HPLC法测定复方保健酒中人参皂苷和西红花苷的含量

采用高效液相色谱仪建立测定复方保健酒中人参皂苷Rg1、人参皂苷Rb1、人参皂苷Rb2、人参皂苷Rc、西红花苷I、西红花苷II含量的方法。结果表明,最佳测定条件为采用Agilent SB-Aq色谱柱（4.6 mm×250 mm,5 μm）,以乙腈-水为流动相梯度洗脱,流速1.0 mL/min,柱温30 ℃,人参皂苷的检测波长203 nm,西红花苷的检测波长为440 nm,进样量10 μL。人参皂苷Rg1、人参皂苷Rb1、人参皂苷Rb2、人参皂苷Rc、西红花苷I、西红花苷II在各自浓度范围内线性关系良好（R≥0.999 9）,平均加标回收率97.83%～101.72%,精密度试验结果相对标准偏差（RSD）0.43%～1.85%。实验结果表明该方法操作简单,精密度和准确度高,重复性好,可用于复方保健酒中人参皂苷和西红花苷含量测定。     

HPLC法同时检测复方产品中西洋参、红景天和刺五加的皂苷含量

采用高效液相色谱法建立了同时检测复方产品中人参皂苷Rb1、人参皂苷Re、红景天苷、刺五加苷B和刺五加苷E含量的方法。以60%乙醇作为提取溶剂,用色谱柱Kromasil 100-5C18(250×4.6mm,5μm)进行分离,以0.1%磷酸-乙腈混合液为流动相进行梯度洗脱,结果表明,在此条件下5种皂苷得到了良好的分离。人参皂苷Rb1、人参皂苷Re、红景天苷、刺五加苷B和刺五加苷E分别在80~800、80~800、40~400、20~160μg/m L和40~320μg/m L范围内呈现良好的线性关系,平均加标回收率在99.5%~106.8%之间,相对标准偏差为0.5%~2.3%。本方法具有重现性好、回收率高等优点,适用于复方产品中人参皂苷Rb1、人参皂苷Re、红景天苷、刺五加苷B和刺五加苷E的同时检测。     

酸水解法测定保健酒中的总皂苷含量

为了开发测定保健酒中总皂苷含量更准确的分析方法,将保健酒中皂苷用反相固相萃取法从酒体中分离出来;所得的皂苷提取物用酸水解后,再用溶剂萃取得到苷元;最后用香草醛-硫酸比色法,以人参皂苷Re为标准,测定总苷元含量。结果表明,人参皂苷元(Re)在6.8~91μg/mL范围线性关系良好,y=0.011x+0.012(R~2=0.999),平均加标回收率为99.15%,RSD值为1.91%,精密度、重复性良好。皂苷经水解后消除了糖基对香草醛显色剂的干扰,提取苷元过程采用液液萃取的方式可将保健酒A中的色素完全除去。方法稳定,可作为保健酒中总皂苷的检测及其活性中药成分含量的质量控制的检测方法。     

双刺参胶囊中紫丁香苷及人参皂苷Rg1、Re、Rb1的含量测定

建立双刺参胶囊中紫丁香苷及人参皂苷Rg₁、Re、Rb₁的高效液相色谱法(HPLC)含量测定方法。分别采用依利特APS和Nano-Micro UniSil 5-120 C₁₈色谱柱,以乙腈-水为流动相,梯度洗脱,流速1.0 mL/min,进样量10 μL,人参皂苷Rg₁、人参皂苷Re及人参皂苷Rb₁在柱温35 ℃、波长203 nm下,紫丁香苷在柱温30 ℃、波长265 nm下进行检测。结果表明:人参皂苷Rg₁、人参皂苷Re、人参皂苷Rb₁及紫丁香苷分别在15.30~306.00 μg/mL(R2=0.9999)、16.95~339.00 μg/mL(R2=1.0000)、18.45~369.00 μg/mL(R2=1.0000)和4.60~46.00 μg/mL(R2=0.9999)范围内呈现良好的线性关系,其检出限分别为0.77、0.89、0.93、0.12 μg/mL;其定量限分别为2.21、2.71、2.74、0.38 μg/mL。其精密度实验的RSD值分别为1.30%、1.21%、1.99%、0.79%;其重复性实验的RSD值分别为2.49%、2.35%、2.55%、0.80%;其平均加样回收率分别为100.13%、100.50%、102.33%、101.55%,其RSD值分别为0.67%、0.99%、0.29%、0.68%。实验结果表明供试品溶液在48 h内稳定,该方法专属性高、重复性好,可用于双刺参胶囊中紫丁香苷及人参皂苷Rg₁、人参皂苷Re、人参皂苷Rb₁的含量测定。本实验为双刺参胶囊的质量标准制定提供了基础数据。     

