高效液相色谱法检测葡萄酒中柠檬酸

目的建立高效液相色谱法(high performance liquid chromatography,HPLC)测定葡萄酒中柠檬酸的含量的分析方法。方法以0.02 mol/L甲醇和磷酸二氢钾(5:95,V:V)为流动相,流速为0.7 m L/min,在此色谱条件下,采用二级管阵列检测器进行检测。结果在0.05~1.00 g/L范围内,浓度与峰面积的线性关系良好,相关系数为0.9999。在加标浓度为5.0、20.0、50.0 g/L时的回收率为93.9%~106.3%,相对标准偏差(relative standard deviation,RSD)为1.67%~2.99%之间。结论该方法具有较高的灵敏度和准确性,且操作简单,适用于检测葡萄酒样品中的柠檬酸。     

柱前衍生-高效液相色谱-二极管阵列法测定葡萄酒中组胺含量

目的建立柱前衍生-高效液相色谱-二极管阵列法(high performance liquid chromatography-diode arraydetector,HPLC-DAD)测定葡萄酒中组胺含量的方法。方法将葡萄酒样品与10mg/mL的丹磺酰氯在70℃柱前衍生10min,衍生样品以乙腈和0.01mol/L乙酸铵溶液(含0.1%乙酸)为流动相进行等度洗脱,于波长254 nm处进行检测。结果该方法的标准曲线回归方程为Y=0.0319X+0.00059, 0.1～100μg/mL的线性范围内,组胺标准品峰面积与内标物峰面积的比值与组胺含量线性关系良好,相关系数r2为0.9987,回收率为92.3%～105.2%,检出限为0.05μg/mL。结论该方法操作简便、准确度高,适用于葡萄酒中组胺含量测定。     

液相色谱-串联质谱法测定畜禽肌肉和表皮组织中松香酸、脱氢松香酸和胡椒酸

目的 建立了畜禽肌肉和表皮组织中松香酸、脱氢松香酸和胡椒酸的液相色谱-四极杆/串联质谱(LC-MS/MS)的检测方法。方法 均质样品中加入乙腈和水分别提取目标物,经涡旋分散、震荡提取、离心和固相萃取柱净化。提取液以乙酸铵-甲醇为流动相梯度洗脱C18色谱柱分离,5 mmol的乙酸铵和甲醇为流动相进行梯度洗脱,三重四级杆质谱ESI+/ESI-切换模式检测,以特征离子峰和保留时间定性,定量离子峰面积定量。结果 松香酸、脱氢松香酸的测定低限为5.0 μg/kg、胡椒酸20.0 μg/kg,线性范围分别为5.0~200.0 μg/kg和20.0~500.0 μg/kg,相关系数(r)在0.999以上。分别添加定量限1、2、4倍的浓度验证加标回收率,三个浓度水平的回收率为68.5% ~ 107.6%,相对标准偏差(RSD)为6.8%~14.2%(n=6)。结论 该方法快速、准确、灵敏,适用于监管部门对市售畜禽食品中工业松香残留的检测。     

超高压液相色谱-质谱法测定水果中添加的3种人工合成甜味剂

目的 建立水果中3 种人工合成甜味剂(甜蜜素、糖精钠、安赛蜜)的超高压液相色谱-串联质谱 (UPLC-MS/MS)检测方法。方法 以反相C18 柱为色谱柱, 乙腈?0.02 mol/L 乙酸铵溶液为流动相, 样品经纯水 提取后用色谱柱进行分离, 串联质谱负离子多反应监测(MRM)模式测定。结果 3 种人工合成甜味剂在10~600 μg/L 范围内响应峰面积和样品质量浓度之间有良好的线性关系(相关系数r≥0.995); 甜蜜素、糖精钠和安赛蜜 的最低检出限分别为0.8、5.0、1.0 μg/kg; 在2 种添加水平下, 样品平均回收率为74.9%~111.2%, 相对标准偏 差<8%。结论 该方法前处理简单, 分析时间短, 具有良好的灵敏度和准确性, 可用于水果中甜蜜素、糖精钠、 安赛蜜的同时检测。     

