基于固相萃取-液相色谱-串联质谱法的纺织品中三氯生和三氯卡班的测定

采用固相萃取-液相色谱-串联质谱技术(SPE-LC-MS/MS)建立了同时测定纺织品中三氯生和三氯卡班的分析方法。样品用二氯甲烷超声提取,C18固相萃取净化后分析。串联质谱在多反应监测(MRM)模式下检测目标分析物,以保留时间和特征离子对(母离子和碎片离子)信息比较进行定性和定量分析。三氯生和三氯卡班的线性范围分别为1.0~50.0 ng/mL、0.25~50.0 ng/mL。方法的定量限为1.0和0.25 μg/kg,平均回收率为84.5% ~ 108.2 %,相对标准偏差小于8.1 %。实验结果表明该方法准确、灵敏,可用于纺织品中三氯生和三氯卡班的分析测定。     

固相萃取/ 固相微萃取- 气相色谱法测定饮用水中多溴联苯醚

目的：建立固相萃取/固相微萃取-气相色谱法测定饮用水中多溴联苯醚(BDE-47和BDE-99)含量的新方法。方法：固相萃取-气相色谱直接取水样100mL,过LC-C18柱,经正己烷洗脱,洗脱液于80℃水浴挥干,异辛烷定容至1mL,直接进样1μL测定,该法对BDE-47和BDE-99的检出限分别为0.0008μg/L和0.0009μg/L,回归方程相关系数分别为0.9996和0.9997,RSD(n＝6)分别为1.0%～4.9%和0.96%～4.4%;固相微萃取-气相色谱直接取水样10mL置于15mL固相微萃取瓶中,于40℃条件下固相微萃取吸附25min后,纤维头经风干,立即进样测定。该法对BDE-47和BDE-99的检出限分别为0.0000μg/L和0.0044μg/L,回归方程相关系数分别为0.9996和0.9992,RSD(n＝6)分别为6.7%～11.4%和6.0%～10.1%。结果：随机抽样某市52个水样进行检测,均未检出BDE-47和BDE-99。结论：建立饮用水中多溴联苯醚固相萃取/固相微萃取-气相色谱检测的新方法,两种方法操作简便、快速,精密度、准确度及回收率均令人满意。     

QuEChERS萃取-液相色谱法测定酱油和酱制品中三氯蔗糖

建立了Qu ECh ERS萃取-液相色谱法测定酱油和酱制品中三氯蔗糖含量的分析方法。样品以乙腈作为萃取溶剂,采用改进的Qu ECh ERS方法进行萃取。以乙腈和水为流动相,C18色谱柱分离,液相色谱-蒸发光散射检测器进行检测。三氯蔗糖在20～1 500μg/m L呈良好线性关系,相关系数(r2)> 0. 99; 3个水平下的加标回收率为83. 2%～95. 4%;相对标准偏差(RSD)为4. 1%～6. 3%;方法检出限为1 mg/kg,定量限为3 mg/kg;方法简单、快速、准确可靠,适用于酱油及酱制品中三氯蔗糖的快速检测。     

反相高效液相色谱法分离测定三氯蔗糖

建立了测定三氯蔗糖的反相高效液相色谱法。色谱柱采用SupelcosilTMLC-18(250mm×4.6mmi.d.,5μm),流动相为V(乙腈)∶V(甲醇)∶V(水)=15∶5∶80。三氯蔗糖在10～800mg/L范围内线性良好,最低检测浓度为0.2mg/L。平均回收率为99.5%,变异系数为0.84%。该方法简便、快速,灵敏度高,重现性好。     

SPE-HPLC-MS/MS法同时测定电子烟烟液中9种甜味剂

为建立固相萃取-液相色谱/串联质谱(SPE-HPLC-MS/MS)法同时测定电子烟烟液中安赛蜜、糖精钠、甜蜜素、三氯蔗糖、阿斯巴甜、阿力甜、新橙皮甙二氢查尔酮、纽甜、甜菊糖苷等9种甜味剂的方法,以水为萃取溶剂对样品进行超声提取,萃取液经C_(18)硅胶键合固相萃取柱净化和氮吹浓缩,采用Waters XBridge C_(18)色谱柱分离,以甲醇-5 mmol/L乙酸铵的水溶液为流动相进行梯度洗脱,使用电喷雾离子源正负离子切换多反应监测(MRM)模式进行质谱检测,采用华法林钠为内标进行定量。结果表明:(1)在优化条件下,目标物在各自测试浓度范围内线性良好(R~2均大于0.998),检出限和定量限分别在0.005～0.287μg/mL和0.017～0.956μg/mL之间,加标回收率在82.96%～114.01%之间,RSDs在2.19%～5.18%之间。(2)对市售8种不同品牌电子烟烟液的检测结果显示,仅在1个样品中检出纽甜,质量分数为5.92 mg/kg。(3)该方法结果准确可靠,适用于电子烟烟液中9种甜味剂的同时定量检测。     

