UPLC-MS/MS与HPLC测定茶叶中10种氨基甲酸酯类农药残留的比较

比较了超高效液相色谱-串联质谱(UPLC-MS/MS)与高效液相色谱(HPLC)法测定茶叶中10种氨基甲酸酯类农药残留的分析方法。样品经乙腈提取,氨基固相萃取柱净化,HPLC和UPLC-MS/MS测定。结果表明,在相同的前处理条件下,两种方法均具有较好的准确度和精密度,UPLC-MS/MS法在0.01~0.1mg/kg添加水平下回收率为75.2%~115.6%,相对标准偏差(RSD)为4.4%~16.7%。HPLC法在0.05~1.0mg/kg添加水平下回收率为82.7%~120.7%,相对标准偏差(RSD)为0.8%~12.9%。UPLC-MS/MS法相对于HPLC法有更高的灵敏度,10种氨基甲酸酯类农药在UPLC-MS/MS上检出限为0.02~0.3μg/kg,HPLC法检出限为3~7.5μg/kg;其高灵敏度和选择性,使其更适于多农药残留同时检测和微量残留检测。     

超高效液相色谱-串联质谱多组分检测牛奶中外源性激素残留

在多反应监测模式条件下采用正离子采集模式建立牛奶中7 种激素的超高效液相色谱- 质谱/ 质谱(UPLCMS/MS)检测方法。样品以甲醇溶液为提取剂超声辅助提取,经LC-C18 柱净化,经BEH-C18(100mm × 2.1mm,1.7μm)柱分离后进行UPLC-MS/MS 多反应监测模式下的定性及定量分析。7 种激素方法检出限为0.01～0.25μg/kg,定量限为0.06～0.5μg/kg,添加水平为10μg/kg 时,平均回收率为83%～124%,相对标准偏差为4.3%～24%。该法灵敏度高、检出限低、分析时间短、操作简便,可应用于实际样品检测。     

超高效液相色谱-串联质谱法检测猪肉中多兽药残留

建立一种超高效液相色谱-串联质谱(ultra performance liquid chromatography/tandem mass spectrometry,UPLC-MS/MS)法同时检测猪肉中β-受体激动剂类、磺胺类、砜类抑制剂类、喹诺酮类、糖皮质激素类以及大环内酯类等20种兽药残留。待测药物使用80%体积分数的乙腈水溶液提取,经固相萃取小柱净化和氮气吹干后使用体积分数10%甲醇水进行复溶,复溶液经微孔滤膜过滤后进行UPLC-MS/MS测定。使用BEH C_(18)色谱柱梯度洗脱分离,选用电喷雾电离源,正离子扫描及多反应监测模式测定。20种药物检出限(limit of detection,LOD)在0.5～5μg/kg之间,定量限(limit of quantitation,LOQ)在1.7～16.7μg/kg之间,当加标水平为1、5、10μg/kg时,平均回收率在62.1%～118.3%范围内,相对标准偏差(relative standard deviation,RSD)在0.4%～16.7%范围内。     

UPLC-MS/MS法和HPLC法测定苹果中氨基甲酸酯类农药的对比

目的:基于检出限、精密度、准确度、加标回收率等指标,考查超高效液相色谱-串联质谱法(UPLC-MS/MS)和高效液相色谱法(HPLC)测定苹果中氨基甲酸酯类农药的一致性及适用性。方法:分别采用UPLC-MS/MS法和HPLC法测定苹果中的氨基甲酸酯类农药。UPLC-MS/MS法:苹果样品中的氨基甲酸酯类农药经乙腈提取,QuEChERS净化后,UPLC-MS/MS进行分离并定量分析;HPLC法:苹果样品中的氨基甲酸酯类农药经乙腈超声提取后,CARB/NH_2固相萃取柱净化,高效液相色谱-柱后衍生法进行分离并定量分析。结果:HPLC法加标回收率在79%～83%,日内精密度(RSD%)为1.9%～5.3%,方法检出限为2.0～5.0 μg/kg;UPLC-MS/MS法加标回收率在83.2%～103.1%,日内精密度(RSD%)为0.9%～3.1%,方法检出限为0.5～1.5 μg/kg。结论:相较于HPLC法,UPLC-MS/MS 法保留时间更短、检出限更低,且操作简便、重现性好,可作为苹果中氨基甲酸酯类农药残留检测的推荐方法。     

