Study of Membrane Separation Technology in Nucleotide and Dairy Production

膜分离技术是一门新型的高效分离、浓缩、提纯及净化技术，近三十年来已广泛应用于传统生产工艺的改造升级。本文主要研究了膜技术在核苷酸和乳品生产中的应用。膜技术在核苷酸的应用研究中，我们首次研究了组合膜技术（超滤＋纳滤）改造核苷酸的传统生产工艺。首先考察了5种不同截留分子量和亲疏水性的Ultra-floTM超滤膜过滤RNA酶解液的效果。结果表明，截留分子量越大、亲水性越强的超滤膜所对应的平均膜通量越大；截留分子量越小、疏水性越强的超滤膜所对应的蛋白截留率越大；截留分子量越小、亲水性越强的超滤膜所对应的膜污染越小、膜清洗越容易。其中，亲水强、截留分子量适中的3＃超滤膜（MWCO30kD，CA）同时兼具...Membrane separation technique belongs to a new high-efficiency technology for separation, concentration and purification. Membrane technique has been extensively used to reform and upgrade the conventional processes in the past thirty years. In this study, membrane application in the production of nucleotide and dairy was explored. In the first part of this thesis, the integrated membrane techniqu...学位：理学硕士院系专业：化学化工学院材料科学系_高分子化学与物理学号：20023600

Research progress of integrated membrane process on high-value development of fish processing by-products

集成膜工艺不仅可以发挥各种膜过程的优势,而且利用集成的协同作用,能够更高效地解决水产加工副产物高值化开发中的分离纯化难题,同时具有节能、低耗、清洁等优点。文章分析了集成膜工艺在水产加工副产物高值化开发中的典型应用,并探讨了实现集成膜工艺产业化应用的关键环节。Integrated membrane process,making use of both individual and synergic advantages of membrane operations,provided more effective separation solution for high-value development of fish processing by-products and had merits of energy saving,low consumption,clean production and so on.Reviewed the typical applications of integrated membrane process on high-value development of fish processing by-products,further discussed the key issues of achieving the industrial application of integrated membrane process.福建省海洋与渔业厅重点项目(闽海渔合同[2010]2-21号);厦门海洋研究开发院项目(K11102

基于二维石墨烯纳米材料优化高分子分离膜的研究进展

高分子分离膜在渗透性与选择性之间一直存在此长彼消的trade-off效应,且抗污染性能、化学稳定性能也亟待提升。有机-无机杂化膜能综合有机高分子材料和无机材料的优点,近年来,纳米材料的快速发展对于传统高分子膜材料具有重要的推动作用,尤其是基于二维石墨烯纳米材料开发新型复合分离膜成为备受关注的研究热点。然而,石墨烯化学稳定性高,其表面呈惰性状态,与其它介质的相互作用较弱,且石墨烯片层之间存在较强的范德华力,易聚集而难溶于水及膜溶剂,严重阻碍了其在高分子分离膜材料中的应用。氧化石墨烯(GO)在其表面和边缘引入了大量含氧极性基团,有助于摆脱了片层间强大的π-π堆积相互作用力,因此,GO在水及膜溶剂中具有良好分散性能;同时,大量的含氧基团也为设计与制备改性石墨烯提供了丰富的反应位点;此外,GO还具有可规模化制备、成本较低的优点,使得GO在高分子分离膜材料中的应用备受青睐。针对聚偏氟乙烯、聚砜与聚醚砜等常用膜材料疏水性强、易污染的缺点,将它们分别与GO、改性GO、或复合纳米材料等共混,通过浸没沉淀相转化法制备混合基质膜,可以有效改善混合基质膜的亲水性、膜孔结构、膜表面粗糙度、荷电性能等,从而提升混合基质膜的渗透性能与抗污染性能,甚至赋予抑菌等新功能。在聚酰胺复合膜的超薄分离层或多孔支撑层中引入适量的GO或改性GO,通过增强超薄分离层的亲水性能、荷电性能以及优化超薄分离层的结构,从而提升纳米复合膜的选择渗透性能、抗污染性能以及耐氯性能。此外,利用GO的静电、氢键、范德华力、π-π等非共价键相互作用力,或者利用GO活性位点与交联剂反应实现共价键连接,可以通过层层组装法制备水平取向、高效堆叠的高通量GO层状膜。本文归纳了基于物理共混、界面聚合、层层组装等常用制膜方法,将二维石墨烯纳米材料填充、交联、吸附、沉积而负载或包裹在高分子膜基质中,实现改善与优化高分子分离膜结构与性能的应用研究进展,并对二维石墨烯纳米材料在高分子分离膜的工业化应用所面临的挑战和应用前景进行了展望。厦门市产学研协同创新及科技合作项目(3502Z20172008);;海洋三所基本科研业务费专项资金资助项目(2016036);;厦门海洋高技术产业基地创业创新共享服务平台项目(16PFW008SF15);;海洋中试技术研发与检测公共服务平台建设(Bhsfs009);;厦门大学校长基金(No.20720170027

