超高效液相色谱-串联质谱法测定鱼油软胶囊中的合成抗氧化剂

目的建立超高效液相色谱-串联质谱法(ultra performance liquid chromatography-tandem mass spectrometry,UPLC-MS/MS)测定鱼油软胶囊中叔丁基对苯二酚(tert-butylhydroquinone,TBHQ)、2,6-二叔丁基-4-甲基苯酚(butylated hydroxytoluene,BHT)、丁羟基茴香醚(butyl hydroxyanisole,BHA)和没食子酸丙酯(propyl gallate,PG)4种合成抗氧化剂的含量。方法采用乙腈为溶剂和涡旋方式对152批次鱼油软胶囊进行提取;UPLC以乙腈-水为流动相进行梯度洗脱,质谱采用电喷雾离子源负离子模式(electrospray ionization,ESI-)及多反应监测模式(multiple reaction monitoring,MRM)进行测定。结果 PG、TBHQ、BHA和BHT在0.50~20μg/mL浓度范围内具有良好的线性关系(r0.997),在2、8和16 mg/kg3个不同浓度加标水平下测得回收率为88.8%~94.2%,RSD为1.6%~4.2%(n=6),检出限为0.2μg/kg。结论该方法灵敏度高、抗干扰性强且准确性好,可适用于鱼油软胶囊中PG、TBHQ、BHA和BHT合成抗氧剂的检测。     

超高效液相色谱串联质谱法测定全蛋粉中的双酚A和双酚S

建立超高效液相色谱-串联质谱测定全蛋粉中双酚A和双酚S的检测方法。全蛋粉经水复溶后经乙腈提取,提取液使用分散系固相萃取-基质增强脂质去除产品进行除脂,使用Oasis PRiME HLB小柱进一步净化,使用超高效液相串联质谱测定,负离子多反应监测(MRM)模式测定,内标法定量。结果显示:双酚A在1~50 μg/kg范围内呈线性,相关系数为0.9991,加标回收率为98.8%~105.0%,日内和日间相对标准偏差分别为3.84%~8.58%和5.65%~8.74%,检出限为0.3 μg/kg,定量限为1.0 μg/kg;双酚S在0.4~20 μg/kg范围内呈线性,相关系数为0.9995,加标回收率为98.5%~102.5%,日内和日间相对标准偏差分别为3.01%~7.86%和3.18%~7.03%,检出限为0.1 μg/kg,定量限为0.3 μg/kg。实际样品测定结果分别为:双酚A 2.4~3.8 μg/kg;双酚S 0.48~0.82 μg/kg。本方法前处理简单、高灵敏度适用于全蛋粉中双酚A和双酚S的日常测定。     

超高效液相色谱-串联质谱法检测牛奶中双酚A

目的通过优化牛奶中双酚A提取纯化和测定条件,建立牛奶中双酚A(bisphenol A,BPA)的超高效液相色谱-串联质谱(ultra performance liquid chromatography-tandem mass spectrometry,UPLC-MS/MS)定量检测方法。方法 采用乙腈作为提取剂和蛋白质沉淀剂,混合型阴离子固相萃取柱净化,采用UPLC-MS/MS在负离子模式下检测,内标法定量。结果该方法在1~100μg/L范围内有良好的线性关系,相关系数r20.990,在空白牛奶基质中,不同添加水平下方法的平均回收率范围为92%~115%,相对标准偏差为3.7%~6.6%;测定低限为1μg/kg。结论 此方法灵敏度高、准确、重现性好,适用于牛奶样品中双酚A的检测。     

GPC-UPLC-MS/MS法测定食用油中壬基酚和双酚A

建立食用油中壬基酚和双酚A的凝胶渗透色谱(GPC)-超高效液相色谱-质谱联用(UPLC-MS/MS)分析检测方法。食用油样品经乙酸乙酯-环己烷溶解,GPC净化后,采用超高效液相色谱-串联质谱法分析测定。仪器使用WATERS ACQUITY UPLC BEH C18色谱柱,以甲醇-0.1%氨水为流动相,梯度洗脱分离后,串联四极杆质谱多反应监测方式检测,采用内标法定量。分析结果表明,目标物检出限为1.0μg/kg,在1.0μg/kg~5.0×10~2μg/kg的范围内呈良好的线性关系(R~20.99),试验中平均添加回收率85.1%~112.5%,相对标准偏差2.57%~6.08%。     

高效液相色谱法检测运动饮料中双酚A的残留

建立一种快速、有效的高效液相色谱法测定运动饮料中双酚A残留的方法。样品经乙醇提取后,采用C18固相萃取小柱进行净化和富集。采用苯基色谱柱(4.6 mm×250 mm,5μm)分离,以乙腈∶水=40∶60(体积比)作为流动相,用PDA检测器检测,外标法峰面积定量。结果表明,双酚A标液在0.10μg/m L~1.00μg/m L浓度范围内线性良好,相关系数r~2为0.999,检出限为5.0μg/kg,定量限为15.0μg/kg,加标回收率达到92.1%~93.8%。该方法具有前处理简单、富集效果好和检测速度快的优点,适用于运动饮料中双酚A残留的定量检测。     

