超高效液相色谱串联质谱法测定咖啡豆中草甘膦、氨甲基膦酸和草铵膦残留量

目的建立超高效液相色谱串联质谱法(ultraperformanceliquidchromat-ography/tandemmass spectrometry, UPLC-MS/MS)定量测定咖啡豆中草甘膦、氨甲基膦酸和草铵膦残留量。方法通过水提取样品,C18固相萃取小柱进行净化, FMOC-Cl溶液衍生,后采用超高效液相色谱串联质谱测定。结果草甘膦、氨甲基膦酸和草铵膦在2～100ng/mL范围内线性良好(r2≥0.999),方法的定量限为0.05mg/kg。在添加水平为0.05 mg/kg和0.5 mg/kg时,回收率为99.6%～107.6%,相对标准偏差低于4.52%。结论该方法准确、稳定、灵敏,能够满足咖啡豆中草甘膦、氨甲基膦酸和草铵膦检测与确证的需要。     

QuEChERS—UPLC/MS/MS快速测定茶叶中的草甘膦和氨甲基磷酸

采用QuEChERS—超高效液相色谱—串联质谱技术同时测定茶叶中的草甘膦和氨甲基磷酸农药残留。茶叶样品用纯水提取,经分散固相萃取净化,以乙腈和0.1%氨水溶液为流动相进行梯度洗脱,采用CORTECSTM UPLC~C_(18+)色谱柱分离,电喷雾—负离子多反应模式监测,内标法定量。草甘膦和氨甲基磷酸农药在5~500μg/L内线性关系良好,相关系数均大于0.999,该方法的检出限为10μg/kg,定量限为30μg/kg。分别添加30,100,500μg/kg 3个浓度水平的草甘膦和氨甲基磷酸农药,草甘膦的回收率为90.5%~93.5%,相对标准偏差为4.1%~7.2%;氨甲基磷酸的回收率为99.2%~102.4%,相对标准偏差为3.4%~8.3%。该方法前处理简便、分析速度快、方法稳定,适用于茶叶中草甘膦和氨甲基磷酸农药残留的同时测定。     

高效液相色谱-质谱/质谱法测定茶叶中的草甘膦和氨甲基膦酸残留

建立了高效液相色谱-质谱/质谱法测定茶叶中的草甘膦(PMG)和氨甲基膦酸(AMPA)残留量的测定方法。样品采用超纯水提取、氯甲酸-9-芴基甲酯衍生,再经HLB柱净化后上机测定,并以内标法定量。结果表明:草甘膦和氨甲基膦酸在0.001~0.5 mg/L内线性良好,相关系数(R2)分别为0.999 9和0.999 8,平均回收率和相对标准偏差分别为78.2%~103.4%和2.1%~6.2%,方法的定量下限分别为1.0μg/kg和7.5μg/kg。该方法基质干扰小、灵敏度高、准确可靠,适用于茶叶中草甘膦及氨甲基膦酸残留量的定量检测。     

QuEChERS-气相色谱-三重四级杆串联质谱法测定茶叶中草甘膦和氨甲基膦酸残留

建立气相色谱-三重四极杆质谱测定茶叶中草甘膦和氨甲基膦酸的分析方法。茶样经超纯水、二氯甲烷提取后,与三氟乙酸酐-七氟丁醇进行衍生反应,衍生后产物经乙二胺-N-丙基硅烷(PSA)、石墨化碳(GCB)、C18混合净化剂净化,TG-1701MS(30 m×0.25 mm,0.25μm)分离,气相色谱-串联质谱进行测定。试验详细考察了PSA、GCB、C18用量对草甘膦和氨甲基膦酸添加回收率的影响,结果表明,2 m L衍生液中加入50 mg PSA、25 mg GCB和25 mg C18时净化效果最好。在5μg/L~500μg/L范围内,草甘膦和氨甲基膦酸均有良好的线性关系(r20.999),定量限(LQD)(S/N=10)分别为0.03 mg/kg和0.015 mg/kg,样品加标浓度为0.50、1.00 mg/kg和2.50 mg/kg时,草甘膦的平均回收率为86.1%~101.2%,相对标准偏差(RSD)(n=6)为3.2%~6.7%;氨甲基膦酸的平均回收率为83.6%~103.4%,相对标准偏差(RSD)(n=6)为3.6%~7.3%。该方法样品前处理简单,分析时间短,回收率和精密度等均符合草甘膦和氨甲基膦酸检测技术的要求,适用于茶叶中草甘膦和氨甲基膦酸残留的检测。     

多壁碳纳米管分散固相萃取-液质联用技术测定茶叶中草甘膦、草铵膦、氨甲基膦酸残留量

目的建立茶叶中草甘膦、草铵膦和氨甲基膦酸残留量的超高效液相色谱串联质谱分析方法。方法样品经水提取后采用分散固相萃取技术,以多壁碳纳米管(MWCNTS)和N-丙基乙二胺键合固相吸附剂(PSA)吸附提取液中的杂质,上清液用9-芴基氯甲酸酯(FMOC-Cl)衍生。衍生物用BEH C18进行分离,以乙腈-4 mmol乙酸铵水溶液为流动相,电喷雾正离子模式电离(ESI+),多反应监测模式检测(MRM),外标法定量。结果方法的线性范围是0.1～1μg/mL,相关系数大于0.999,定量限为10μg/kg,以绿茶为基质,三种物质添加水平分别为0.25、0.50、1.00 mg/kg,回收率范围分别为草甘膦95%~116%,草铵膦98%~118%,氨甲基膦酸74%~84%,精密度均小于6.79%(n=6)。结论该方法具有简便快速、灵敏度高、准确性强等特点,适合于测定茶叶中草甘膦、草铵膦和氨甲基膦酸的含量。     

