离子色谱-质谱联用同时测定海产加工品中亚氯酸盐、氯酸盐、高氯酸盐和溴酸盐

建立了离子色谱-质谱联用技术同时测定海产加工品中亚氯酸盐、氯酸盐、高氯酸盐和溴酸盐的分析方法。选用高容量、亲水性的Ion Pac AS16(250 mm×2 mm)阴离子交换柱为分析柱,以EGC(自动淋洗液发生器)在线产生KOH为淋洗液,采用外接水模式,串联质谱进行检测。质谱以MRM(多元反应监测)模式分别监控以下离子对:亚氯酸盐m/z 66.9/50.8、氯酸盐m/z 84.3/68.9、高氯酸盐m/z 98.9/82.9和溴酸盐m/z 126.8/112.9,并以峰面积定量。结果表明,在一定的质量浓度范围内,4种阴离子的色谱峰面积与质量浓度呈线性相关,线性相关系数(r)均大于0.999,在1、5、10μg/L 3个加标水平下,4种目标离子的平均回收率均在89.6%~96.4%范围内,RSD(相对标准偏差)均在3.7%~5.3%之间(n=6)。该方法对亚氯酸盐、氯酸盐、高氯酸盐、溴酸盐的检出限(S/N=3)分别为0.2、0.5、0.01、0.02μg/L。上述研究表明,此方法可用于海产加工品中痕量亚氯酸盐,氯酸盐、高氯酸盐和溴酸盐的同时测定。     

超高效液相色谱-串联质谱法测定生活饮用水中氯酸盐和高氯酸盐

目的 建立超高效液相色谱-串联质谱（UPLC-MS/MS）法同时测定生活饮用水中的氯酸盐和高氯酸盐的含量。方法 采用Anionic Polar Pesticide色谱柱（2.1 mm×150 mm,5 μm）为分析柱对高氯酸盐、氯酸盐进行分离,选用50 mmol/L甲酸铵甲酸水溶液（含0.9%甲酸）和乙腈作为流动相进行梯度洗脱。在电喷雾离子源,负离子多反应监测模式下测定,通过内标法进行定量。结果 氯酸盐和高氯酸盐在0.5～80 μg/L范围内线性关系良好,相关系数R2不低于0.999,氯酸盐和高氯酸盐的检出限、定量限均分别为0.5 μg/L和1.0 μg/L。氯酸盐和高氯酸盐均在1.0、2.0、20.0、80 μg/L 4个水平下回收率为83.98%～106.80%,相对标准偏差为0.57%～3.50% (n=6);结论 该方法简便、快捷、准确,适用于快速检测生活饮用水中的氯酸盐和高氯酸盐。     

固相萃取-高效液相色谱-串联质谱法测定蜂蜜中高氯酸盐

目的建立一种固相萃取-高效液相色谱-串联质谱法测定蜂蜜中高氯酸盐的含量。方法样品用酸化甲醇水提取, WAX固相萃取柱净化,经Phenyl-hexyl色谱柱分离,以电喷雾离子源在负离子多反应监测模式下进行测定,内标法定量。结果高氯酸盐的检出限和定量限分别为0.33μg/kg和1μg/kg,高氯酸盐在1～10μg/kg的加标水平内的回收率为91.6%～108.3%,相对标准偏差为2.81%～3.47%。结论该方法准确、灵敏,适用于蜂蜜中高氯酸盐的测定。     

