清咽类保健食品中非法添加盐酸二氧丙嗪的检测方法研究

目的建立对保健食品中非法添加的盐酸二氧丙嗪的筛查方法。方法采用薄层色谱法(TLC)进行快速筛查,采用高效液相色谱法(HPLC)对盐酸二氧丙嗪进行定性分析以及定量测定,并采用超高效液相-质谱联用法(UPLC-MS)进行确证。结果薄层色谱法盐酸二氧丙嗪斑点显色明显;高效液相色谱法在11.149~222.977μg/mL范围内线性良好,质谱图中盐酸二氧丙嗪分子离子峰及二级碎片离子明显。结论本方法专属性强,灵敏度高,重现性好,可作为清咽类保健食品是否添加盐酸二氧丙嗪的检测方法。     

高效液相色谱法测定保健食品中非法添加盐酸二氧丙嗪的不确定度分析

目的采用高效液相色谱法测定保健食品中非法添加盐酸二氧丙嗪的含量,进行不确定度分析。方法依据标准JJF 1059.1-2012《测量不确定度评定与表示》,建立数学模型,对测定不确定度的来源进行分析和量化。结果保健食品中非法添加盐酸二氧丙嗪含量为1.90 g/kg时,其相对扩展不确定度为0.088,测定结果可表示为X=(1.90±0.17)g/kg(k=2)。根据测量结果分析,在影响检测结果不确定度的各分量中,拟合标准曲线求溶液中目标物浓度所引入的不确定度是对结果影响较大的不确定度分量,可通过减少这个不确定度分量提高测量结果的质量。结论该研究可为实验室评定保健食品中非法添加盐酸二氧丙嗪的测定结果质量提供参考。     

全自动固相萃取-UPLC-MS/MS法检测清咽类保健食品中非法添加的盐酸二氧丙嗪和沙丁胺醇

建立全自动固相萃取-超高效液相色谱-串联质谱法（UPLC-MS/MS）检测清咽类保健食品中非法添加的盐酸二氧丙嗪和沙丁胺醇的方法。样品用乙酸铵缓冲溶液和甲醇溶解,采用MCX固相萃取柱进行在线净化,然后通过ACQUITY UPLC BEH C₁₈ （2.1 mm×50 mm,1.7 μm）分离,以甲酸溶液（0.1%甲酸和10 mmol/L甲酸铵）和甲醇为流动相,梯度洗脱,流速0.2 mL/min,采用电喷雾离子源（ESI）正离子模式,多反应监测（MRM）进行检测。所测盐酸二氧丙嗪和沙丁胺醇的线性范围分别为 4.9~49.2 ng·mL?1 和 4.3~42.7 ng·mL?1,线性回归方程的决定系数分别为0.9999和0.9998。盐酸二氧丙嗪和沙丁胺醇呈良好的线性关系,且得到较好的分离度。低、中、高3个添加水平的平均回收率为87.4%~98.8%,RSD为0.83%~3.9%（n=3）,盐酸二氧丙嗪和沙丁胺醇的检出下限分别为0.65和0.58 μg/kg。经方法学验证,所建立的分析方法可靠、灵敏、准确,可用于清咽类保健食品中非法添加的盐酸二氧丙嗪和沙丁胺醇同时定性和定量分析。     

高效液相色谱-二极管阵列检测器测定兽药、保健食品中茶碱、二羟丙茶碱和盐酸二氧丙嗪

目的 建立兽药中三种非法添加物茶碱、二羟丙茶碱和盐酸二氧丙嗪的检测方法。方法 采用Waters XBridge C18(4.6×250 mm,5 μm)作为高效液相色谱(HPLC)的色谱柱,二极管阵列紫外检测器(PDA)作为检测器。同时测定茶碱和二羟丙茶碱：以水-甲醇(70:30,V:V)为流动相,流速为1.0 mL/min,检测波长为272 nm。测定盐酸二氧丙嗪：以0.025 mol/L磷酸溶液-乙腈(72:28,V:V)为流动相,流速为1.0 mL/min,检测波长264 nm。结果 茶碱和二羟丙茶碱能得到良好分离,272 nm波长处色谱图清晰可辨。在 1～50 μg/mL范围内线性关系良好,相关系数大于0.9999,在不同样品中的回收率分别为99.2%～101.8%、96.0%～103.6%。盐酸二氧丙嗪在 1～50 μg/mL范围内线性关系良好,相关系数大于0.999,在不同样品中的回收率在95.9%～103.9%之间。结论 本方法简便、灵敏、快速、经济,可对兽药中非法添加的上述三种平喘类药物进行定性和定量检测。     