QuEChERS结合液相色谱-串联质谱法测定食用菌中13种农药残留

目的:建立并应用QuEChERS结合液相色谱-串联质谱法测定食用菌中13种农药残留。方法:样品5.0 g用乙腈-水(4:1)15 mL超声提取,经N-丙基乙二胺(PSA)30.0 mg和无水硫酸镁15.0 mg分散固相萃取吸附剂净化。使用HSS T3色谱柱,0.1%甲酸和乙腈为流动相梯度洗脱。质谱采用电喷雾正离子源和多反应监测模式。结果:13种农药的质量浓度在0.5~200 μg/L范围内与峰面积呈良好的线性关系,检出限(S/N=3)0.03~0.3 μg/kg。加标回收率84.3%~102%,相对标准偏差(n=6)2.8%~6.3%。结论:该方法可用于食用菌中13种农药残留的检测。     

液相色谱-质谱联用技术测定葡萄酒中的赭曲霉毒素A残留

建立葡萄酒中赭曲霉毒素A的高效液相色谱-串联四极杆质谱联用测定方法,该方法经HLB固相萃取柱净化样品,以ZORBAX Eclipse XDB-C18柱(3.0×50 mm,1.8μm)分离,流动相为0.1%甲酸水溶液和甲醇(梯度洗脱),电喷雾正离子MRM模式检测.该方法的检出限0.20 μg/L,方法定量下限0.20 μg/L,线性范围0.20 μg/L～100 μg/L,加标回收率86.6%～91.0%,相对标准偏差为1.67%.     

液相色谱-串联质谱法测定水体中8种典型喹诺酮类抗生素

目的 建立一种检测8种喹诺酮类抗生素的液相色谱-串联质谱法并评价其在水体环境中的应用。方法 采用C18色谱柱(10 mm×2.1 mm,1.7 μm)为分离柱,以甲醇～0.1%甲酸水溶液为流动相,设定柱温为35 ℃、流速为0.35 mL/min;质谱条件采用电喷雾离子源 (Electron Spray Ionization, ESI) 正离子模式(ESI+)及多反应监测(multiple reaction monitoring, MRM)模式采集。结果 在0.1~100.0 μg/L浓度范围内,马波沙星、氧氟沙星、洛美沙星、达氟沙星、恩诺沙星、沙拉沙星6种抗生素的质量浓度与峰面积线性关系良好(r2>0.99), 检出限为0.1 μg/L; 在5.0~500.0 μg/L浓度范围内,培氟沙星、诺氟沙星的质量浓度与峰面积线性关系良好(r2>0.99),检出限为5.0 μg/L。8种喹诺酮在环境水样品中的平均回收率为98.30%~111.77%,相对标准偏差为0.71%~12.80%。结论 该方法简单、灵敏、准确,可以满足水体环境中喹诺酮类抗生素检测。     

高压液相色谱-线性离子阱串联质谱法测定红葡萄酒中多菌灵和甲基硫菌灵

目的 建立红葡萄酒中多菌灵和甲基硫菌灵残留的高压液相色谱-串联线性离子阱质谱(HPLC-LIT-MS/MS)检测方法。方法 样品经过乙腈提取, 在梯度洗脱程序下经CAPCELL PAK CR 1:20色谱柱分离后, 采用HPLC-LIT-MS/MS, 在二级质谱选择反应监测(SRM)模式进行测定。结果 红葡萄酒中多菌灵和甲基硫菌灵添加水平为10、20、50 μg/L时, 平均回收率分别为82.5%~103.1%和93.7%~115.2%。检出限(LODs)分别为0.063 μg/L和0.019 μg/L, 定量限(LOQs)分别为0.125 μg/L和0.075 μg/L。结论 该方法快速简便, 灵敏度高, 准确度和精密度均满足痕量分析要求。     

高效液相色谱/质谱联用直接测定鱼油中EPA/DHA含量

建立快速、简单、准确测定鱼油样品中EPA和DHA两种ω-3 PUFA含量的高效液相色谱/电喷雾质谱联用(HPLC ESI/MS)分析方法.鱼油经2 mol/L NaOH乙醇溶液皂化、3 mol/L HCL酸化后,使用Waters液相色谱仪、SymmetryC8柱(2.1×150mm),以甲醇一水为流动相、十七酸为内标,利用质谱定性定量测定EPA/DHA含量.质谱在电喷雾负离子模式下,对m/z 301、m/z 327和m/z269进行选择离子监测.该方法下EPA、DHA分别在5.55～55.50μg/mL和0.90～9.00μg/mL范围内峰面积和浓度呈良好的线性关系,相关系数REPA=0.999 5、RDHA=0.999 3;EPA、DHA的回收率分别为98.63%～99.23%、97.12%～99.17%.EPA、DHA的相对标准偏差分别为1.57%、1.20%(n=5).此方法流动相简单,分析时间短且无需衍生处理,不受色谱分离度的限制并可实现对样品的重复分析,能准确快速测定鱼油中EPA和DHA含量.     

