HPLC测定氨酪酸氯化钠注射液中氨酪酸的含量

目的 建立测定氨酪酸氯化钠注射液中氨酪酸的HPLC方法.方法 采用CAPCELL PAK C18柱,流动相:以磷酸二氢钾溶液(取磷酸二氢钾10.0 g与己烷磺酸钠1.1g,加水溶解并稀释至1000mL,磷酸调节pH 2.1)-甲醇(90∶10)为流动相;流速1.0 mL/min,检测波长210nm,柱温30℃,进样量10μL.结果 氨酪酸在0.08～1.6 mg/mL范围内线性关系良好(r=0.9999),平均回收率99.89％(RSD=0.25％,n=6).结论 该方法准确、简便、快速,适用于测定氨酪酸氯化钠注射液中氨酪酸的含量.     

高效液相色谱法测定氯雷他定片溶出度

目的 采用高效液相色谱法(HPLC)测定氯雷他定片的溶出度.方法 色谱柱:Agilent C18柱(4.6 mm× 150 mm,5 μm)色谱柱;流动相:磷酸盐缓冲液(取磷酸氢二钾2.28 g,加水800 mL溶解,磷酸调pH6.0,加水至1000 mL)-甲醇(20∶80);检测波长247 nm;流速1.0 mL/min;进样量20μL.结果 氯雷他定在0.1～10 μg/mL浓度范围内呈良好的线性关系(R=0.9998),平均回收率99.09％,RSD=0.4％(n=6).结论 此法可排除辅料对溶出度的影响,可用于该制剂的质量控制.     

HPLC测定吡嗪酰胺片的含量

目的 为吡嗪酰胺片含量测定建立新的质量控制方法.方法 采用高效液相色谱法(HPLC)测定吡嗪酰胺片中吡嗪酰胺的含量.色谱柱:Agilent C18(250 mm×4.6 mm,5μm),流动相:甲醇-水(10∶90),检测波长269 nm,流速1.0mL/min,柱温30℃,理论板数按吡嗪酰胺峰计算应不低于3000.结果 在2.024～20.24 μg/mL浓度范围内,吡嗪酰胺进样量与峰面积呈良好的线性关系,r=0.9999,平均回收率为99.8％(n=6),RSD=0.8％.结论 本法简便、准确,重现性及灵敏度高,可用于吡嗪酰胺片中吡嗪酰胺的含量测定.     

HPLC测定葛根汤颗粒中葛根素的含量

目的 建立RP-HPLC测定葛根汤颗粒中葛根素含量的方法.方法 采用HPLC法,C18色谱柱(250 mm×4.6 mm,5 μm),以乙腈-甲醇-水(10∶8∶82)为流动相,检测波长250 nm.结果 葛根素浓度在4.008～200.4 μg/mL范围内与峰面积呈良好的线性关系,y=0.012 6x+0.014 1,r=1.000 0(n=6),平均回收率100.02%,RSD0.1%.结论 此方法简便、准确,可作为葛根汤颗粒的质量控制方法.     

卫生整理纺织品中芦荟组分含量的HPLC/DAD测定法

采用高效液相色谱-二级管阵列检测器(HPLC/DAD),建立测定纺织品中芦荟主要成分(芦荟苷,芦荟大黄素和大黄酚)含量的方法.HPLC的色谱柱为Agilent Eclipse XDB-C18(4.6×150 mm,5 m),流动相为甲醇-0.1％磷酸水溶液(80∶20,体积比),流速为1.0 mL/min;检测波长为256 nm和358 nm.通过验证,其标准曲线在检测范围内均呈良好线性(R2≥0.999),日内和日间精密度的相对标准偏差RSD小于2.97％,3个加标水平的平均回收率为95.1％～ 101.1％.     

