Study on the stability of glucosamine sulfate prepared by spray drying

目的硫酸氨基葡萄糖喷雾干燥后稳定性试验。方法采用喷雾干燥法制得微囊化硫酸氨基葡萄糖,以产品得率、流动性、玻璃转化温度和贮藏稳定性为指标,考察不同配料的不同添加量对产品稳定性的影响。结果分别添加0.5%、1.0%、2.0%、3.0%和5.0%的环糊精、明胶、共聚维酮能有效地改善硫酸氨基葡萄糖的喷雾干燥粉末得率、粉末流动性,提高产品的贮藏稳定性和玻璃化转变温度结论环糊精、明胶、共聚维酮能有效提高硫酸氨基葡萄糖的稳定性。Objective To study the stability of glucosamine sulfate prepared by spray drying.Methods The microcapsules of glucosamine sulfate were produced by spray drying,and the effects of different adjuvants on the indices of the microcapsules,such as the yield,fluidity,glass transition temperature and store stability were compared.Results and conclusion The yield,fluidity,glass transition temperature and stability of glucosamine sulfate could be greatly improved by adding 0.5%,1.0%,2.0%,3.0% and 5.0% cyclodextrin,gelatin and copvidone.福建省自然科学基金计划资助项目(No.U0750010

基于枯草芽孢杆菌重组菌株构建技术制备海洋源金属硫蛋白

为构建安全高效表达海洋源金属硫蛋白的益生菌重组菌株,以海洋源褶牡蛎内脏团为模板,PCR克隆得到褶牡蛎金属硫蛋白基因(Op-MT),大小为324 bp,经pMD19-T载体亚克隆到融合表达载体pHT43-SUMO中,然后通过电转化法将重组质粒转入八种蛋白酶缺陷的宿主枯草芽孢杆菌(Bacillus subtilis)WB800N中。SDS-PAGE电泳显示诱导表达的融合蛋白SUMO-Op-MT分子量约为23 kD,与预期一致,说明可溶性融合蛋白SUMO-Op-MT在宿主菌中得到了表达,且通过Western blotting进一步得到验证。同时,HPLC检测重组枯草芽孢杆菌发酵液,结果也表明重组枯草芽孢杆菌成功表达了可溶性目的蛋白Op-MT。通过对重组工程菌中MT活性检测发现,其对重金属镉耐受力增强,说明重组工程菌成功表达出有活性的金属硫蛋白。这为以后开发天然、高效海洋源重金属解毒剂提供理论基础。福建省科技计划项目(2017N0016);;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(海三科2016031)共同资

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

2-去氧-D-葡萄糖的离子色谱法分析

开发一种分析2-去氧-D-葡萄糖样品的离子色谱方法,该方法可准确定量2-去氧-D-葡萄糖样品的含量.经色谱分离条件优化,选用DIONEX CarboPac PA10(4 mm×250 mm)色谱柱,以18 mmol/L NaOH溶液为流动相,流速为0.8 mL/min,用脉冲安培检测器检测,实现2-去氧-D-葡萄糖、葡萄糖和氨基葡萄糖3种结构极为相似单糖的高效分离,建立起2-去氧-D-葡萄糖的离子色谱法.2-去氧-D-葡萄糖在0.618~61.8μg/mL范围内呈现良好的线性关系,相关系数为0.998 6,最低检测限为27.2μg/L,最低定量限为216.3μg/L,平均回收率101.3%,实验结果表明该离子色谱法检测2-去氧-D-葡萄糖,简单、灵敏,测定结果准确,是测定2-去氧-D-葡萄糖含量的有效方法

低场核磁共振技术在鱼用冻干疫苗保护剂筛选中的应用

为筛选适合鱼类冻干疫苗中使用的保护剂,采用低场核磁共振技术(LF-NMR)对冻干后不同保护剂中的水分分布和迁移规律进行了分析。根据水中氢质子的弛豫时间,可将保护剂中的残留水分为结合水、不易移动水和自由水3种形态。结果显示:冷冻干燥过程中二次干燥温度对甘露醇和蔗糖中残留水的分布有较大影响,随着温度从4℃升高到37℃,大部分自由水解吸而小部分转化为结合水。当冻干后的样品暴露在相对湿度43%和温度25℃的环境中时,大部分保护剂吸收水分,并将其固定为结合水,而甘露醇中的部分结合水则转变为自由水,并解吸到环境中。不同冻干保护剂中的水分分布和迁移并不相同,代表其具有不同的水分结合能力。该研究结果有助于鱼用冻干疫苗中保护剂的筛选和冻干工艺的优化,以便获得更加稳定的疫苗产品。厦门海洋高技术产业基地创业创新共享服务平台项目(16PFW008SF15);;福建省高职院校海洋生物应用技术协同创新中心(2017);;“十三五”北海市海洋经济创新发展示范项目(Bhsfs003,Bhsfs009);;2010海洋公益行业科研专项(201005020-1

