QuEChERS-UPLC-MS/MS同时测定鸡肉中80种兽药残留

目的:建立一种同时测定鸡肉中包括喹诺酮类、磺胺类、β-受体激动剂类、糖皮质激素类、大环内酯类、抗病毒类药物、四环素类等在内的80种兽药的QuEChERS-超高效液相色谱—串联质谱法(UPLC-MS/MS)分析方法。方法:样品经1%甲酸乙腈水溶液提取,QuEChERS多兽药残留净化柱净化,超高效液相色谱—串联质谱(UPLC-MS/MS)多反应监测模式检测,基质标准曲线外标法定量。结果:80种兽药在特定质谱条件下响应性高,样品在质谱检测条件下检测灵敏,无杂峰干扰。80种药物质量浓度在5.0～100μg/L的范围内,线性关系良好,相关系数均大于0.99。80种兽药的方法检出限均为1.0μg/kg。样品中2.0,5.0,10.0μg/kg加标浓度的平均回收率为62.2%～106.8%,相对标准偏差为2.07%～10.85%。结论:80种药物在样品中加标回收率均符合GB/T 27404—2008《实验室质量控制规范食品理化检测》标准要求,适用于鸡肉中80种兽药残留的筛查测定。     

QuEChERS-超高效液相色谱-串联质谱法同时测定淡水鱼和淡水虾中的11种喹诺酮类兽药残留量

目的 优化并建立 UPLC-MS /MS 法测定淡水鱼和淡水虾中 11 种喹诺酮类兽药残留的检测方法。方法 样品中的喹诺酮残留经酸化乙腈提取, C18基质分散固相萃取净化,超高效液相色谱－串联质谱测定其中11种喹诺酮类兽药残留量。结果 恶喹酸在1～50.0μg/L,其余10种喹诺酮类化合物在1～100.0μg/L范围内线性关系良好,11种喹诺酮药物的检出限为0.0005mg/kg～0.0010mg/kg,定量限为0.0015mg/kg ～0.0030mg/kg,精密度＜ 12 % ,低、中、高三个浓度加标回收率为 70.0%～120.1% 。结论：该方法样品前处理简单、重现性好、灵敏度高、能满足限量标准的要求,可用于淡水鱼和淡水虾样品 中喹诺酮类药物残留的分析检测。     

QuEChERS法-液相色谱-串联质谱法测定蔬菜中7种农药及其代谢物的残留量

样品经乙腈提取,C_(18)吸附剂和石墨化碳黑分散固相萃取净化,液相色谱-三重四极杆串联质谱在动态多反应监测模式下检测,基质匹配标准曲线外标法进行定量,建立了蔬菜中7种农药及其代谢物的多残留分析方法。在10、20μg/kg 7种农药及其添加物添加水平下,农药及其代谢物的平均回收率为71.9%~117.8%,相对标准偏差为0.8%~9.6%,定量限为0.2~10μg/kg。该方法简便、快速、灵敏,适用于蔬菜中多种农药及其代谢物的同时检测。     

不同前处理方法对猪组织中喹诺酮类兽药残留检测效果对比

采用超高效液相色谱-三重四极杆质谱和飞行时间质谱技术,比较EMR-L、Oasis PRiME HLB和液液萃取法对猪组织中16?种喹诺酮类兽药残留检测效果的影响。目标兽药以基质匹配工作曲线进行定量,在1.0～100.0?μg/L范围内线性关系良好,在5、10、20?μg/kg加标量条件下使用超高效液相色谱-串联质谱检测,EMR-L和Oasis?PRiME?HLB方法处理的猪组织中加标回收率（71.7%～106.9%、70.7%～118.3%）、相对标准偏差（0.2%～16.8%、0.1%～17.8%）、定量限（0.13～0.56、0.27～1.36?μg/kg）和检出限（0.04～0.23、0.08～0.41?μg/kg）均满足方法学要求。针对不同基质成分样品,采用不同的前处理技术减少假阳性结果的产生,以适用于日益增长的动物源性食品兽药残留检测的需求。本研究采用的2?种方法操作简便、灵敏度高、重复性好,满足对猪组织中多兽药残留的定性、定量分析。     

液相色谱-串联质谱法检测速冻调制肉制品中糖皮质激素类药物残留

建立液相色谱-串联质谱法检测速冻调制肉制品中糖皮质激素类药物残留的方法。样品经乙酸乙酯提取后,过Silica固相萃取柱净化,最后用乙腈定容,经液相色谱-串联质谱仪测定。样品采用外标峰面积法进行定量,该方法的最小检出限量分别为0.2、0.5、1.0μg/kg,定量限分别为0.5、1.0、2.0μg/kg,添加回收率范围为85.0%～96.4%,RSD为2.3%～6.1%。     

QuEChERS-高效液相色谱-串联质谱法测定稻田水产品中氟虫腈及其代谢物残留

以QuEChERS作为样品前处理方法,结合高效液相色谱-串联质谱技术建立检测稻田水产品中氟虫腈及其代谢物氟甲腈、氟虫腈砜、氟虫腈亚砜残留的方法。样品通过体积分数为0.10%甲酸-乙腈溶液及陶瓷均质子旋涡振荡法提取,由0.15 g乙二胺?N?丙基硅烷分散萃取净化后采用ZORBAX Extend-C18色谱柱（2.1 mm×100.0 mm,1.8 μm）进行分离,电喷雾负离子模式测定,基质匹配标准曲线后运用外标法定量。结果表明,稻田水产品中氟虫腈、氟甲腈、氟虫腈砜和氟虫腈亚砜的平均回收率在85.2%～112.6%之间,相对标准偏差在1.2%～12.4%之间,氟虫腈及其代谢物在质量浓度0.5～100.0 ng/mL之间线性良好,相关系数均大于0.999,检出限为1.0～1.5 μg/kg、定量限为3.0～5.0 μg/kg,二者均低于GB 2763—2019《食品中农药最大残留限量》对禽肉中氟虫腈最大残留限量10 μg/kg的规定,实验方法简单、快速、灵敏,能够满足稻田水产品中氟虫腈及其代谢物的检测需求。     