RP-HPLC测定溴芬酸钠滴眼液中苯扎溴铵的含量

目的建立反相高效液相色谱法(RP-HPLC)测定溴芬酸钠滴眼液中苯扎溴铵含量。方法采用ZorbaxC18(250mm×4.6mm,5μm)色谱柱,流动相为0.003mol/L磷酸氢二铵溶液(每1000mL含三乙胺10mL,用磷酸调节pH3.0)-乙腈(40:60),流速1.0mL/min,检测波长214nm,进样量20μL。结果阴性溶液对苯扎溴铵含量测定无干扰。苯扎溴铵浓度在10.10~202.00μg/mL范围内与峰面积线性关系良好(r=0.9999)。本法精密度、重复性、回收率、耐用性良好,供试品溶液在24h内稳定,定量限为62ng。结论本法与药典方法比较,基线噪音明显降低。该方法操作简单,能准确、快速测定苯扎溴铵,可用于滴眼液中苯扎溴铵的含量测定。     

HPLC法测定盐酸奥洛他定滴眼液的含量

目的 建立HPLC测定盐酸奧洛他定滴眼液含量的方法.方法 以十八烷基键合硅胶为填充剂,流动相0.05 mol/L磷酸二氢钾-乙腈-三乙胺(760:240:2),用磷酸调pH至4.5,检测波长254 nm,流速1.0 mL/min.结果 盐酸奧洛他定在0.05～0.15 mg/mL范围内早良好的线性关系(r=0.999 7),平均回收率100.2%(n=9),RSD=0.99%.结论 HPLC方法简便灵敏准确,重复性好,可用于盐酸奧洛他定的质量控制.     

HPLC测定盐酸左氧氟沙星滴眼液中防腐剂羟苯乙酯含量

目的 建立HPLC测定盐酸左氧氟沙星滴眼液中防腐剂羟苯乙酯含量的方法.方法 以十八烷硅烷基键合硅胶为填充剂;以0.005 mol/L醋酸铵溶液(每1 000 mL含三乙胺10 mL,用冰醋酸调pH 5.0)-乙腈(50∶50)为流动相;检测波长256 nm;流速1.0 mL/min;柱温35℃.结果 羟苯乙酯在0.017 7～0.041 3 mg/mL范围内呈良好的线性关系(r=0.999 97).平均回收率100.4%(n=9),RSD=0.97%.结论 此法简便、快速、准确,可有效控制产品质量.     

钛胶反相高效液相色谱法测定饮料中的咖啡因

建立了利用钛胶反相柱快速测定饮料中咖啡因的含量的高效液相色谱方法.色谱条件:分离柱为Titania Sachtopore - RP柱(250mm×4.6mm i.d.,5μm),柱温30℃,流动相为水∶甲醇=83∶17 (V/V),流速1 mL/min,检测波长273nm.线性范围为12 - 900μg/mL,此范围内标准曲线线性良好(R2=0.9998).最低检出限(S/N =3)为0.03 μg/mL,样品加标回收率范围为98.6％～102.2％,精密度即相对标准偏差(n=9)小于0.23％.本法简单易操作、分析速度快,精密度和准确度均取得满意效果,适用于各种饮料样品中咖啡因的定量分析.本研究不仅是对食品中咖啡因检测方法的补充,更重要的是发挥了钛胶固定相不可比拟的优势.     

HPLC测定注射用盐酸表柔比星的含量

目的 建立HPLC测定注射用盐酸表柔比星的含量.方法 三甲基硅烷键合硅胶柱(250 mm×4.6 mm,5μm),流动相:乙腈-水-甲醇-85％磷酸溶液(290∶540∶170∶1)并含0.2％十二烷基硫酸钠,流速1.0 mL/min,检测波长254 nm,柱温35℃,进样量20 μL.结果 盐酸表柔比星在0.0518～0.1554 mg/ml的浓度范围内有良好的线性关系(r＝0.9999),平均回收率为99.64％(RSD ＝0.71％).结论 此法是一种简便,快速,准确的分析方法,专属性强,能有效地控制盐酸表柔比星的含量.     

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