3种拟青霉发酵三七及其产物检测

采用3种拟青霉:蝙蝠蛾拟青霉(Paecilomyces hepiali)、蛹草拟青霉(Paecilomyces militaris)和蝉拟青霉(Paecilomyces cicadae)分别发酵三七药材,并检测发酵产物的功效成分。结果显示,蝙蝠蛾拟青霉和蛹草拟青霉能有效地将人参皂苷Rb1转化为Rd,从而高产稀有人参皂苷Rd,同时合成甘露醇、虫草素和腺苷。表明药用微生物与植物药相互作用可获得丰富的、新的药用资源。     

气相色谱-质谱联用法和高效液相色谱法测定4种人参酒中的皂苷和挥发性成分

目的 探究不同种人参醇提物中皂苷和挥发性成分的差异。方法 将四种参粉碎后用乙醇浸泡后,经顶空固相微萃取 (Headspace solid phase microextraction)结合气相色谱-质谱联用法（Gas chromatography-mass spectrometry）测定其挥发性成分,再用高效液相色谱法（High performance liquid chromatography）测定其皂苷成分。结果 分别在红参、西洋参、鲜参和生晒参酒中检测出39种、28种、39种和28种挥发性成分,其中白菖烯、(E)-β-金合欢烯、表蓝桉醇为共有的挥发性成分,倍半萜类化合物是人参酒的主要化合物,相对含量分别为42.3%、37.71%、46.25%和54.68%;分别在红参、西洋参、鲜参和生晒参酒分别检测出11种、9种、13种和9种皂苷,其中Rg3仅在红参酒中检测出。结论 4种参酒中的皂苷种类和挥发性成分均有差异,红参酒和鲜参酒呈现出更多种类的皂苷和挥发性成分。     

[1]保加利亚乳杆菌发酵转化人参皂苷工艺研究

摘 要: 目的 以人参为原料, 通过保加利亚乳杆菌发酵提高人参皂苷含量。方法 利用单因素试验和响应面法优化发酵工艺, 并对发酵过程中原型人参皂苷生物转化可能途径进行分析。结果 在发酵培养基为MRS液体培养基的前提下, 最适发酵条件为发酵温度40℃, 发酵时间3 d, 接种量3%, 转化稀有人参皂苷含量在150 μg/mL。经对比发现, 原参中检测出Re、Rg1、Rb1、Rc、Rb2、Rd、Rh1 7种皂苷, 经过发酵后的人参中检测出Re、Rg1、Rb1、Rc、Rb2、Rh1、Rd、R-rg3、CK 9种皂苷。同时原参中的常规皂苷含量经发酵后有所下降, 稀有皂苷含量有所增加, 且多酚、黄酮含量增加, 总糖含量减少, 发酵过程中人参皂苷生物转化的可能途径与人参皂苷含量变化趋势一致。结论 保加利亚乳杆菌发酵人参能够有效将原型皂苷转化成稀有人参皂苷, 为人参的深加工奠定基础, 为人参发酵产品的开发和利用提供参考。     