超高效液相色谱-串联质谱法检测卤肉中36种兽药残留

建立了卤肉中金刚烷胺、磺胺类、喹诺酮类及氯霉素类等36种兽药残留的检测方法。卤肉样品通过乙腈-水溶液(V:V=8:2)提取,PRiME HLB固相萃取柱净化,配有电喷雾离子源(ESI±)的超高效液相色谱-串联质谱(UPLC-MS/MS),在正负离子多反应监测(MRM)模式下同时测定,基质匹配标准曲线定量。结果表明,所研究的36种兽药在0.5～20.0 ng/mL浓度范围内均呈良好线性关系(R²>0.999)。本方法中36种药物的检出限均为0.10μg/kg,定量限均为0.33μg/kg,在高中低3个不同浓度(0.5,1.0和5.0μg/kg)36种兽药的添加回收率为70.8%～106.9%,相对标准偏差(RSD, n=6)0.2%～6.2%。该研究建立的方法操作简单、准确性高、回收率和重现性好,可同时对卤肉中的36种兽药残留进行测定。     

QuPPe-超高效液相色谱-串联质谱法测定蔬菜中呋虫胺及其代谢物残留

建立超高效液相色谱-串联质谱检测蔬菜中呋虫胺及其代谢物1-甲基-3-[（3-四氢呋喃）甲基]二氢胍盐（1-methyl-3-(tetrahydro-3-furylmethyl) guanidium?dihydrogen,DN）、1-甲基-3-[（3-四氢呋喃）甲基]脲（1-methyl-3-(tetrahydro-3-furylmethyl) urea,UF）残留的方法。蔬菜样品采用QuPPe分析方法处理后,经BEH-C18超高效液相色谱柱分离,采用电喷雾正离子模式,通过多反应监测方式测定,基质匹配标准曲线外标法定量。结果表明,呋虫胺及其代谢物在1.25～500?μg/L的质量浓度范围内线性关系良好,相关系数均大于0.991,方法检出限为0.04～0.66?μg/L,定量限为0.13～2.20?μg/L。在3?个添加水平条件下,呋虫胺及其代谢物DN、UF在黄瓜、番茄、马铃薯、甘蓝4?种基质中的添加回收率为72.0%～109.1%,相对标准偏差为1.4%～12.8%,最低添加量均为10?μg/kg。基质效应结果显示,呋虫胺及其代谢物大都表现为中等强度基质效应或强基质效应。该方法简单、准确、高效,可用于蔬菜样品中呋虫胺及其代谢物农药残留的快速筛查和定量检测。     

QuEChERS-气相色谱串联质谱法同时测定番茄中46种农药残留

建立一种QuEChERS结合气相色谱-串联质谱同时检测番茄中46种杀菌剂和杀虫剂残留的分析方法。样品用乙腈提取,经PSA、C₁₈、无水MgSO₄净化,HP-5MS色谱柱分离,采用多反映监测（MRM）模式检测,基质匹配外标法定量。结果表明,46种农药在0.005～0.500 μg/mL的浓度范围内线性关系良好（R2>0.999）,方法检出限和定量限分别在0.07～2.63 μg/kg和0.21～8.39 μg/kg之间;在0.0025、0.025、0.25 mg/kg的加标水平下,46种农药化合物平均加标回收率在70.40%～115.08%范围内,相对标准偏差为0.22%～4.89%。50批次番茄样品中9批次检出毒死蜱和嘧菌酯残留,含量范围在0.0043～0.0365 mg/kg,均未超出GB 2763-2021标准规定的限量值。本方法快速、简单、灵敏、准确,能够满足番茄中多农药残留的检测。     

超高效液相色谱-串联质谱法检测熟肉制品中10种工业染料残留

目的建立超高效液相色谱—串联质谱法(ultraperformanceliquidchromatography-tandemmass spectrometry, UPLC-MS/MS)测定熟肉制品中10种工业染料的检测方法。方法熟肉制品样品均质后经乙腈、乙腈水溶液(1:1,V:V)分别提取后,采用冷冻离心处理去除提取液中油脂及天然大分子色素。采用ACQUITY UPLC BEH C18色谱柱分离后,用UPLC-MS/MS于电喷雾正离子源和多反应监测扫描模式下测定10种工业染料,基质匹配标准曲线结合稳定同位素内标法定量。结果 10种目标化合物阴性加标水平在2、5、10μg/kg下,回收率为68.5%～91.3%,相对标准偏差为2.4%～12.8%。10种目标化合物的检出限为0.05～0.7μg/kg,定量限为0.15～2.0μg/kg。用该方法对30件熟牛肉、熟猪肝、烤肠、香肠等样品进行了目标化合物的检测,未检测到工业染料残留。结论该方法操作简便、快速,灵敏度和准确度高,包含种类较宽,具有一定的拓展性,可为熟肉制品中工业染料残留的日常监控提供更方便、快捷的检测方法支持。     

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.     

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.     

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.     

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.