顶空-固相微萃取/气相色谱串联质谱法测定葡萄酒中多种氯酚及氯代茴香醚

样品中氯酚经乙酰化生成乙酰氯酚后,通过优化萃取头、离子强度、温度、时间等固相微萃取条件后,建立顶空-固相微萃取-气相色谱串联质谱法同时测定测定葡萄酒中的3种氯酚2,4,6-三氯酚(TCP)、2,3,4,6-四氯酚(TeCP)、五氯酚(PCP)以及两种氯代茴香醚2,4,6-三氯苯甲醚(TCA)、五氯苯甲醚(PCA)含量的方法。结果表明：该方法检出限为0.1ng/L,回收率为86.0%～105.9%,相对标准偏差小于16.5%。该方法前处理简单、高效、检测灵敏度高,可应用于进出口葡萄酒中木塞污染物的监控。     

罐头食品中双酚A和双酚F环氧衍生物残留的高效液相色谱分析

建立了一种高效液相色谱分析罐头食品中双酚A(BPA)和双酚F(BPF)环氧衍生物的方法。样品经微波辅助萃取后过PPL(填料为苯乙烯-二乙烯苯(SDVB)聚合物)固相萃取柱进行净化试验。结果表明,微波辅助萃取法的提取效果理想;采用PPL固相萃取回收率在73.26%~104.98%,除杂效果明显。将微波辅助—PPL固相萃取净化法应用于多种食品进行分析,结果表明该方法适用于食品中双酚A和双酚F环氧衍生物残留分析。     

分散固相萃取-高效液相色谱法测定水果中三氯生及三氯卡班

目的建立分散固相萃取-高效液相色谱法测定水果中三氯生及三氯卡班残留的新方法。方法样品采用乙腈溶液涡旋超声提取后,加入十八烷基键合硅胶吸附剂(C18)作为分散固相萃取净化剂进行净化(200mg),用高效液相色谱法在278 nm处测定,采用PICKERING C8色谱柱(4.6 mm×250 mm i.d.,5μm),以甲醇:水(78:22,V:V)的溶液为流动相等度洗脱,流速1.2 m L/min。结果在最优检测条件下,各目标化合物的加标回收率为72.9%~104.4%,相对标准偏差在2.1%~9.1%之间。三氯生及三氯卡班的检出限分别为0.05和0.02 mg/kg,定量限分别为0.15和0.06 mg/kg。结论该方法分析快速、简便,适用于水果中三氯生及三氯卡班的测定。     

ASE/SPE-GC/MS测定17种含氯苯类有机污染物

建立加速溶剂-固相萃取-气质联用（ASE/SPE-GC/MS）法同时测定纺织固废物中17种氯苯类和氯甲苯类有机污染物（CCBs）的检测方法。加速溶剂萃取试验采用萃取溶剂丙酮∶二氯甲烷（1∶3）,萃取温度110℃,萃取压力11 MPa,循环萃取3次;采用固相萃取净化比较以Si和Florisil为填料的两类固相萃取柱在不同溶剂淋洗下对CCBs萃取效果的影响。结果表明,Si基质的固相萃取柱在二氯甲烷的洗脱下对CCBs回收率最高;以ASE/SPE-GC/MS法测得纺织固废物的回收率为80.0%～103.5%,相对偏差RSD(n=7)小于5.5%。     

固相萃取柱净化-高效液相色谱法测定谷物中的呕吐毒素残留量

目的 建立固相萃取柱净化-高效液相色谱法快速检测小麦、大麦、玉米及大米等谷物中呕吐毒素的残留量。方法 样品经乙腈-水提取液(85:15, V:V)提取,过HLB固相萃取柱净化。采用C_18柱为分离柱,对流动相的组成和洗脱斱式等参数进行优化和探讨。以水和甲醇为流动相进行梯度洗脱,流速为0.8 mL/min,柱温35℃,外标法定量。结果 呕吐毒素浓度在0.05～5.0 mg/L的范围内线性关系良好,相关系数均大于0.9999。呕吐毒素在0.5、1.0和2.0 mg/L添加水平的回收率为79.7%～106.0%,相对标准偏差(relative standard deviation,RSD)小于4.2%(n=5),斱法定量限为300μg/kg。结论 该斱法简便、快捷、准确、灵敏度较高,适用于小麦、大麦、玉米及大米等的谷物中呕吐毒素的快速检测。     

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