HPLC法测定妇炎净片中氯化两面针碱的含量

目的建立HPLC测定妇炎净片中氯化两面针碱含量的方法。方法选用不同的方法处理样品。采用VP-ODSC18柱,流动相为乙腈:水:三乙胺(25:75:0.3),流速为1.0 ml/min,检测波长为328 nm,测定氯化两面针碱的含量。结果氯化两面针碱对照品在1.125￣18μg/ml之间呈良好的线性关系,相关系数为0.999 9,两种样品处理方法效果较好,氯化两面针碱平均回收率分别为100.26%(RSD 2.11%)和99.82%(RSD 1.85%)。结论HPLC测定上述两种处理方法的样品稳定性好,重现性高,均可用于测定妇炎净片中氯化两面针碱的定量。     

高效液相色谱法同时测定心动颗粒中阿魏酸和欧前胡素的含量

目的建立高效液相色谱法(HPLC)同时测定心动颗粒中阿魏酸和欧前胡素含量。方法色谱柱为Welchrom@C18反相色谱柱(4.6 mm×250 mm,5μm);流动相为乙腈(A)-水(10 mmol/L磷酸)(B),梯度洗脱:0~3.5 min,15%A;3.5~12 min,15%A→25%A;12~21 min,25%A);流速1.0 m L/min;检测波长310 nm;柱温35℃。结果阿魏酸和欧前胡素的质量浓度分别在5.19~51.90μg/m L和5.20~52.05μg/m L浓度范围内呈良好的线性关系(r20.9995),平均回收率分别为98.34%和98.06%,RSD分别为1.02%和0.96%(n=6)。结论本测定方法简便、准确,稳定性、重复性好,适用于心动颗粒中阿魏酸和欧前胡素的含量测定。     

HPLC同时测定决明子配方颗粒中2种成分

目的建立高效液相色谱法(HPLC)同时测定决明子配方颗粒中橙黄决明素和大黄酚的含量。方法采用HPLC,采用C_(18)柱(150 mm×4.6 mm,5μm),以乙腈-甲醇-0.1%磷酸(49:7:44)为流动相,检测波长为222 nm,流速为1.0 ml/min,对决明子配方颗粒中橙黄决明素、大黄酚的含量进行测定。结果橙黄决明素和大黄酚分别在进样量为12.32～154 ng(r=0.999 99),10.48～131 ng(r=0.999 99)范围内与峰面积线性关系良好,平均回收率分别为99.88%,101.07%,RSD分别为0.75%,0.10%(n=6)。结论该方法简便、准确可靠、重现性好,可作为决明子配方颗粒的质量控制方法。     

胃康散质量标准研究

目的制定胃康散的质量标准。方法采用TLC对胃康散中的白及、延胡索、甘草进行定性鉴别;采用HPLC法测定胃康散中氯化两面针碱的含量:色谱柱为Agilent 5 TC-C_(18)(250 mm×4.6 mm,5μm),流动相为甲醇-0.1%磷酸(用N, N-二乙基乙胺调pH 6.0)(60:40),检测波长为273 nm,流速为1.0 ml/min,柱温为25℃,进样量为10μl。结果 TLC专属性强,分离度较好。氯化两面针碱在7.6～76.1μg/ml范围内浓度与峰面积呈良好的线性关系(r=0.9995),平均加样回收率为98.83%,RSD为2.5%(n=9),精密度、稳定性、重复性试验的RSD均小于3%。结论所建方法简单准确,专属性强,重复性好,可用于胃康散的质量标准控制。     

酸性染料比色法测定两面针药材总生物碱的含量

以氯化两面针碱为标样,采用溴麝香草酚蓝为酸性染料,在总生物碱与其形成稳定络合物时间范围内,利用比色法测定两面针药材中总生物碱的含量,测定波长为393nm。两面针总生物碱检测浓度在2.56～10.26μg/ml范围内线性关系良好(r=0.9997),平均回收率为101.00%(RSD=2.46%,n=6)。该法测定两面针总生物碱含量简便快捷,准确易行。     

芪精镇痛颗粒质量标准研究

目的建立芪精镇痛颗粒的质控方法。方法采用薄层色谱法(TLC)定性鉴别炙黄芪、升麻和炙甘草;采用高效液相色谱法(HPLC)同时测定阿魏酸和异阿魏酸的含量。结果 TLC斑点清晰,分离效果较好,且阴性无干扰。阿魏酸在40.4～808 ng(r=1.0000)范围内线性关系良好,异阿魏酸在40.8～816 ng(r=1.0000)范围内线性关系良好。两者的加样回收率分别为100.6%,100.8%,RSD分别为2.0%(n=6),1.7%(n=6)。结论本文建立的定性鉴别方法和含量测定方法,可用于检测芪精镇痛颗粒的质量。     