基于UPLC一测多评法测定西洋参及其保健食品中人参皂苷的含量

目的基于超高效液相色谱法(UPLC)建立西洋参药材及其保健食品中皂苷类成分的一测多评法(QAMS),对人参皂苷的含量进行快速、准确的测定,并比较一测多评法与外标法实测值的差异,进而判断一测多评法的适用性。方法采用UPLC,色谱柱为Acquity UPLC BEH C18柱(50 mm×2.1 mm,1.7μm);流动相A为乙腈,流动性B为水,梯度洗脱:流速为0.3 ml/min;柱温30℃;检测波长203 nm;以人参皂苷Rb1为内参物,建立该成分与人参皂苷Re、Rg1、Rb2、Rb3、Rc、Rd的相对校正因子,进而测定样品中各人参皂苷的含量。结果以Rb1为内参物,人参皂苷Rg1、Re、Rc、Rb2、Rb3、Rd的相对校正因子分别为1.084,0.869,0.972,1.044,1.010,1.261。在测定范围内各成分呈良好的线性关系(r≥0.999),平均回收率位于87.6%~99.7%之间,RSD均小于3.0%,并在不同的耐用性条件下方法适用性良好。对21批西洋参药材、饮片及5批西洋参类保健食品同时采用QAMS和外标法测定皂苷成分的含量,结果表明两种方法无显著性差异。结论本文建立的基于UPLC的一测多评法具有较高的选择性,分析时间短,耐用性较强,适用于西洋参药材及其保健食品中7种人参皂苷成分的含量测定。     

不同产地竹节参中7种皂苷含量测定及化学计量学评价

目的：建立UPLC法同时测定竹节参中7种皂苷含量,并结合化学计量学分析评价其质量。方法：采用ACQUITYUPLCBEHC18色谱柱(2.1mm×100mm,1.7μm),流动相为水(A)—乙腈(B),梯度淋洗;流速0.4mL/min,温度30℃,进样体积1μL,检测波长203nm。应用化学计量学中聚类分析、主成分分析及质量波动分析对含量测定结果进行识别,以分析不同产地竹节参药材间相似性及差异性。结果：7种皂苷(人参皂苷Rg1、人参皂苷Re、人参皂苷Rb1、竹节参皂苷Ⅴ、竹节参皂苷Ⅳ、竹节参皂苷Ⅳa与假人参皂苷RT1)在核定范围内线性关系良好(R2≥0.9994);平均加样回收率在99.00%~104.37%;人参皂苷Rg1、人参皂苷Re、人参皂苷Rb1、竹节参皂苷Ⅴ、竹节参皂苷Ⅳ、竹节参皂苷Ⅳa与假人参皂苷RT1的含量范围分别为0.21~18.85,0.59~2.82,1.25~8.12,59.14~97.16,22.21~47.19,15.97~32.66,0.07~34.09mg/g。通过聚类分析和主成分分析可将9批竹节参样品分为3类,竹节参样品S6为Ⅰ类,S3、S7和S8为Ⅱ类,S1、S2、S4、S5和S9为Ⅲ类;通过质量波动分析发现人参皂苷Rg1与假人参皂苷RT1含量波动大。结论：竹节参中7种皂苷成分含量同时测定的UPLC法及化学计量学综合评价可用于竹节参的质量评价。     

HPLC法测定8个不同产地绞股蓝中4种人参皂苷类成分的含量

高效液相色谱(high performance liquid chromatography,HPLC)法比较不同产地绞股蓝中人参皂苷Rb1、Rb3、Rc、Rd的含量。采用Sun Fire~(TM)-C_(18)(250 mm×4.6 mm,5.0μm)色谱柱,流动相为乙腈-水,梯度洗脱,流速0.8 mL/min,检测波长203 nm,柱温25℃。结果表明内蒙古产的绞股蓝中人参皂苷Rb1含量最大,江西产的绞股蓝中人参皂苷Rb3含量最大,湖北产的绞股蓝中人参皂苷Rc含量最大,江西产的绞股蓝中人参皂苷Rd含量最大,广东和江西产的绞股蓝中4种人参皂苷在成分和含量上都较为占优势。该方法简便、稳定、可行,不同产地绞股蓝中人参皂苷在成分和含量上存在差异,该结果为今后绞股蓝的开发利用和深入研究提供一定的参考。     

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.