DLLME-UPLC-MS/MS法测定食用油中的双酚类化合物

基于分散液液微萃取(DLLME)技术和同位素稀释-超高效液相色谱-质谱/质谱(ID-UPLC-MS/MS),建立了一种快速测定食用油中7种双酚类化合物的方法。优化了萃取剂种类及体积、涡旋分散时间等影响萃取的关键因素;优化了UPLC分离条件和质谱定性定量参数。优化条件为:400μL甲醇/乙腈(1∶1,v/v)混合溶液作为萃取剂,涡旋分散萃取1 min;以C18色谱柱和甲醇-0.05%氨水梯度洗脱分离,质谱多反应监测模式(MRM)测定。结果表明,7种双酚类化合物在0.5μg/L~500μg/L内线性关系良好,相关系数均在大于0.998,方法定量限(S/N=10)在0.2μg/L~3.0μg/kg之间,3个添加水平的平均回收率为80.1%~93.7%,相对标准偏差(n=6)为4.4%~9.1%。本方法前处理简单,节省溶剂和时间,准确灵敏,适用于食用油中7种双酚类化合物的检测。     

分散液液微萃取/气相色谱-串联质谱技术联用快速测定酱油中糠醛类物质

建立了分散液液微萃取/气相色谱-串联质谱法(GC-MS/MS)测定酱油中糠醛、5-甲基糠醛、5-羟甲基糠醛的方法。样品经乙腈提取,提取液进一步进行分散液液微萃取(DLLME)处理,然后用GC-MS/MS多反应监测模式(MRM)进行测定。3种糠醛物质在0.002～10 mg/L范围内均呈良好的线性关系,相关系数R≥0.999;检出限(S/N=3)为0.005～0.01 mg/kg,加标回收率为87.6%～100.2%。该法简便、快速、可靠、灵敏度高,适用于酱油中糠醛类物质的测定。     

盐辅助分散液液微萃取-气相色谱-串联质谱法检测葡萄酒中的氨基甲酸乙酯

目的建立了盐辅助分散液液微萃取(salt-assisted dispersive liquid-liquid microextraction,SADLLME),稳定同位素稀释,气相色谱-串联质谱法(gas chromatography-tandem mass spectrometry,GC-MS/MS)检测葡萄酒中氨基甲酸乙酯(ethyl carbamate,EC)的方法。方法取30 mL葡萄酒于50 mL离心管中,加入浓度为10μg/mL的EC-d5溶液100μL和硫酸钠3 g,震荡溶解,注射针快速打入700μL二氯甲烷,震荡1 min,离心,取下层有机相,经DB-INNWAX UI色谱柱(30 m×0.25 mm,0.25μm)分离,多重反应监测方式进行质谱检测。结果方法在验证浓度范围内(5～1500 ng/mL),线性良好,r~2=0.9988,检出限为0.73μg/L,定量限为2.18μg/L,回收率为91.5%～97.8%,相对标准偏差为2.55%～5.26%。对市场上3个品牌红葡萄酒进行检测,EC含量为6.82～15.3μg/L。结论该方法样品处理简便、快速,相对绿色,定性、定量可靠,能够满足葡萄酒中EC风险监测的需要。     

ASE-GC-MS/MS法测定海产品中苯并(a)芘含量方法的建立

建立快速溶剂萃取-气相色谱-三重四级杆串联质谱(GC-MS/MS)法测定海产品中的苯并(a)芘的分析方法。方法利用快速溶剂萃取仪进行提取,以丙酮和乙腈体系(2︰1, V/V)为提取溶剂, GC-MS/MS法进行定性定量分析。结果表明,苯并(a)芘浓度在0.5～20 ng/mL范围内线性关系良好,相关系数为0.999 1;检出限为0.03μg/kg;两种海产品加标回收率(低点0.1μg/kg,中点0.4μg/kg,高点4.0μg/kg)分别为94.9%和90.0%;精密度RSD (n=6)分别为1.39%和1.65%;重复性RSD (n=6)分别为3.83%和3.26%。试验证明,该方法具有前处理简单、分析速度快、检出限低、检测结果准确等优点。     

气相色谱-串联三重四极杆质谱法测定甘蔗中苯酰胺类农药残留

建立了气相色谱-串联三重四极杆质谱(GC-MS/MS)同时测定甘蔗中22种苯酰胺类农药残留的方法。破碎的甘蔗样品用乙腈提取,经QuEChERS法净化后,采用GC-MS/MS进行分析检测,在动态多反应监测模式下(dMRM),外标法定量。22种苯酰胺类农药在5～500μg/L范围内线性良好(r2>0.999),检出限为0.1～3.8μg/kg,定量限为0.4～12.5μg/kg。分别在样品中添加22种苯酰胺类农药标准溶液,进行3水平(10、50、500μg/kg)添加回收实验,加标回收率范围为71.7%～104.0%,日内精密度相对标准偏差(RSD)(n=6)为0%～6.7%,日间精密度相对标准偏差(RSD)(n=3)为4.7%～9.0%。该方法高效便捷、灵敏度和准确度高,适用于甘蔗中22种苯酰胺类农药残留的检测。     

