液质联用法检测降血糖类保健食品中非法添加的13种化学药物

建立同时检测保健食品中非法添加的13 种化学降糖药物的液相色谱串联质谱分析方法并用于实际检测。保健食品样品经甲醇超声提取后,以色谱柱(2.1 mm×150 mm,5 μm)进行分离,甲醇和10 mmol/L乙酸铵水溶液(含0.1 %甲酸)为流动相梯度洗脱;采用电喷雾电离源正离子(electrospray ionization positive,ESI+),多反应监测(multiple reaction monitoring,MRM)模式进行检测。13 种化学降糖药物线性相关系数均大于0.999,定量限(limits of quantitation,LOQ)为45.7 μg/kg^79.6 μg/kg,回收率为78.6 %~112.1 %,相对标准偏差(relative standard deviations,RSD)为 0.6 %~3.5 %。从11种样品中检测出5种样品含非法添加化学药物,且均为复合添加。2种样品添加二甲双胍,5种样品添加苯乙双胍,2种样品添加罗格列酮,1种样品添加甲苯磺丁脲,1种样品添加吡格列酮,5种样品添加格列本脲。     

超高效液相色谱-串联质谱法检测多基质保健食品中27种非法添加降糖类化合物

目的 建立超高效液相色谱-三重四极杆质谱检测保健食品中27种降糖类非法添加化合物的方法。方法 4种不同基质保健品样品经甲醇超声提取后，采用Waters XBridge Amide色谱柱 (2.1 mm×100 mm, 3.5 μm)，以5 mmol/L甲酸铵水溶液和5 mmol/L甲酸铵乙腈作为流动相进行梯度洗脱，分离苯乙双胍、二甲双胍、伏格列波糖、阿卡波糖、丁二胍共5种化合物；采用Waters CORTECS T3色谱柱 (2.1 mm×100 mm, 2.7 μm)，以0.1%甲酸水溶液和乙腈作为流动相进行梯度洗脱，分离维达列汀、罗格列酮、西他列汀、吡格列酮等22种化合物；环格列酮采用电喷雾离子化负离子模式，其余26种化合物采用电喷雾离子化正离子模式，以多反应监测方式进行检测。结果 伏格列波糖、阿卡波糖、达格列净、卡格列净、曲格列酮、环格列酮6种化合物在250 ng/mL~12.5 μg/mL范围内线性关系良好，其余21种化合物在5~250 ng/mL范围内线性关系良好，线性相关系数r均大于0.99；27种化合物检出限(limit of detection, LOD)范围为1~1000 μg/kg；在低、中、高三水平加标，其回收率均在70%~120%范围内，相对标准偏差(relative standard deviation, RSD)为0.7%~10% (n=6)。结论 本方法快速、灵敏、高效、准确，适用范围广，可用于保健食品中降糖类化合物的高通量检测。     

TLC-UPLC-MS/MS法检测网红保健品中非法添加的8种化学药物

建立薄层色谱-超高效液相色谱-串联质谱法同时检测网红保健品中非法添加的8 种化学药物。样品采用薄层色谱法进行前处理,采用Kinetex 100 RP-18（100 mm×2.1 mm,1.6 μm）色谱柱分离,以乙腈-1 mmol/L乙酸铵（含0.1%乙酸）溶液为流动相梯度洗脱,采用多重反应监测方式检测西布曲明、洛伐他汀、辛伐他汀、麻黄碱、咖啡因、酚酞、苯乙双胍和西地那非等8 种药物。结果表明,8 种化合物在0.5～100 μg/L范围内线性关系良好,相关系数≥0.995 8,各组分的检出限在0.09～0.29 μg/kg之间,定量限在0.31～0.79 μg/kg之间。待测物在不同样品中的平均回收率介于67.3%～101.1%,变异系数≤16.5%。45 批保健食品检出23 批非法添加阳性样品。本法经方法学验证,可用于网红保健品中8 种非法添加药物的快速筛查和定量测定。     