HPLC法同时测定旱芹中木犀草素和旱芹素的含量

建立HPLC法同时测定旱芹中木犀草素和旱芹素含量的方法。采用C1(8 150 mm×4.6 mm,5μm)柱,流动相为乙腈∶0.01 mol/L醋酸铵(pH=4.8)=40∶60,等强度洗脱,检测波长330 nm,柱温25℃,流速1.0 mL/min。木犀草素和旱芹素的质量浓度分别在0.93μg/mL~4.94μg/mL(r=0.999 1)及1.03μg/mL~5.06μg/mL(r=0.999 4)范围内与峰面积呈现良好的线性关系,平均加样回收率依次为99.7%(RSD为2.4%),99.0%(RSD为1.8%)。     

HPLC法测定黑豆皮中原儿茶酸、表儿茶素的含量

建立HPLC波长切换法同时测定黑豆皮中原儿茶酸、表儿茶素含量的方法。固定相为shim-pack VP-ODS C18(250 mm×4.6 mm,5μm),流动相为乙腈-0.1%磷酸溶液,流速为1.0 m L/min,检测波长为260、280 nm,柱温35℃。原儿茶酸、表儿茶素分别在0.010 52 mg/m L~1.052 mg/m L(r=0.999 6)和0.012 24 mg/m L~1.224 mg/m L(r=0.998 9)浓度范围内与峰面积呈良好的线性关系,平均回收率分别为99.46%(RSD=1.08%,n=6)和99.06%(RSD=1.02%,n=6)。     

高效液相色谱法测定南瓜果肉中胡芦巴碱含量

以脱脂南瓜粉为原料,70% 乙醇溶液为溶剂,微波辅助萃取样品中的胡芦巴碱,建立南瓜果肉中胡芦巴碱含量的高效液相色谱(HPLC)检测方法。实验过程中,采用的色谱柱为Agilent-ZORBX SB-C18(4.6mm × 150mm,5μm)柱,流动相为0.40mmol/L 磷酸溶液(pH3.2),流速为0.6mL/min,进样量为10μL,检测波长265nm,柱温为室温。研究结果表明,胡芦巴碱在5.6～134.4μg/mL 范围内具有良好的线性关系,相关系数r=0.9999(n=5);平均回收率为97.09%,RSD 为1.02%(n=5)。本法简便、准确、重复性好,可用于南瓜果肉中胡芦巴碱的含量测定。此外,采用此方法测定了13 个品种南瓜果肉中胡芦巴碱的含量,结果表明胡芦巴碱含量为172.5～475.5μg/g。     

HPLC法测定芹菜中绿原酸和芹菜苷的含量

建立芹菜中绿原酸和芹菜苷的HPLC测定方法。测定3个不同产地的芹菜叶和茎中的绿原酸和芹菜苷含量。采用Luna C18ODS柱(250 mm×4.6 mm,5μm);乙腈-1%乙酸溶液梯度洗脱;流速:1.0 m L/min;柱温:30℃;检测波长:330 nm。绿原酸和芹菜苷分别在0.51μg/m L~102μg/m L(R2=0.999 9)和0.505μg/m L~101μg/m L(R2=0.999 8)范围内线性关系良好,回收率分别为98.90%和97.83%,RSD分别为0.87%和0.39%。经测定芹菜中绿原酸和芹菜苷的含量分别在0.268 mg/g~1.712 mg/g和1.802 mg/g~63.870 mg/g之间。     

Textural Properties of Cold-set Gels Induced from Heat-denatured Whey Protein Isolates

A 9% whey protein (WP) isolate solution at pH 7.0 was heat-denatured at 80°C for 30 min. Size-exclusion HPLC showed that native WP formed soluble aggregates after heat-treatment. Additions of CaCl2 (10–40 mM), NaCl (50–400 mM) or glucono-delta-lactone (GDL, 0.4–2.0%, w/v) or hydrolysis by a protease from Bacillus licheniformis caused gelation of the denatured solution at 45°C. Textural parameters, hardness, adhesiveness, and cohesiveness of the gels so formed changed markedly with concentration of added salts or pH by added GDL. Maximum gel hardness occurred at 200 mM NaCl or pH 4.7. Increasing CaCl2 concentration continuously increased gel hardness. Generally, GDL-induced gels were harder than salt-induced gels, and much harder than the protease-induced gel.     