基于二维石墨烯纳米材料优化高分子分离膜的研究进展

高分子分离膜的渗透性与选择性之间存在此长彼消的Trade-off效应,且其抗污染性能、化学稳定性能也亟待提升。有机-无机杂化膜综合了有机高分子材料和无机材料的优点。近年来,纳米材料的快速发展对传统高分子膜材料具有重要的推动作用,尤其是基于二维石墨烯纳米材料开发的新型复合分离膜成为备受关注的研究热点。然而,石墨烯化学稳定性高,其表面呈惰性状态,与其他介质的相互作用较弱,且石墨烯片层之间存在较强的范德华力,易聚集而难溶于水及膜溶剂,严重阻碍了其在高分子分离膜材料中的应用。氧化石墨烯(GO)在石墨烯的表面和边缘引入了大量的含氧极性基团,有助于摆脱片层间强大的π-π堆积相互作用力,因此,GO在水及膜溶剂中具有良好的分散性能;同时,大量的含氧基团也为设计与制备改性石墨烯提供了丰富的反应位点;此外,GO还具有可规模化制备、成本较低的优点,使得GO在高分子分离膜材料中的应用备受青睐。针对聚偏氟乙烯、聚砜与聚醚砜等常用膜材料疏水性强、易污染的缺点,将它们分别与GO、改性GO或复合纳米材料等共混,通过浸没沉淀相转化法制备混合基质膜,可以有效改善混合基质膜的亲水性、膜孔结构、膜表面粗糙度、荷电性能等,从而提升混合基质膜的渗透性能与抗污染性能,甚至赋予其抑菌等新功能。在聚酰胺复合膜的超薄分离层或多孔支撑层中引入适量的GO或改性GO,通过增强超薄分离层的亲水性能、荷电性能以及优化超薄分离层的结构,从而提升纳米复合膜的选择渗透性能、抗污染性能以及耐氯性能。此外,利用GO的静电、氢键、范德华力、π-π等非共价键相互作用力,或者利用GO活性位点与交联剂反应实现共价键连接,可以通过层层组装法制备水平取向、高效堆叠的高通量GO层状膜。本文归纳了基于物理共混、界面聚合、层层组装等常用制膜方法,将二维石墨烯纳米材料填充、交联、吸附、沉积,从而负载或包裹在高分子膜基质中,实现改善与优化高分子分离膜结构与性能的应用研究进展,并对二维石墨烯纳米材料在高分子分离膜的工业化应用中所面临的挑战和前景进行了展望。厦门市产学研协同创新及科技合作项目(3502Z20172008);;\n海洋三所基本科研业务费专项资金(2016036);;\n厦门海洋高技术产业基地创业创新共享服务平台项目(16PFW008SF15);;\n海洋中试技术研发与检测公共服务平台建设(Bhsfs009);;\n厦门大学校长基金(20720170027)~

Development of Squalene Certified Reference Material

为研制角鲨烯国家标准样品。以角鲨烯粗品为原料,制备高纯角鲨烯,采用红外光谱、高分辨质谱和核磁共振谱进行结构确证。样品分装成150瓶后,采用气相色谱-氢火焰离子化检测器法进行均匀性、稳定性检验和定值分析。从样品中随机抽取15瓶进行均匀性检验,经f检验表明在95%置信区间范围内样品均匀性良好;稳定性考察按照-18℃长期实验稳定性(24个月)进行,结果表明在考察期间内样品稳定性良好;标准样品经国内8家具有分析资质的实验室进行协同定值,并评定了定值结果的不确定度,角鲨烯标准样品定值结果为99.57%,相对扩展不确定度为0.30%(k=1.96)。该标准样品达到国家标准样品的技术要求,可用于有关角鲨烯的方法校正和质量控制。Squalene certified reference material was developed by purification of crude squalene.The structure of the certified reference material was confirmed by infrared spectroscopy(IR), high resolution mass spectrometry(HRMS) and nuclear magnetic resonance(NRM) and squalene was divided into 150 aliquots.The homogeneity and stability tests and quantitative analysis were carried out by gas chromatography-flame ionization detection(GC-FID).Fifteen randomly selected aliquots showed good homogeneity as indicated by F-test analysis at a 95% confidence interval.The test samples were stable at-18 ℃ for 24 months.A cooperative certification was conducted with 8 qualified laboratories.The certified purity value of the reference material was 99.57% with a relatively expanded uncertainty of 0.30%(k = 1.96).The reference material can conform to the technical requirement of the certified reference material.This material was intended for use in the method validation and quality control regarding squalene.厦门海洋研究开发院共建项目(2014); 海洋生物技术产业化中试技术研发公共服务平台项目(12PZP001SF10); 广东海洋经济发展区域示范项目(GD2012-D01-001