二维高效液相色谱法测定葡萄酒中柠檬酸含量

目的建立二维高效液相色谱测定葡萄酒中柠檬酸的分析方法。方法样品经稀释后,13000 r/min高速离心10 min,以pH 1.6 20 mmol/L磷酸二氢钾缓冲溶液/甲醇为流动相,经一维C_8色谱柱预分离,将目标物通过流通阀切换至二维C_(18)分析柱。结果在优选条件下,方法线性范围为15~200 mg/L,线性相关系数r~2不低于0.9999,检出限(S/N=3)为4.7 mg/L,样品回收率为98.84%~102.40%,测定结果的相对标准偏差(RSD)为0.095%~0.94%。结论该方法操作简便,能准确快速测定葡萄酒中柠檬酸含量。     

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.     

An internet compendium of analytical methods and spectroscopic information for monomers and additives used in food packaging plastics

An internet website (http://cpf.jrc.it/smt/) has been produced as a means of dissemination of methods of analysis and supporting spectroscopic information on monomers and additives used for food contact materials (principally packaging). The site which is aimed primarily at assisting food control laboratories in the European Union contains analytical information on monomers, starting substances and additives used in the manufacture of plastics materials. A searchable index is provided giving PM and CAS numbers for each of 255 substances. For each substance a data sheet gives regulatory information, chemical structures, physico-chemical information and background information on the use of the substance in particular plastics, and the food packaging applications. For monomers and starting substances (155 compounds) the infra-red and mass spectra are provided, and for additives (100 compounds); additionally proton NMR are available for about 50% of the entries. Where analytical methods have been developed for determining these substances as residual amounts in plastics or as trace amounts in food simulants these methods are also on the website. All information is provided in portable document file (PDF) format which means that high quality copies can be readily printed, using freely available Adobe Acrobat Reader software. The website will in future be maintained and up-dated by the European Commission's Joint Research Centre (JRC) as new substances are authorized for use by the European Commission (DG-ENTR formerly DGIII). Where analytical laboratories (food control or other) require reference substances these can be obtained free-ofcharge from a reference collection housed at the JRC and maintained in conjunction with this website compendium.     

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.     

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.     

Analysis of benzo[a]pyrene in spiked fatty foods by second derivative synchronous spectrofluorimetry after microwave-assisted treatment of samples

A simple, rapid and inexpensive method has been developed for the determination of benzo[a     

The development of reference materials for paralytic shellfish poisoning toxins in lyophilized mussel. II: Certification study

This paper describes the second part of a project undertaken to develop certified mussel reference materials for paralytic shellfish poisoning toxins. In the first part two interlaboratory studies were undertaken to investigate the performance of the analytical methodology for several PSP toxins, in particular saxitoxin and decarbamoyl-saxitoxin in lyophilized mussels, and to set criteria for the acceptance of results to be applied during the certification exercise. Fifteen laboratories participated in this certification study and were asked to measure saxitoxin and decarbamoyl-saxitoxin in rehydrated lyophilized mussel material and in a saxitoxin-enriched mussel material. The participants were allowed to use a method of their choice but with an extraction procedure to be strictly followed. The study included extra experiments to verify the detection limits for both saxitoxin and decarbamoyl-saxitoxin. Most participants (13 of 15) were able to meet all the criteria set for the certification study. Results for saxitoxin.2HCl yielded a certified mass fraction of <0.07 mg/kg in the rehydrated lyophilized mussels. Results obtained for decarbamoyl-saxitoxin.2HCl yielded a certified mass fraction of 1.59+/-0.20 mg/kg. The results for saxitoxin.2HCl in enriched blank mussel yielded a certified mass fraction of 0.48 +/- 0.06 mg/kg. These certified reference materials for paralytic shellfish poisoning toxins in lyophilized mussel material are the first available for laboratories to test their method for accuracy and performance.     

Announcing a new international peer-reviewed journal:Food Science and Human Wellness now accepting manuscript submission in English

<正>We are pleased to announce the launch of a new international peer-reviewed journal-Food Science and Human Wellness,ISSN 2213-4530,which is an open access journal,produced and hosted by Elsevier B.V.on behalf of Beijing Academy of Food Sciences.Food Science and Human Wellness is an international peer-reviewed English journal that provides a forum for the dissemination of the