DSPE-UPLC-MS/MS测定畜禽产品中壬基酚和双酚A

建立了分散固相萃取-超高效液相色谱-串联质谱法(DSPE-UPLC-MS/MS)测定畜禽产品中壬基酚和双酚A的分析方法。样品采用乙腈超声提取,无水Mg SO_4去除水分后,用N-丙基乙二胺(PSA)和十八烷基硅胶(C_(18))吸附剂分散固相萃取净化。采用Agilent Poroshell 120 EC-C_(18)柱(4.6 mm×50 mm,2.7μm)为分离柱,以甲醇和2 mmol/L氟化铵溶液为流动相,梯度洗脱。采用电喷雾离子源在负离子多反应监测扫描(MRM)模式下进行测定,内标法定量。在优化的试验条件下,壬基酚和双酚A的检出限为0.1μg/kg,定量限为0.3μg/kg;线性范围为1.0~50μg/kg,相关系数大于0.99。不同畜禽产品(猪肉、牛肉、鸡肉、猪肝和鸡蛋)在1.0,5.0和10μg/kg三个添加水平下的平均回收率为85.9%~110.7%,相对标准偏差(RSD)(n=6)为2.75%~10.65%。该方法准确灵敏、简便快速,适用于畜禽产品中壬基酚和双酚A的分析检测。     

同位素稀释-超高效液相色谱-串联质谱法测定茶叶中的高氯酸盐

目的建立茶叶中高氯酸盐的超高效液相色谱-串联质谱测定方法。方法茶叶中高氯酸盐用0.2%乙酸提取,经石墨炭黑柱净化,优选Synergi~(TM)MAX-RP柱(4.6 mm×250 mm,4μm)为分析柱,以超高效液相色谱-串联质谱法测定,内标法定量。结果高氯酸盐在0.25~50.0μg/L范围内线性良好,回归方程y=1.569x+0.0268,相关系数r~2=0.999 6。加标浓度为0.05~0.50 mg/kg时,回收率95.6%~120.0%,相对标准偏差(RSD)1.9%~17.5%。检出限为2.5μg/kg。结论本方法前处理简单、准确、灵敏度高,适用于茶叶中高氯酸盐的测定。     

免疫亲和柱净化/色谱技术测定婴幼儿配方乳粉中V_(B12)

建立了婴幼儿配方乳粉中VB12的超高效液相色谱-串联质谱和超高效液相色谱测定方法。样品采用pH=4.0的醋酸钠溶液提取,经免疫亲和柱净化,采用Waters BEH C18色谱柱分离,液相法采用0.03 mol/L的磷酸缓冲盐(pH=3.5)和乙腈为流动相进行等度洗脱,紫外检测器波长为361 nm。质谱法以0.1%的甲酸水和甲醇为流动相进行梯度洗脱,采用电喷雾-正离子模式多反应监测进行定性和定量分析,外标法定量。VB12在10~500μg/L的质量浓度范围内线性关系良好,VB12的检出限均为0.5μg/kg,定量限均为1.5μg/kg,液相方法回收率为90.2%~98.3%,相对标准偏差为1.4%~2.5%,液相色谱-质谱法回收率为89.3%~95.7%,精密度在1.9%~3.1%。该方法简单、灵敏度高、分析时间短、定量准确,适用于婴儿乳粉中VB12的测定。     

分散固相萃取-超高效液相色谱-串联质谱法测定农产品中螺虫乙酯及其3种代谢产物残留量

目的建立农产品中螺虫乙酯及其3种代谢产物的超高效液相色谱-串联质谱检测方法。方法样品经乙腈涡旋提取,采用乙二胺-N-丙基硅烷(primary secondary amine,PSA)和HC-C_(18)分散固相萃取剂净化,经超高效液相色谱串联质谱仪多反应监测模式检测,外标法定量。结果螺虫乙酯及其3种代谢产物在0.1~100μg/L质量浓度范围内与其呈良好的线性关系(r~20.999),检出限为0.1μg/kg,螺虫乙酯代谢产物S1定量限为1.0μg/kg,其余为0.2μg/kg,在添加水平为1.0、25、50μg/kg时,平均回收率为82.5%~99.1%,测定结果的相对标准偏差为1.3%~8.4%(n=6)。结论该方法简单、快速,重复性好,灵敏度和准确度均能满足农产品中螺虫乙酯残留量的测定。     

超高效液相色谱-串联质谱法测定茶叶中的百草枯

文章建立了一种利用超高效液相色谱-串联质谱法测定茶叶中百苹枯含量的方法.茶叶样品使用甲醇-0.1 mol/L盐酸溶液(3:7,V/V)提取,经Poly-sery MCX柱净化后用超高效液相液相色谱-串联质谱进行测定.在5～100μg/L浓度范围内,百草枯的线性良好(R2=0.9991),方法定量限为0.01 mg/kg...     

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