Development of Anhydrotetrodotoxin Certifi ed Reference Material

研制4,9-脱水河豚毒素国家标准样品。以河豚鱼卵巢为原料,提取制备4,9-脱水河豚毒素,采用红外光谱(Ir)、高分辨质谱和核磁共振谱(nMr)进行结构确证。样品分装成140瓶后,采用柱后衍生–高效液相荧光法进行均匀性、稳定性检验和定值分析。从样品中随机抽取15瓶进行均匀性检验,经f检验表明在95%的置信区间范围内样品均匀性良好;稳定性考察按照40℃加速试验稳定性(6个月)进行,结果表明在考察期间内样品稳定性良好;标准样品经国内8家具有分析资质的实验室进行协同定值,并评定了定值结果的不确定度,4,9-脱水河豚毒素标准样品定值结果为97.77%,相对扩展不确定度为0.4%(k=1.96)。该标准样品达到国家标准样品的技术要求,可用于有关脱水河豚毒素的方法校正和质量控制。4,9-anhydrotetrodotoxin certified reference material was developed.4,9-anhydrotetrodotoxin was made from the ovarium of pufferfish.The structure of anhydrotetrodotoxin certified reference material was comfirmed by mass spectrometry and NRM,infrared spectroscopy(IR).4,9-anhydrotetrodotoxin was divided into 140 bottles.The homogeneity and stability testing and quantitative analysis were evaluated by post column derivation high performance liquid chromatography–fl uorescent detection(HPLC–FLD) method.According to analysis procedure of homogeneity,15 bottles of sample were randomly taken from 140 bottles,and the results were validated by F-test statistical method.The stability inspection was carried on the short-term(6 months),and the results indicated that the period for anhydrotetrodotoxin of storage was 6 months at 40℃.A cooperative certifi cation was conducted with 8 qualifi ed laboratories.The certifi ed purity value of the reference material of 4,9-anhydrotetrodotoxin was 97.77% with relative expaned uncertainty of 0.40%(k=1.96).The reference material can conform to the technical requirement of the certified reference material.The material was intended for use in the method validation and quality control regarding anhydrontetrodotoxin.广东海洋经济发展区域示范项目(GD2012-D01-001); 海洋生物产业化中试技术研发公共服务平台(12PZP001SF10); 厦门市重大科技创新平台项目(3502Z20111001); 国家科技支撑计划(NO.2011BAK04B09

柱前衍生化高效液相色谱法测定2-去氧葡萄糖的含量

目的建立柱前衍生化高效液相色谱法测定2-去氧葡萄糖(2-DG)含量的方法。方法采用1-苯基-3-甲基-5-吡唑酮(PMP)为柱前衍生化试剂,将2-DG在碱性条件下衍生化后直接进样测定。分离柱为HypersilODS2色谱柱(4.6 mm×250 mm,5μm),流动相为100 mmol·L-1醋酸铵缓冲液(pH 5.5)-乙腈(78∶22),流速1.0 mL·min-1,波长249 nm。结果 2-DG在19.68~393.6μg·mL-1浓度范围内与峰面积具有良好的线性关系(r=0.9997);其定量限(S/N=10)和最低检出限(S/N=3)分别为7.8和3.1 ng;平均回收率为101.21%,RSD 0.63%。结论该方法简便实用、检测灵敏度高、测定结果准确,适用于2-DG的质量控制