液相色谱-串联质谱法测定饮用水中的卤氧化物

目的建立一种液相色谱-串联质谱(liquid chromatography-tandem mass spectrometry,LC-MS/MS)同时检测饮用水中3种卤氧化物(高氯酸盐、氯酸盐及溴酸盐)的分析方法。方法水样直接经0.22μm水系滤膜过滤,采用100 mmol/L乙酸铵(A)和乙腈(B)作为流动相进行等度洗脱,经IC-Pak~(TM) Anion HR色谱柱分离,质谱(ESI-)采用多离子检测模式(MRM)对3种卤氧化物的定量离子和定性离子进行监测。结果本方法在6min内即完成3种目标化合物的分离分析。高氯酸盐及溴酸盐在0.5~50μg/L浓度范围内线性良好、氯酸盐在0.5~100μg/L浓度范围内线性良好(r≥0.999)。添加浓度为0.5、10.0、50.0μg/L,实验结果表明高氯酸盐、氯酸盐及溴酸盐的回收率可达84.8%~101.4%,相对标准偏差均小于10.0%(n=6)。高氯酸盐、氯酸盐及溴酸的检出限分别为0.1、0.2、0.2μg/L。结论该方法快速、准确、灵敏,适合测定饮用水中高氯酸盐、氯酸盐及溴酸盐的同时测定。     

固相萃取-超高效液相色谱-串联质谱法测定土壤中的高氯酸盐

目的建立了一种同位素稀释超高液相色谱-串联质谱法测定土壤中高氯酸盐含量的分析方法。方法试样经0.2%乙酸水溶液和二氯甲烷提取,上清液经HLB小柱净化,液相色谱-串联质谱法测定,内标法定量。结果高氯酸盐在0.1～100μg/L浓度范围内线性关系良好,相关系数为0.9995,检出限为0.3μg/kg,定量限为1.0μg/kg,加标回收率在85.2%～102%,相对标准偏差(relative standard deviation, RSD)小于8.0%。结论该方法简便、可靠、稳定,可用于土壤中高氯酸盐含量的测定。     

离子色谱法同时测定饮用水中的溴酸盐和高氯酸盐

建立离子色谱同时测定饮用水中溴酸盐和高氯酸盐的方法。通过加热浓缩对水样中的Br O3-和Cl O4-进行富集,选用亲水性AS19分析柱作为分离柱、氢氧化钾溶液为淋洗液,优化离子色谱测试条件后,采用电导检测器测定水中溴酸盐和高氯酸盐的含量。结果表明,当进样体积为100μL时, Br O3-和Cl O4-浓度分别在5～125μg/L、0.02～1.25 mg/L范围内与其对应的峰面积呈线性关系,线性回归方程分别为y=0.000 21C-0.000 23、y=0.302 98C-0.005 27,相关系数分别为0.999 8和0.999 9,方法检出限分别为0.50μg/L和5.2μg/L。对每份样品进行3个水平的加标回收试验,加标回收率均在90.33%～103.79%之间,测定结果的相对标准偏差在0.34%～4.46%之间,并与液相色谱-质谱/质谱法的测定结果进行比较,结果无显著性差异。方法具有准确度高、选择性好和操作简单等优点,可应用于多种饮用水中溴酸盐和高氯酸盐含量的同时测定。     

离子色谱串联质谱法测定婴幼儿配方奶粉中氯酸盐和高氯酸盐

目的建立离子色谱串联质谱法(ion chromatography tandem mass spectrometry, IC-MS/MS)检测婴幼儿配方奶粉中氯酸盐和高氯酸盐的分析方法。方法样品经提取、净化除去蛋白质及脂类物质后,采用离子色谱法分离,电喷雾串联质谱法测定,并采用氯酸盐-~(18)O_3和高氯酸盐-~(18)O_4作为同位素内标物质进行定量。结果在10min内完成了氯酸盐和高氯酸盐的分离分析。氯酸盐和高氯酸盐在低中高3个添加水平的回收率为79.7%～96.4%,相对标准偏差小于5%(n=6),氯酸盐检出限为1.0μg/kg,高氯酸盐检出限为0.3μg/kg。结论该方法准确、可靠,可同时检测婴幼儿配方奶粉中氯酸盐和高氯酸盐的含量。     