高效液相色谱-串联质谱法测定降压类保健食品中5种α-受体阻断剂类非法添加药物的含量

目的 建立高效液相色谱-串联质谱(high performance liquid chromatography-tandem mass spectrometry,HPLC-MS/MS)法检测降压类保健食品中5种α-受体阻断剂含量的检测斱法。方法 样品经甲醇提取,残留物经Waters Sunfire C_18 (100 mm×2.1 mm, 5μm)色谱柱分离,以0.1%甲酸水溶液-0.1%甲酸乙腈溶液为流动相梯度洗脱,流速为0.3 mL/min,采用多反应监测正离子模式,定性和定量测定降压类保健食品中酚妥拉明、妥拉唑林、哌唑嗪、特拉唑嗪和育亨宾等5种α-受体阻断剂。结果 5种α-受体阻断剂分别在0.5～160μg/L浓度范围内呈现良好的线性关系,相关系数均大于0.993;酚妥拉明和哌唑嗪斱法的检出限为5μg/kg,定量限为10μg/kg;特拉唑嗪和育亨宾的检出限为2μg/kg,定量限为5μg/kg;妥拉唑林的检出限为15μg/kg,定量限为40μg/kg;添加水平分别为10～100、5～50、40～400μg/kg时,样品平均回收率为81.6%～113.5%,相对标准偏差为0.69%～4.80%(n=5)。结论 该斱法简便、快捷、准确、灵敏度高,适用于降压类保健食品中非法添加的酚妥拉明、妥拉唑林、哌唑嗪、特拉唑嗪及育亨宾等5种α-受体阻断剂的快速检测。     

减肥保健食品中违禁添加双胍类西药的分析方法研究

目的：建立测定减肥保健食品中违禁添加二甲双胍和苯乙双胍的超高效液相色谱-串联质谱分析方法．并通过研究其质谱特征,推测质谱裂解途径。方法：不同基质类型的减肥保健食品超声提取15min．经弱阳离子交换固相萃取小柱WCX净化后,以ACQUITY UPLC BEHHILIC（1．7um,100mm×2．1mm）分离,进行UPLC—MS／MS多反应监测模式下的定性及定量分析。结果：苯乙双胍在0．1～50ug／L的范围内呈良好的线性关系,相关系数为0．9996;二甲双胍在0．05-50ug／L的范围内呈良好的线性关系,相关系数为0．9995。在3个添加水平范围内的平均回收率为80．7％．96.3％：日内精密度均小于8％,日间精密度均小于10％。结论：本方法分析速度快,灵敏度高,回收率好,可用于不同减肥保健食品中违禁添加二甲双胍和苯乙双胍的同时检测。     

超高效液相色谱-串联质谱法测定鲟鱼中庆大霉素和新霉素残留量

目的建立超高效液相色谱-串联质谱法(ultra performance liquid chromatography-tandemmass spectrometric,UPLC-MS/MS)检测鲟鱼中庆大霉素和新霉素的分析方法。方法样品经10mmol/L磷酸盐缓冲溶液提取, 0.1%甲酸沉淀蛋白, HLB固相萃取柱净化。采用CORTECS HILIC(100 mm×2.1 mm, 1.6μm)色谱柱分离,以0.1%甲酸溶液(A)和乙腈(B)作为流动相进行梯度洗脱,通过电喷雾正离子扫描(electronic spray ion,ESI+),多反应监测模式(multiplereaction monitoring,MRM)对庆大霉素和新霉素的定量离子和定性离子进行测定。结果本方法在5 min内完成2种目标化合物的分离分析。庆大霉素在25～300μg/L浓度范围内呈现良好的线性关系,相关系数r20.995;方法检出限为10μg/kg,定量限为25μg/kg;添加量为25、50、100μg/kg时回收率在76.7%～106.3%之间,相对标准偏差(relative standard deviation, RSD)在0.18%～2.15%之间(n=6)。新霉素在50～600μg/L浓度范围内呈现良好的线性关系,相关系数r20.996;方法检出限为20μg/kg,定量限为50μg/kg;在50、100、200μg/kg添加水平的回收率为96.1%～109.0%之间,相对标准偏差(RSD)在0.72%～2.84%之间(n=6)。结论该方法精密度好、灵敏度高,能简便、准确地测定鲟鱼中庆大霉素和新霉素的药物残留。     