Occurrence of bisphenol-F-diglycidyl ether (BFDGE) in fish canned in oil

The levels of bisphenol-F-diglycidyl ether (BFDGE) were quantified as part of a European survey on the migration of residues of epoxy resins into oil from canned fish. The contents of BFDGE in cans, lids and fish collected from all 15 Member States of the European Union and Switzerland were analysed in 382 samples. Cans and lids were separately extracted with acetonitrile. The extraction from fish was carried out with hexane followed by re-extraction with acetonitrile. The analysis was performed by reverse phase HPL C with fluorescence detection. BFDGE could be detected in 12% of the fish, 24% of the cans and 18% of the lids. Only 3% of the fish contained BFDGE in concentrations considerably above 1mg/kg. In addition to the presented data, a comparison was made with the levels of BADGE (bisphenol-A-diglycidyl ether)analysed in the same products in the context of a previous study.     

Contribution of European research to risk analysis

The European Commission's, Quality of Life Research Programme, Key Action 1—Health, Food & Nutrition is mission-oriented and aims, amongst other things, at providing a healthy, safe and high-quality food supply leading to reinforced consumer confidence in the safety of European food. Its objectives also include the enhancing of the competitiveness of the European food supply. Key Action 1 is currently supporting a number of different types of European collaborative projects in the area of risk analysis. The objectives of these projects range from the development and validation of prevention strategies including the reduction of consumers risks; development and validation of new modelling approaches; harmonization of risk assessment principles, methodologies, and terminology; standardization of methods and systems used for the safety evaluation of transgenic food; providing of tools for the evaluation of human viral contamination of shellfish and quality control; new methodologies for assessing the potential of unintended effects of genetically modified (genetically modified) foods; development of a risk assessment model for Cryptosporidium parvum related to the food and water industries; to the development of a communication platform for genetically modified organism, producers, retailers, regulatory authorities and consumer groups to improve safety assessment procedures, risk management strategies and risk communication; development and validation of new methods for safety testing of transgenic food; evaluation of the safety and efficacy of iron supplementation in pregnant women; evaluation of the potential cancer-preventing activity of pro- and pre-biotic ('synbiotic') combinations in human volunteers. An overview of these projects is presented here.     

低温带皮菜籽粕微粉的不同粒级部分的功能特性

为研究低温带皮菜籽粕微粉的不同粒级部分的功能特性,以经低温脱脂的带皮菜籽粕为原料,经微粉碎后筛分成212~425μm、150~212μm和106~150μm的3个不同粒级的微粉样品,检测这些样品的吸水性、吸油性、乳化性和乳化稳定性、蛋白质体外消化率。结果表明:1 3个不同粒级的微粉样品之间的粗纤维含量存在显著差异,表明三者的结构组成成分有一定差异。23个微粉样品的乳化活性和乳化稳定性随粒度级别的减小而显著增加(P0.01)。33个微粉样品的蛋白质体外消化率随粒度级别的减小而显著增加(P0.01)。4不同粒级带皮菜籽粕微粉样品的吸水性与吸油性受其结构组成物质不同和粒度的双重影响,与粒度的相关性不明显。     

Microbiology of food taints

Fresh and processed foods are often spoilt by the presence of undesirable flavours and odours caused by microbial action. The aim of this paper is to review the current knowledge of microbiologically induced taints that occur in a wide range of foodstuffs, including meats, poultry, fish, crustaceans, milk, dairy products, fruits, vegetables, cereals and cereal products. Examples have been chosen where the compounds responsible for the taint have been identified and sufficient data obtained to demonstrate the involvement of microorganisms. However, in some cases the full identity of the causative organism may not have been elucidated. The types of microorganisms covered by this review include bacteria, fungi, yeasts, actinomycetes and cyanobacteria. Although cyanobacteria do not in general infect foods, their presence in aqueous systems and water supplies can lead to off-flavours in aquatic organisms and processed foodstuffs. Several examples of each of these processes are discussed. Wherever possible, the likely biosynthetic pathway used by the microorganism to produce the offending compound in a foodstuff is indicated.     