液相色谱-串联质谱法检测植物源食品中 草甘膦及其代谢物的残留量

目的建立一种高效液相色谱-串联质谱测定植物源食品中草甘膦及其代谢物氨甲基膦酸残留量的分析方法。方法样品经水超声提取,用二氯甲烷去除脂肪,并用C18固相萃取小柱进行净化,以9-芴甲基氯甲酸酯(FMOC-Cl)进行衍生,最后采用高效液相色谱-串联质谱进行测定。结果对茶叶和其他植物源食品的检出限分别为0.1 mg/kg和0.02 mg/kg,在5~100 ng/m L线性范围内线性关系良好(r20.999)。草甘膦各浓度水平的平均回收率为74.6%~96.5%,相对标准偏差为0.041%~0.553%(n=6);氨甲基膦酸的平均回收率为65.1%~79.4%,相对标准偏差为0.024%~0.338%(n=6)。结论建立的方法快速简便,灵敏度较高,精密度较好,符合国家标准对植物源食品中农药残留测定的要求,可用于食品安全监管。     

多壁碳纳米管分散固相萃取-液质联用技术测定 茶叶中草甘膦、草铵膦、氨甲基膦酸残留量

摘 要：目的 建立茶叶中草甘膦、草铵膦和氨甲基膦酸残留量的超高效液相色谱串联质谱分析方法。方法 样品经水提取后采用分散固相萃取技术,以多壁碳纳米管（MWCNTS）和N-丙基乙二胺键合固相吸附剂（PSA）吸附提取液中的杂质,上清液用9-芴基氯甲酸酯（FMOC-Cl）衍生。衍生物用BEH C18进行分离,以乙腈-4 mmol乙酸铵水溶液为流动相,电喷雾正离子模式电离（ESI ）,多反应监测模式检测（MRM）,外标法定量。结果 方法的线性范围是0.1?1 μg/mL,相关系数大于0.999,定量限为10 μg/kg,以绿茶为基质,三种物质添加水平分别为0.25、0.50、1.00 mg/kg,回收率范围分别为草甘膦95%~116%,草铵膦98%~118%,氨甲基膦酸74%~84%,精密度均小于6.79%（n=6）。结论 该方法具有简便快速、灵敏度高、准确性强等特点,适合于测定茶叶中草甘膦、草铵膦和氨甲基膦酸的含量。     

液相色谱串联质谱法测定蛋及蛋制品中三聚氰胺残留

本文建立了液相色谱串联质谱法（LC-MS/MS）测定蛋及蛋制品中三聚氰胺残留量的方法,优化了样品前处理方法及液相色谱串联质谱测定条件。采用1%三氯乙酸提取,亚铁氰化钾和乙酸锌沉淀蛋白质、脂肪等物质,固相萃取小柱净化,液相色谱串联质谱检测。结果表明：在优化条件下,本方法测定三聚氰胺在0～3.0mg/kg范围内线性良好,其线性方程为y=12 342x＋242.73,相关系数R2=0.998 4,方法检出限和定量限分别为0.01mg/kg和0.05mg/kg,加标回收率为60.0%～85.0%。该方法可满足蛋及蛋制品中三聚氰胺残留量的检测要求。     

液相色谱-串联质谱法检测牛奶中10种β-兴奋剂

建立了液相色谱-串联质谱同时检测牛奶中10种β-兴奋剂残留量的方法.样品经沉淀蛋白质,酸性水溶液提取, 提取液经Oasis MCX 固相萃取柱净化,LC/MS/MS方法测定.采用了Thermo Hypersil Gold (150×2.1 mm,5 μm) 色谱柱;5 mmol 乙酸铵水溶液-甲醇流动相,梯度洗脱.方法线性相关系数r均大于0.999.克伦特罗检出限为1.68 μg/kg,其余9种β-兴奋剂的检出限在0.146～0.203 μg/kg之间;克伦特罗定量限为3.37 μg/kg,其余9种β-兴奋剂的定量限在0.290～0.407 μg/kg之间.3个添加水平下,10种β-兴奋剂平均回收率在91% ～127%之间.     

超高效液相色谱-串联质谱法同时测定刺梨原汁中27种游离营养成分

目的：采用超高效液相色谱-串联质谱(Ultra-high performance liquid chromatography-tandem mass spectrometry,UPLC-MS/MS)技术建立同时测定刺梨原汁中27种游离营养成分的分析方法。方法：样品用50%(V:V)乙腈水提取,经Agilent Poroshell 120 HILIC-Z色谱柱(2.1 mm×100 mm,2.7μm)分离,以20 mmol/L甲酸铵水溶液-20 mmol/L甲酸铵乙腈溶液为流动相梯度洗脱,质谱采用电喷雾离子源,正负离子同时扫描,多反应监测模式。结果：待测化合物在相应浓度范围内线性关系良好(R2>0.995),检出限为0.05～0.90 mg/kg,定量限为0.20～3.00 mg/kg。加标回收率为80.11%～107.13%,相对标准偏差为2.97%～9.82%。应用该方法对4批次刺梨原汁样品进行分析,样品中游离氨基酸总量在1405.66～2061.28 mg/kg,游离维生素B族化合物总量在6.98～10.56mg/kg,游离儿茶素平均含量为517.97 mg/kg。结论：该方...     

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.     

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.     

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