Process in Antimicrobial Mechanisms of Graphene Oxide

石墨烯自2004年被发现以来便引起全世界广泛关注。由于其热力学、电学和机械强度等方面的特性,在电子、物理、信息、能源和材料领域一直有广泛的应用前景。氧化石墨烯(graphene oxide,GO)作为石墨烯的衍生物,是一种尺寸可调节的新型纳米材料。GO有着独特的生物化学特性,近年来在抗菌方面的研究一直有被报道。其抗菌机理有很多不同版本的研究报道,但对于其真正的抗菌机理一直未被阐述清楚,且存在争议。本文综述及回顾了近年对于GO抗菌机理的不同描述,包括物理破坏理论(包括边缘切割和机械包裹)、过氧化作用理论和磷脂分子抽提破坏理论,并对未来机理研究作了展望。Graphene had attracted worldwide attention since its discovery in 2004. Its electrical, thermodynamical, mechanical and other aspects of the characteristics made it possible to apply in a wide range of fields included electronics, physics, information, energy, materials and etc. Graphene oxide(GO), as one of the derivatives of graphene, was a new nanomaterial with adjustable size. GO has unique biochemical characters, and had been reported to be a good antimicrobial materials in many different researches. Though some antibacterial mechanisms of GO had been reported, the truth was still vague and some were even controversial. So this review just focued on different antimicrobial mechanisms of GO in the past few years, included physical damage theories(edge cutting and mechanical wrapping), oxidative stress theory, and molecular extraction and damage theory. In the end, there was a prospect for the future in this area.国家自然科学基金(21406185);; 福建省科技计划重点项目(2014H0017);; 国家海洋局第三海洋研究所基本科研业务费专项资金资助项目(2013015

Application of membrane separation technology in pharmaceutical industry

［中文文摘］膜分离技术在制药工业中的应用包括生物发酵制药、中药生产和现代生物技术等 .膜分离技术在抗生素、半合成抗生素、维生素和氨基酸生产中尤其常见 .随着膜材料、膜组件和膜设备的不断改进 ,膜分离技术在制药工业中将扮演越来越重要角色。［英文文摘］The application of membrane separation technology in pharmaceutical industry includes biofermentation pharmaceutical industry,the production of Chinese traditional medicine,the modern biotechnology etc.Membrane separation technology is especially common in the production of antibiotics,semisynthetic antibiotics,vitamin and amino acid.With the improvement of membrane material,membrane module and membrane plant,membrane separation technology will play a more and more important role in the pharmaceutical industry.福建省科技重点项目;教育部科技重点项目;福建省青年科技人才创新项目资助课题

Detection of 2-Deoxyglucose by Pre-column Derivation Reversed Phase High Performance Liquid Chromatography

采用对氨基苯甲酸乙酯为衍生化试剂,建立柱前衍生化反相高效液相色谱法(rP-HPlC)测定2-去氧葡萄糖的含量。结果表明,最适的衍生化条件为反应温度85℃,反应时间1.5H,衍生化试剂(AbEE)和单糖(2-dg/glu)的摩尔比为25∶1;色谱条件为色谱柱HyPErSIl OdS2(250MMx4.6MM,5μM),流动相为0.02%TfA-乙腈(80∶20,V/V),流速1.0Ml/MIn,波长307nM。本方法在1~700Mg/l浓度范围内与峰面积呈良好的线性关系(r=0.9999);定量限(S/n=10)及检出限(S/n=3)分别为450和100μg/l;平均加标回收率为101.7%;rSd为0.7%;日内及日间精密度均小于0.7%。表明本方法灵敏度高,测定结果准确,重复性好,可用于2-去氧葡萄糖样品的准确定量分析。A method was developed for the determination of 2-deoxyglucose(2-DG)by reversed phase high performance liquid chromatography(RP-HPLC) after pre-column derivated with p-aminobenzoic ethyl ester(ABEE).The results showed that the optimum derivation conditions were as follows: reaction temperature was 85 ℃,reaction time was 1.5 h and molar ratio of derivative reagent(ABEE) to monosaccharide(2-DG/Glu) was 25∶1.The derivative was analyzed on a Hypersil ODS 2(250 mm×4.6 mm,5 μ) column with a mixture of acetonitrile to 0.02% trifluoroacetic acid(TFA)(2∶80,V/V) as the mobile phase,at the flow rate of 1.0 mL/min and the detection wavelength at 307 nm.This method has a good linearity at the concentration from 1 mg/L to 700 mg/L(r=0.9999).The limit of detection was 100 μg/L while the quantitative limit was 450 μg/L.The average recovery of 2-DG was 101.7% and the relative standard deviation(RSD) was 0.7%.The inter-day and intra-day precision were both less than 0.7%,This method is of high sensitivity,precision and repetition,indicating that it is suitable for precise quantitative determination of 2-DG.海洋公益性行业科研专项经费基金(No.201005020);福建省科技重大专项经费基金(No.2010NZ0001-2);厦门市海洋与渔业局科技计划项目经费基金(厦海渔合[2010]9号)资助项