粒级的微粉样品,检测这些样品的吸水性、吸油性、乳化性和乳化稳定性、蛋白质体外消化率。结果表明:1 3个不同粒级的微粉样品之间的粗纤维含量存在显著差异,表明三者的结构组成成分有一定差异。23个微粉样品的乳化活性和乳化稳定性随粒度级别的减小而显著增加(P0.01)。33个微粉样品的蛋白质体外消化率随粒度级别的减小而显著增加(P0.01)。4不同粒级带皮菜籽粕微粉样品的吸水性与吸油性受其结构组成物质不同和粒度的双重影响,与粒度的相关性不明显。     

Microbiology of food taints

Fresh and processed foods are often spoilt by the presence of undesirable flavours and odours caused by microbial action. The aim of this paper is to review the current knowledge of microbiologically induced taints that occur in a wide range of foodstuffs, including meats, poultry, fish, crustaceans, milk, dairy products, fruits, vegetables, cereals and cereal products. Examples have been chosen where the compounds responsible for the taint have been identified and sufficient data obtained to demonstrate the involvement of microorganisms. However, in some cases the full identity of the causative organism may not have been elucidated. The types of microorganisms covered by this review include bacteria, fungi, yeasts, actinomycetes and cyanobacteria. Although cyanobacteria do not in general infect foods, their presence in aqueous systems and water supplies can lead to off-flavours in aquatic organisms and processed foodstuffs. Several examples of each of these processes are discussed. Wherever possible, the likely biosynthetic pathway used by the microorganism to produce the offending compound in a foodstuff is indicated.     

Analysis for organic residues from aids to polymerization used to make plastics intended for food contact

Polymers intended for food contact use have been analysed for organic residues which could be attributed to a range of substances employed as polymerization aids (e.g. initiators and catalysts). A wide range of polymers was extracted with solvents and the extracts analysed by gas chromatography-mass spectrometry (GC-MS). The overwhelming majority of substances identified were not derived from aids to polymerization but were oligomers, additives and adventitious contaminants. However, a small number of substances were identified as initiator residues. These included tetramethylsuccinonitrile (TMSN) which was observed in two polymers and it derived from recombination of two azobisisobutyronitrile (AIBN) initiator radicals. Methyl benzoate, benzoic acid, biphenyl and phenyl benzoate were detected in one poly(methyl methacrylate) sample and in two polyvinylchlorides and they are thought to be derived from benzoyl peroxide initiator. TMSN was subsequently targeted for analysis of poly-(methyl methacrylate) plastics using proton nuclear magnetic resonance spectrometry (¹     

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

Experiments were performed to characterize the kinetics of the permeation of different medium molecular weight model permeants: bisphenol A, warfarin and anthracene, from liquid paraffin, through a surrogate potential functional barrier (25 microns-thick orientated polypropylene--OPP) into the food simulants olive oil and 3% (w/v) acetic acid. The characterization of permeation kinetics generally observed the permeation models previously reported to explain the experimental permeation results obtained for a low molecular weight group of model permeants. In general, the model permeants exhibited behaviour consistent with their relative molecular weights with respect to (a) the time taken to attain steady-state permeation into the food simulant in which they were more soluble, (b) their subsequent steady-state permeation rates, and (c) their partition between liquid paraffin and the OPP membrane.     

The development of reference materials for paralytic shellfish poisoning toxins in lyophilized mussel. I: Interlaboratory studies of methods of analysis

This paper describes the first part of a project undertaken to develop mussel reference materials for Paralytic Shellfish Poisoning (PSP) toxins. Two interlaboratory studies were undertaken to investigate the performance of the analytical methodology for several PSP toxins, in particular saxitoxin (STX) and decarbamoyl-saxitoxin (dc-STX) in lyophilized mussels, and to set criteria for the acceptance of results to be applied during the second part of the project: the certification exercise. In the first study, 18 laboratories were asked to measure STX and dc-STX in rehydrated lyophilized mussel material and to identify as many other PSP toxins as possible with a method of their choice. In the second interlaboratory study, 15 laboratories were additionally asked to determine quantitatively STX and dc-STX in rehydrated lyophilized mussel and in a saxitoxin-enriched mussel material. The first study revealed that three out of four postcolumn derivatization methods and one pre-column derivatization method sufficed in principle to determine STX and dc-STX. Most participants (13 of 18) obtained acceptable calibration curves and recoveries. Saxitoxin was hardly detected in the rehydrated lyophilized mussels and results obtained for dc-STX yielded a CV of 58% at a mass fraction of 1.86 mg/kg. Most participants (14 out of 18) identified gonyautoxin-5 (GTX-5) in a hydrolysed extract provided. The first study led to provisional criteria for linearity, recovery and separation. The second study revealed that 6 out of 15 laboratories were able to meet these criteria. Results obtained for dc-STX yielded a CV of 19% at a mass fraction of 3.49mg/kg. Results obtained for STX in the saxitoxin-enriched material yielded a CV of 19% at a mass fraction of 0.34mg/kg. Saxitoxin could not be detected in the PSP-positive material. Hydrolysis was useful to confirm the identity of GTX5 and provided indicative information about C1 and C2 toxins in the PSP-positive material. The methods used in the second interlaboratory study showed sufficiently consistent analysis results to undertake a certification exercise to assign certified values for STX and dc-STX in lyophilized mussel.     

The Ministry of Environmental Protection Issued "Feasible Technology Guidelines for Pollution Prevention and Control in Wood Pulping Process of the Paper Industry (Trial)" and Two Other Guiding Technical Documents

On December 27t＂, 2013, the Ministry of Environmenta Protection announced that, in order to implement ＂The Environmental Protection Law of the People＇ s Republic of China＂, improve the working system in environmenta protection technologies, and promote technologica advancement in pollution prevention, the Ministry of Environmental Protection sponsored the formulation of three guiding technical documents including ＂Feasible Technology Guidelines for Pollution Prevention and Contro n Wood Pulping Process of the Paper Industry （Trial）＂     

1~(st) Intelli-Tissue~ EcoEc Tissue Machine Supplied by PMP Group Successfully Put into Operation in China

正On April 29th,2014,Intelli-Tissue EcoEc tissue machine supplied by PMP Group successfully put into operation at Hebei Xuesong Paper Co.,Ltd.,this is the first such kind of paper machine of PMP Group in China.