Analysis for organic residues from aids to polymerization used to make plastics intended for food contact

Polymers intended for food contact use have been analysed for organic residues which could be attributed to a range of substances employed as polymerization aids (e.g. initiators and catalysts). A wide range of polymers was extracted with solvents and the extracts analysed by gas chromatography-mass spectrometry (GC-MS). The overwhelming majority of substances identified were not derived from aids to polymerization but were oligomers, additives and adventitious contaminants. However, a small number of substances were identified as initiator residues. These included tetramethylsuccinonitrile (TMSN) which was observed in two polymers and it derived from recombination of two azobisisobutyronitrile (AIBN) initiator radicals. Methyl benzoate, benzoic acid, biphenyl and phenyl benzoate were detected in one poly(methyl methacrylate) sample and in two polyvinylchlorides and they are thought to be derived from benzoyl peroxide initiator. TMSN was subsequently targeted for analysis of poly-(methyl methacrylate) plastics using proton nuclear magnetic resonance spectrometry (¹     

Tests of potential functional barriers for laminated multilayer food packages. Part II: Medium molecular weight permeants

Experiments were performed to characterize the kinetics of the permeation of different medium molecular weight model permeants: bisphenol A, warfarin and anthracene, from liquid paraffin, through a surrogate potential functional barrier (25 microns-thick orientated polypropylene--OPP) into the food simulants olive oil and 3% (w/v) acetic acid. The characterization of permeation kinetics generally observed the permeation models previously reported to explain the experimental permeation results obtained for a low molecular weight group of model permeants. In general, the model permeants exhibited behaviour consistent with their relative molecular weights with respect to (a) the time taken to attain steady-state permeation into the food simulant in which they were more soluble, (b) their subsequent steady-state permeation rates, and (c) their partition between liquid paraffin and the OPP membrane.     

The development of reference materials for paralytic shellfish poisoning toxins in lyophilized mussel. I: Interlaboratory studies of methods of analysis

This paper describes the first part of a project undertaken to develop mussel reference materials for Paralytic Shellfish Poisoning (PSP) toxins. Two interlaboratory studies were undertaken to investigate the performance of the analytical methodology for several PSP toxins, in particular saxitoxin (STX) and decarbamoyl-saxitoxin (dc-STX) in lyophilized mussels, and to set criteria for the acceptance of results to be applied during the second part of the project: the certification exercise. In the first study, 18 laboratories were asked to measure STX and dc-STX in rehydrated lyophilized mussel material and to identify as many other PSP toxins as possible with a method of their choice. In the second interlaboratory study, 15 laboratories were additionally asked to determine quantitatively STX and dc-STX in rehydrated lyophilized mussel and in a saxitoxin-enriched mussel material. The first study revealed that three out of four postcolumn derivatization methods and one pre-column derivatization method sufficed in principle to determine STX and dc-STX. Most participants (13 of 18) obtained acceptable calibration curves and recoveries. Saxitoxin was hardly detected in the rehydrated lyophilized mussels and results obtained for dc-STX yielded a CV of 58% at a mass fraction of 1.86 mg/kg. Most participants (14 out of 18) identified gonyautoxin-5 (GTX-5) in a hydrolysed extract provided. The first study led to provisional criteria for linearity, recovery and separation. The second study revealed that 6 out of 15 laboratories were able to meet these criteria. Results obtained for dc-STX yielded a CV of 19% at a mass fraction of 3.49mg/kg. Results obtained for STX in the saxitoxin-enriched material yielded a CV of 19% at a mass fraction of 0.34mg/kg. Saxitoxin could not be detected in the PSP-positive material. Hydrolysis was useful to confirm the identity of GTX5 and provided indicative information about C1 and C2 toxins in the PSP-positive material. The methods used in the second interlaboratory study showed sufficiently consistent analysis results to undertake a certification exercise to assign certified values for STX and dc-STX in lyophilized mussel.     

The Ministry of Environmental Protection Issued "Feasible Technology Guidelines for Pollution Prevention and Control in Wood Pulping Process of the Paper Industry (Trial)" and Two Other Guiding Technical Documents

On December 27t＂, 2013, the Ministry of Environmenta Protection announced that, in order to implement ＂The Environmental Protection Law of the People＇ s Republic of China＂, improve the working system in environmenta protection technologies, and promote technologica advancement in pollution prevention, the Ministry of Environmental Protection sponsored the formulation of three guiding technical documents including ＂Feasible Technology Guidelines for Pollution Prevention and Contro n Wood Pulping Process of the Paper Industry （Trial）＂     

1~(st) Intelli-Tissue~ EcoEc Tissue Machine Supplied by PMP Group Successfully Put into Operation in China

正On April 29th,2014,Intelli-Tissue EcoEc tissue machine supplied by PMP Group successfully put into operation at Hebei Xuesong Paper Co.,Ltd.,this is the first such kind of paper machine of PMP Group in China.