保健食品中13种那非类物质快速检测及确证

建立一种高效液相色谱同时测定保健食品中13种那非类非法添加物质的定性及定量分析方法,采用超高液相色谱串联质谱对阳性样品进行快速确证。样品中的那非物质经乙腈提取后,采用Waters Symmetry Shield C18 (250 mm×4.6 mm, 5μm)色谱柱,以乙腈-20 mmol/L乙酸铵水溶液(含0.1%乙酸)进行梯度洗脱,液相色谱紫外检测器进行检测,超高液相色谱串联质谱进行确证。结果表明, 13种那非类物质在50 min内有良好的分离度,在0.3～50μg/mL范围内线性关系良好,相关系数(R2)≥0.998,检出限(LOD)为28.52～39.71 mg/kg,定量限(LOQ)为62.60～143.50 mg/kg,低(1倍定量限)、中(5倍定量限)、高(10倍定量限) 3个水平的平均回收率为92.64%～109.17%。该方法简便、快捷、准确度高,适合保健食品中非法添加物质的快速检测和准确定量。     

GC检测虾中氯霉素残留的研究

建立了虾中氯霉素残留的带电子捕获检测器的气相色谱方法.通过改进虾样品前处理的操作,结果表明:氯霉素浓度在0.5μg/L～500μg/L的范围内呈良好的线性关系(R2=0.9996),最低检测限为0.1μg/kg,定量限为0.5 μg/kg;向样品中分别添加10、100、200μg/kg3个浓度水平的氯霉素回收率分别为99.3%、109.9%和116.9%,变异系数为3.1%～9.2%.该方法灵敏.精密度高.     

UPLC-MS/MS测定牛奶中9种青霉素

建立超高效液相色谱-串联四极杆质谱多反应离子监测模式同时测定牛奶中9种青霉素类抗生素(包括羟氨苄青霉素、氨苄青霉素、邻氯青霉素、双氯青霉素、乙氧柰胺青霉素、苯唑青霉素、苄青霉素、苯氧甲基青霉素、甲氧苯基青霉素)残留量的检测方法。样品采用乙腈沉淀蛋白、脱脂后,过HLB小柱净化、富集。以0.01 mol/L乙酸铵水(甲酸调节p H 4.5)-乙腈梯度洗脱,经Agilent Eclipse plus C18色谱柱(2.1×100 mm,粒径1.8μm)分离后,采用MRM模式进行定量定性分析。结果:结果表明9种抗生素在0.1μg/L~100μg/L范围内线性关系良好,高中低浓度回收率在67.7%~92.8%,相对标准偏差(n=6)小于15%,各组分定量限为0.1μg/kg~4μg/kg。     

反相高效液相色谱法测定油类保健食品中 混合生育酚

目的建立测定油类保健食品中混合生育酚的反相高效液相色谱法。方法样品经氢氧化钾甲醇溶液皂化,盐酸甲醇溶液中和;用反相高效液相色谱:色谱柱(SUPELCO,C18,4.6 mm×150 mm,5μm);流速:1.0 m L/min;柱温:40℃;进样量:20μL;波长:294 nm;流动相:水和甲醇,梯度洗脱;将α-、γ-及δ-生育酚分离;外标法定量。结果本方法标准曲线在0.01~0.20 mg/m L范围内有良好的线性关系,r0.9990,回收率为93.5%~103.8%,RSD4.0%,检出限为0.02μg/kg,定量限为0.1μg/kg。结论该方法结果准确可靠,节省样品前处理时间及试剂,有利于降低检验成本,适用于油类保健食品中混合生育酚含量的测定。     

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.     

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.     

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.     

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.     

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.