分散液相微萃取-液相色谱法测定奶瓶中的双酚A

建立了分散液相微萃取提取婴儿奶瓶中溶出痕量双酚A(BPA)的方法,并用高效液相色谱测定了其含量。奶瓶浸泡液用0.5 mL氯仿作萃取剂,0.5 mL甲醇作分散剂,以3 500 r/min离心10 min,吸取萃取剂20μL,进样,采用高效液相色谱法(HPLC)测定BPA的含量。色谱柱为Inertsil C18柱(5μm,4.6×150 mm),流动相为甲醇∶水(V∶V)=70∶30,流速为0.8 mL/min,检测波长为280 nm。该方法 BPA在0.05 mg/L~0.25 mg/L范围内线性关系良好(R=0.999 7),BPA检出限(S/N=3)为0.50μg/L。该法用于婴儿奶瓶中BPA含量的检测,测得婴儿奶瓶中双酚A的含量范围在0~18.93μg/L,平均加标回收率为96.44%,RSD为4.57%(n=4)。方法结果满意,可适用于婴儿奶瓶、矿泉水等食品和饮料容器中溶出BPA的含量测定。     

基于碳纳米管分散固相萃取及测定皮革中磷酸三酯物

基于分散固相萃取(d-SPE)结合超高效液相色谱串联三重四级杆质谱(UPLC-MS/MS)技术,建立了测定皮革中9种磷酸三酯类化合物(包括:TMP、TEP、TBP、TCEP、TBEP、TCPP、TTP、TPh P和TEHP)的新方法。结果表明,9种磷酸三酯类化合物在0.5~200μg/L浓度范围内线性关系良好,相关系数均大于0.998,方法检出限(S/N=3)为3~10μg/kg,添加水平为10~300μg/kg时,9种目标物的平均回收率为73%~105%,相对标准偏差(n=6)为2.3%~8.6%。本方法具有前处理简单、分析快速、准确等特点,适用于皮革样品中9种磷酸三酯类化合物的测定。     

盐辅助分散液液微萃取结合气相色谱-串联质谱法快速检测啤酒中N-二甲基亚硝胺

目的建立盐辅助分散液液微萃取(salt assisted dispersi ble liquid-liquid microextraction, SADLLME)气相色谱-串联质谱法(gas chromatography-tandem mass spectrometry, GC-MS/MS)检测啤酒中N-二甲基亚硝胺(N-dimethylnitrosamine, NDMA)的分析方法。方法取30 mL啤酒于50 mL的离心管中,加入浓度为1μg/mL的NDMA-d6甲醇溶液50μL,硫酸钠3 g,振荡溶解,快速打入二氯甲烷600μL,振荡1 min,离心,弃去上清液,取下层有机相,上机检测。结果方法在考察浓度为1～100μg/L的范围内线性良好,相关系数大于0.998;添加回收率为97.7%～104.8%,相对标准偏差为4.07%～8.46%;检出限为0.03μg/L,定量限为0.10μg/L。实际样品检测显示,啤酒样品中均检出含有NDMA,但含量远低于国际限量5μg/L,处于较安全水平。结论该方法具有样品处理简便、快速、成本低廉,方法检出限极低,准确度高,可满足啤酒中NDMA检测的需要。     

液相色谱-串联质谱法测定烟草制品中的羰基化合物

建立了测定烟草制品中8种羰基化合物的液相色谱-串联质谱(LC-MS/MS)方法。以d3-甲醛-2, 4-二硝基苯腙为内标,样品经乙腈萃取后用DNPH将其衍生化反应、过0.45μm有机相滤膜后直接进行LC-MS/MS分析。结果表明:8种羰基化合物在1～80 ng/m L范围内,线性相关系数均≥0.999 0, 3个加标水平的回收率在92.1%～96.3%之间,相对标准偏差(RSD)为2.3%～4.9%。方法的检出限(LOD)和定量限(LOQ)分别为0.14～0.3μg/g (S/N=3)和0.5～1.0μg/g (S/N=10)。该方法准确、灵敏,适合用于烟草样品中羰基化合物的测定。     

气相色谱-串联质谱法同时测定花生中97种农药

采用气相色谱-串联质谱法(GC-MS/MS)测定花生中97种农药。花生样品加水浸润后以0.1%乙酸乙腈为提取溶剂,超声波辅助萃取,采用改进的Qu ECh ERS法净化,气相色谱在选择反应扫描模式下测定。97种农药在6.25～200μg/L浓度范围内线性良好,线性相关系数均大于0.99,在10、20、50μg/kg 3个浓度水平下平均添加回收率在73%～120%,相对标准偏差小于17.4%(n=6)。该方法适用于花生中多种农药残留快速定量分析。     

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.     

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     

Chinese CTP Market

According to Printing and Printing Equipment Industries Association of China（PEIAC）＇s statistics to the plate manufucturer in China, in 2013, the actual offset plate production has reached 346 million square meters in China. Among them, the CTP production volume was 245 million square meters, up by 11% than that of last year; the total sales of the CTP plate was 239 million square meters, up by 13%.     

Preparatory Work of Print China 2015 is Going Smoothly

正Held at Guangdong Modern International Exhibition Center,Print China 2015 will cover 7exhibition halls,besides the original Hall No.3,4,5,6,7,the newly built F zone of Hall 3 will be used too.The total area will be140,000 square meters.Hall 3:Offset and large printing equipment,package printing equipment,post press