高效液相色谱法测定保健食品中丙氨酰-酪氨酸的含量

目的 建立高效液相色谱法测定保健食品中丙氨酰-酪氨酸含量的分析方法。方法 样品经一级水超声提取, 采用Agilent C18柱(150 mm×4.6 mm, 2.7 μm)进行分离, 以乙腈-水溶液为流动相进行等度洗脱, 采用高效液相色谱法检测, 外标法定量。结果 很好地分离了丙氨酰-酪氨酸, 在浓度0.01~0.05 mg/mL之间呈现良好的线性关系, 平均回收率在95%~105%之间, 相对标准偏差(relative standard deviation, RSD)为1.0%。 结论 该方法准确、灵敏度高、重现性好, 适用于保健食品中丙氨酰-酪氨酸含量的测定。     

减肥保健食品中非法添加盐酸西布曲明的检测

建立减肥保健食品中非法添加化学成分盐酸西布曲明的定性、定量检测方法.采用薄层色谱法、高幸合嗌?二极管阵列检测法、LC/MS/MS联用技术进行定性鉴别,并采用高效液相色谱法测定其中盐酸西布曲明的含量.结果在抽取的43种市售产品中,有9种检出了盐酸西布曲明.该方法快速、简便、准确、可靠,可用于有效监测保健食品中非法添加的盐酸西布曲明.     

安神类保健食品中新型非法添加药物的检测研究

目的建立超高效液相色谱法(UPLC)及气相色谱-质谱(GC-MS)法,用于检测并确证安神类保健食品中的新型非法添加药物。方法采用溶剂超声或液-液萃取方式对样品进行提取后,采用UPLC进行测定。UPLC采用ZORBAX SB-C_(18)(2.1×150 mm,1.8μm)色谱柱分离,采用乙腈和0.1%磷酸溶液为流动相进行梯度洗脱,流速为0.4 m L/min,采集210 nm色谱图进行样品初筛。GC-MS采用DB-5MS毛细管色谱柱(30 m×0.25mm×0.25μm)分离,程序升温条件为:初始温度150℃(1 min),以8℃/min升至250℃(5 min),12℃/min升至280℃(15 min),选择EI离子源,溶剂延迟2 min,质谱扫描50~600 amu。结果本方法能够在23 min内快速检测安神类保健食品中的新型非法添加药物,先经UPLC分析样品发现可疑色谱峰,再运用气质联用技术确证为一种新型非法添加药物盐酸氟桂利嗪。结论该方法快速、简便、准确,为保健食品中新型非法添加药物的检测提供了研究思路和参考。     

高效液相色谱法测定保健食品中三氯蔗糖的含量

目的建立一种保健食品中三氯蔗糖含量测定的高效液相色谱检测法。方法样品采用Rad pak C18色谱柱(4.6 mm×250 mm,5μm)进行分离,以1.0 m L/min乙腈:水(V:V=15:85)为流动相,最后用高效液相色谱法(HPLC)-示差折光仪为检测器进行测定,外标法定量分析。结果高效液相色谱法在0.482~2.892 mg/m L浓度范围,三氯蔗糖的浓度和峰面积的线性良好,相关系数为0.999(r0.99),该方法的检出限和定量限分别为19.58 mg/g和65.27 mg/g,在不同的添加水平下,该方法的回收率范围为95.0%~95.6%,相对标准偏差为0.3%(n=9)。结论高效液相色谱法灵敏度、准确度均较高,适用于保健食品中三氯蔗糖的含量测定。     

超高效液相飞行串联质谱检测改善睡眠类保健食品中22种非法添加化学物质方法的研究

目的建立超高效液相飞行串联质谱(ultra performance liquid chromatography/time-of-flight mass spectrometry,UPLC-Q-TOF-MS-MS)快速检测改善睡眠类保健食品中22种违法添加化学物质的方法。方法样品经甲醇提取后,采用超高效液相色谱/质谱测定法,以ACQUITYTM UPLC HSS T3(50 mm×1.8 mm×1.7μm)为分析柱,0.1%甲酸溶液-乙腈为流动相进行梯度洗脱,电喷雾电离(ESI),正、负离子模式进行质谱数据采集,对改善睡眠类保健食品中22种违法添加化学物质进行筛选分析。结果建立了快速分离检测保健食品中22种非法添加物质的测定方法,22种违法添加化学物质的色谱图分离度良好,检测限均低于1 ng,质谱分辨率符合鉴别要求。结论该方法专属性强、灵敏度高,快捷,可作为改善睡眠类违法添加药物的有效检测方法。     

LC-MS及HPLC快速定性分析盐酸曲美他嗪制备过程中杂质

目的建立一种盐酸曲美他嗪制备过程中杂质快速定性分析的方法。方法采用液相色谱-质谱联用(LC-MS)和高效液相色谱法(HPLC)对反应过程进行跟踪监测。结果对盐酸曲美他嗪杂质5和杂质8进行了定性分析。结论该方法可快速鉴定工艺研发过程中杂质,对研发过程质量控制及工艺优化有较好的指导意义。     

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