高效凝胶色谱法测定注射用美罗培南聚合物含量

目的建立了注射用美罗培南中美罗培南聚合物的测定方法。方法采用TSK GEL G2000SW/600凝胶柱,以磷酸盐缓冲液(pH 7.0)[0.01 mol/L磷酸氢二钠溶液-0.01 mol/L磷酸二氢钠溶液(61:39)]为流动相,流速为0.5 ml/min,检测波长为254 nm,外标法计算聚合物的含量。结果美罗培南聚合物与美罗培南能较好地分离;美罗培南浓度在0.5040～4.0359 mg/ml范围内,与美罗培南峰面积或聚合物峰面积和的线性关系良好,重复性RSD为2.41%(n=6)。结论所采用的方法科学、简便、结果可靠,可用于注射用美罗培南聚合物的检测。     

替比培南酯原料药中钯残留监测方法的建立

目的建立测定替比培南酯(1)原料药中微量钯的方法。方法采用微波消解处理样品,石墨炉原子吸收分光光度法测定1中钯的残留量。结果钯在0.01~0.1μg/mL范围内与吸光度呈良好的线性关系(r=0.994);检测限为0.0024μg/mL;方法重复性试验RSD为5.27%;平均回收率为105.1%,RSD为2.10%(n=9)。结论该方法操作简便、灵敏准确,可用于微量钯含量的测定,为1质量控制提供依据。     

气相色谱法测定替比培南酯中的残留溶剂

目的建立替比培南酯中残留溶剂含量测定方法。方法采用程序升温顶空气相色谱法,使用毛细管色谱柱(DB-624,30 m×0.53 mm,3.0μm),测定乙腈、乙醇、乙酸乙酯、正丁醇、异丙醇、甲基叔丁基醚和N, N-二甲基甲酰胺的含量。结果 7种残留溶剂的检测限在70.173～2.084μg/ml之间,精密度试验结果RSD在1.25%～4.34%之间,回收率测定结果在96.36%～100.98%。结论本方法简便、快速、灵敏度好、可有效测定替比培南酯中残留溶剂含量。     

RP-HPLC测定阿奇霉素缓释阴道栓的含量

目的建立RP-HPLC测定阿奇霉素缓释阴道栓的含量。方法用C18（4.6 mm×150 mm,5μm）柱,以乙腈-磷酸氢二钾溶液（0.02 mol/L）-磷酸二氢钾溶液（0.07 mol/L）溶液（60：25：15）为流动相,柱温40℃,流速1.2 mL/min,检测波长215 nm。结果阿奇霉素的线性范围为60～800μg/mL,r=0.999 8;低、中、高3种浓度的平均回收率分别为101.4%,99.1%,101.2%。结论本方法简便、灵敏、准确。     

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。     

TSK凝胶色谱系统测定注射用盐酸头孢替安有关物质Ⅱ

目的建立测定注射用盐酸头孢替安中的有关物质Ⅱ的高效液相凝胶色谱法。方法采用TSK GEL2000SWXL色谱柱(TOSOH,7.8 mm×300 mm,5μm),以pH 7.0的0.005 mol/L磷酸盐缓冲液[磷酸氢二钠溶液-磷酸二氢钠溶液(50:50)]-乙腈=90:10为流动相,检测波长为254 nm,流速为0.6 ml/min。结果头孢替安对照品溶液在0.19～19.05μg/ml范围内,溶液浓度和峰面积呈良好的线性关系(r=0.9999)。重复性试验RSD为1.42%(n=6),中间精密度试验RSD为1.60%(n=12)。结论该凝胶色谱方法操作简便,专属性强,灵敏度高,结果可靠,适用于注射用盐酸头孢替安中有关物质Ⅱ的检测。     

达肝素钠原料药中游离硫酸盐测定方法的研究

目的建立达肝素钠原料中游离硫酸盐测定方法。方法采用离子色谱法,色谱柱为Waters IC-Pak Anion(50mm×4.6 mm,10μm),流动相为7 mmol/L四硼酸钠-0.1 mol/L氢氧化钠,梯度洗脱,流速1.0 mL/min,进样量25μL,电导检测器,抑制电流50 mA。结果硫酸根离子与其他离子分离度好,在0.4~15μg/mL浓度范围内线性关系良好,相关系数r=0.999,重复性试验的RSD为1.6%,检出限为0.05μg/mL,定量限为0.4μg/mL,平均回收率为103.0%,RSD为2.3%(n=9)。结论此法可用于达肝素钠中游离硫酸盐测定。     

HPLC测定维拉佐酮片的含量

目的建立高效液相色谱法(HPLC)测定维拉佐酮片含量的方法。方法采用Waters Symmetry色谱柱(250 mm×4.6 mm,5μm),以0.01 mol/L醋酸铵溶液(取醋酸铵0.77 g,加水950 mL,加三乙胺1 mL,用醋酸调节p H值至6.0±0.05,加水至1000 mL)-乙腈(50:50)为流动相,流速1.0 mL/min,检测波长242 nm,进样体积20μL。结果维拉佐酮峰面积与浓度在12.1~28.1μg/mL范围内线性良好(r=0.9999);回收率为99.88%(n=9),RSD为0.37%。结论此法操作简便,结果准确度高,精密度好,可用于维拉佐酮片的含量测定。     

RP-HPLC法测定薁磺酸钠滴眼液的含量

目的测定薁磺酸钠滴眼液中薁磺酸钠的含量。方法用RP-HPLC法,色谱柱：Dikma C18柱（150 mm×4.6 mm,5μm）;流动相：乙腈-0.02 mol/L磷酸二氢钾水溶液（体积比为33：67,用磷酸调pH 4.5）;检测波长：293 nm;柱温：室温;流速：0.9 mL/min。结果薁磺酸钠在12.0～60.0μg/mL范围内线性关系良好（R=0.999 9）;薁磺酸钠的平均回收率为100.1%,RSD为0.14%。结论该方法简单、快捷,回收率和重复性良好,可作为薁磺酸钠滴眼剂质量评价的方法。     

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。     

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.     

Detection of adulteration of locust bean gum with guar gum by capillary electrophoresis and polarized light microscopy

Capillary electrophoresis (CE) and polarized light microscopy (PLM) were utilized in the detection of the adulteration of locust bean gum with guar gum. For CE analyses, standards of locust bean and guar gums were extracted with 30% CH₃CN, removing the residual proteins from the gum matrix. A 8.75 mM NaH₂PO₄-20.6 mM Na₂B₄O₇ buffer, pH 9, was used to separate these proteins and to identify marker proteins that were present in the guar gum. These markers did not co-migrate with components in the extracts of mechanically processed locust bean gum, and are used as indicators of adulteration. Using PLM with toluidine blue and iodine staining techniques, unadulterated locust bean gum samples were distinguished from mixed samples through the differential staining of components in locust bean versus guar and tara gums. These experiments in the use of CE and PLM provide orthogonal and complementary methods for the verification of 'true' positives and the elimination of 'false' positives.     

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%.