高效液相色谱-串联质谱法测定肉类中的氯酸盐和高氯酸盐

建立了高效液相色谱-串联质谱法同时测定肉类中氯酸盐和高氯酸盐的分析方法。样品经乙腈-水（13:7,V:V）提取后离心,上清液经PRiME HLB固相萃取柱净化,Acclaim Trinity P1复合离子交换柱分离,以乙腈及20 mmol/L乙酸铵为流动相进行梯度洗脱,串联质谱分析中采用电喷雾正离子源和多反应监测模式,内标法定量。结果表明,氯酸盐和高氯酸盐分别在2～200.0 ng/mL、1～100.0 ng/mL范围内呈现良好线性关系,决定系数分别为0.9983和0.9998,方法的定量限分别为2.0、1.0μg/kg。氯酸盐和高氯酸盐分别在三种肉类四个添加水平6.0、20、40、200μg/kg和3.0、10、20、100μg/kg的加标回收率为91.0%～105.7%和94.2%～110.5%,相对标准偏差为1.8%～9.7%和0.7%～9.4%。本方法具有操作简单、灵敏度高、稳定性好等优点,可很好地满足肉中氯酸盐、高氯酸盐的检测。     

内蒙古地区婴幼儿配方乳粉中高氯酸盐与氯酸盐膳食暴露风险评估

目的 了解内蒙古地区婴幼儿配方乳粉中高氯酸盐和氯酸盐的污染水平，评估婴幼儿高氯酸盐和氯酸盐的膳食摄入风险，为指导内蒙古地区婴幼儿健康膳食提供科学依据。方法 采集内蒙古地区市售各段位的婴幼儿配方乳粉539份，乳粉冲调用水（冲调乳粉时可能使用的饮用水）254份，采用超高效液相色谱-串联质谱（UPLC-MS/MS）法对婴幼儿配方乳粉、乳粉冲调用水中的高氯酸盐和氯酸盐含量进行检测。以2015年中国婴幼儿食品消费量调查数据中内蒙古地区婴幼儿的消费量数据为依据，采用简单分布评估和累积暴露评估方法计算内蒙古地区婴幼儿配方乳粉中高氯酸盐和氯酸盐的膳食摄入风险。结果 婴幼儿配方乳粉中高氯酸盐的总体检出率为92.39%(498/539)，检测值在未检出～89.30μg/kg，平均值为14.45μg/kg，中位数为9.00μg/kg；氯酸盐的总体检出率为73.10%(394/539)，检测值在未检出～1 061.00μg/kg，平均值为93.25μg/kg，中位数为45.50μg/kg。乳粉冲调用水中高氯酸盐的总体检出率为67.32%(171/254)，检测值在未检出～26.59μg/L，平均值为1.25μ...     

UPLC-MS/MS测定特殊医学用途配方乳粉中氯酸盐和高氯酸盐

建立一种特殊医学用途配方乳粉中氯酸盐和高氯酸盐测定的超高效液相色谱-串联质谱法。样品用0.1%（体积比）甲酸水-乙腈提取，经Oasis PRiME HLB固相萃取柱净化，复合离子交换色谱柱分离后，以乙腈-20 mmol/L甲酸铵溶液为流动相进行梯度洗脱，多反应模式检测，同位素内标法定量。结果显示，氯酸盐和高氯酸盐在1～200 ng/mL质量浓度范围内呈良好的线性关系，相关系数大于0.999，检出限为3.75μg/kg，定量限为7.5μg/kg。氯酸盐和高氯酸盐在7.5、50、500、1 500μg/kg 4个加标水平回收率为97.1%～104.8%之间，相对标准偏差为2.55%～6.05%(n=6)。该方法简单快速、定量准确，能用于特殊医学配方乳粉中氯酸盐和高氯酸盐含量的测定。     

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.     

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.     

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.     

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.     

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.     

Analysis on Economic Indicators from 62 Enterprises in Printing Machinery Industry in Q1 2014

Operation of printing machine industry was still unsatisfactory in the first quarter of 2014.Analysis on operation of printing machine industry.a.Market demand was not strong;sales of product undulated and declined.According to the statistics,the total industrial output value fell by 19.28% in the first quarter of 2014 than the average quarter value in 2013; industrial added value decreased by 4.16%; sales revenue dropped by 22.83%. h. Business operation of enterprises was in poor condition. c. R＆D of new products is an important transformation guarantee for enterprises. d. To take self explore new ways upgrading advantages,and explore new ways.