超高效液相色谱-串联质谱法测定畜禽肉中17种磺胺类药物残留

目的建立超高效液相色谱-串联质谱(ultra performance liquid chromatography-tandem mass spectrometry,UPLC-MS/MS)测定畜禽肉组织中17种磺胺类药物残留的方法。方法样品经乙腈提取、浓缩,正己烷脱脂后在正离子模式下以电喷雾电离串联质谱进行测定,外标法定量。结果 17种磺胺类药物在5μg/L~100μg/L范围内线性良好,相关系数0.99,方法检出限为2μg/kg,定量限为5μg/kg。在10、20、100μg/kg的添加水平下,17种磺胺类药物的平均回收率在84.0%~114.2%之间,相对标准偏差(relative standard deviation,RSD,n=6)在0.59%~7.96%之间。结论本方法快速、准确、灵敏,可应用于畜禽肉中17种磺胺类药物残留的同时检测。     

UPLC-MS/MS测定蔬菜中氨基甲酸酯类农药

建立超高效液相色谱-串联质谱(UPLC-MS/MS)测定蔬菜中氨基甲酸酯类农药的方法。用乙腈提取蔬菜中的氨基甲酸酯类农药,经QuEChERS净化后UPLC-MS/MS定量分析。实验浓度范围内线性关系良好,方法加标回收率在82.2%~104.1%,精密度(RSD)为1.9%~4.0%,检出限为0.2~1.5μg/kg。UPLC-MS/MS法测定蔬菜中氨基甲酸酯类农药有较好的回收率、重现性和较低的检出限,能满足大批量样品氨基甲酸酯类农药的快速检测需求。     

酸奶中违禁性激素多残留同时测定方法

在多反应监测模式下采用正离子采集模式建立了酸奶中7种激素的超高效液相色谱一质谱/质谱(UPLC-MS/MS)检测方法.样品以甲醇为提取剂超声提取,经LC-C18净化,经BEH-C18(1.7 μm,2.1mm×100mm)柱分离后进行UPLC/MS/MS多反应监测模式下的定性及定量分析.7种激素方法检出限为0.011～0.05 μg/kg,定量限为0.037～0.36 μg/kg,添加水平为0.5 μg/kg时,平均回收率为72%～124%,相对标准偏差为8.0%～24%.     

高效液相色谱一串联质谱法测定鱼肉中8种喹诺酮类药物的残留量

目的建立鱼肉中恩诺沙星、丹诺沙星、环丙沙星、诺氟沙星、培氟沙星、沙拉沙星、双氟沙星、氧氟沙星等8种喹诺酮类药物残留量的高效液相色谱-串联质谱检测方法。方法以氘代试剂为内标,样品经酸性乙腈提取后,用正己烷脱脂,旋转蒸发浓缩,采用LC-MS/MS多反应监测(MRM)正离子模式测定。结果 8种喹诺酮的水平为1.0μg/kg和3.0μg/kg时回收率为88.4%～114.9%,检出限(S/N=3)为0.03～0.1μg/kg。结论该方法简便快捷,精密度好,准确度高,可满足鱼肉中多种喹诺酮类药物残留的定性、定量检测要求。     

免疫亲和净化-超高效液相色谱串联质谱法同时测定猪肉和鸡蛋中的12种磺胺类药物

建立了猪肉和鸡蛋中12种磺胺类药物的免疫亲和净化-超高效液相色谱串联质谱的确证方法。样品用超声提取后,直接过磺胺类药物免疫亲和净化柱净化;氮气吹干后用1∶9（v/v）的甲醇/水溶液定容,超高效液相色谱-串联质谱（UPLC-MS/MS）测定,电喷雾正离子（ESI＋）、多反应模式下监测;实验结果表明,样品中磺胺类药物浓度在10～200μg/kg范围内时与其峰面积成良好线性关系,仪器检出限为0.4～2.0μg/L,方法的检出限为1.0～5.0μg/kg,3个加标水平下平均回收率为67%～100%,相对标准偏差为0.9%～10.0%,符合痕量分析的要求。     

超高效液相色谱-串联质谱法测定果蔬中4种乙撑二硫代氨基甲酸酯农药残留

目的 建立超高效液相色谱-串联质谱法(UPLC-MS/MS)测定蔬菜、水果中4种乙撑二硫代氨基甲酸酯类农药残留量的方法。方法 试样采用L-半胱氨酸盐酸盐和碱性EDTA-Na₂溶液进行提取，碘甲烷衍生，QuEChERS原理净化浓缩，UPLC-MS/MS对乙撑二硫代氨基甲酸酯类农药衍生物进行测定，外标法定量。结果 水果的检出限为5μg/kg，蔬菜的检出限为10μg/kg，相关系数大于0.998，添加回收率的范围为82.3%～115.1%，相对标准偏差为2.3%～6.9%。结论 本文所建立的方法能够满足多种水果和蔬菜中乙撑二硫代氨基甲酸酯类农药快速准确检测。     

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.