超临界流体色谱法分析非对映异构体d4T-5'-N-磷酰化苯丙氨酸甲酯

采用超临界CO2流体色谱技术,分析d4T-5'-N-磷酰化苯丙氨酸甲酯手性磷的非对映异构体。色谱柱为Hpersil ODS2(250 mm×4.6 mm,5μm),流动相为夹带改性剂甲醇、乙醇和异丙醇的超临界CO2流体。以容量因子、选择性和分离度为指标,考察改性剂、背压和柱温对分离的影响。在甲醇、乙醇和异丙醇3种改性剂中,甲醇为最好的改性剂,其中在7%甲醇改性剂下,该化合物的分离度可达到3.35。在7%甲醇改性剂条件下,考察了压力(10～20 MPa)和温度(303.15～318.15 K)的影响。在优化的分离条件(改性剂为7%甲醇,流速为2 mL/min,柱温为308.15 K,背压为15 M Pa)下,d4T-5'-N-磷酰化苯丙氨酸甲酯的两种非对映异构体完全达到基线分离,分离时间约15 min

Determination of Astaxanthin by High Performance Liquid Chromatography with Photodiode Array Detector

建立虾青素含量测定的高效液相色谱–光电二极管阵列法。采用PurOSPHEr STAr rP 18(4.6 MMx250MM,5μM)色谱柱,以甲醇–水(体积比为95∶5)为流动相,流速1.0 Ml/MIn,检测波长为482 nM,柱温为30℃,进样量为20μl。在所选定的液相色谱条件下,虾青素主峰与其它杂质峰分离良好,虾青素在0.2~16μg/Ml范围内线性良好,线性相关系数r=0.999 9,检出限为0.01μg/Ml,测定结果的相对标准偏差为0.42%(n=6),平均回收率为100.4%。该法分析快速准确、灵敏度高、重现性好。A method using high-performance liquid chromatography(HPLC) coupled with photodiode array detector(PDA) was established for determination of astaxanthin.The separation was performed on Purospher STAR RP 18 column(4.6 mm×250 mm,5μm) with the mobile phase of methanol–water(Volume ratio was 95∶5).The detector was photodiode array detector and the variable wavelength detector(VWD) was set at 482 nm.The column temperature was 30℃ and the injection volume was 20 μL.The calibration curve was linear in the range of 0.2–16 μg/mL,and the correlation coefficient was 0.999 9.The relative standard deviation of determination results was 0.42%(n=6).The average recovery was 100.4%, and the detection limit was 0.01 μg/mL.This method is characteristic of rapidity,accuracy,high sensitivity and good reproducibility.海洋生物产业化中试技术研发公共服务平台项目(厦海渔合[2013]19号

质谱和动力学技术研究胰岛素-多糖纳米粒稳定性和释放胰岛素速率

以海藻酸钠(sodium alginate,SA)和壳聚糖(chitosan,CS)为纳米粒包被材料,构建胰岛素(insulin,INS)多糖纳米粒.采用基质辅助激光解吸电离飞行时间(Matrix-assisted laser desorption ionization/time of flight,MALDI-TOF)质谱技术研究若干化学因素影响INS-多糖纳米粒的稳定性.选用电子光谱技术研究INS-多糖纳米粒控释INS速率及动力学特性.实验结果表明,INS-SA纳米粒在Tris-HCl缓冲液(pH7.2)和醋酸介质中均呈不稳定状态,易释放INS;而INS-CS纳米粒在Tris-HCl缓冲液中呈较为稳定状态,其释放INS速率明显慢于INS-SA纳米粒,并遵循一级反应动力学过程.INS-SA和INS-CS纳米粒均能有控制INS释放速率能力,但两者释放速率明显不同,其速率可分为快速与慢速释放方式.CS比SA更适合于作为包被材料研制INS-多糖纳米粒口服制剂

Development of Trehalose Certified Reference Material

研制了海藻糖国家标准样品。以食品级海藻糖粗品为原料,纯化制备海藻糖,采用红外光谱(Ir)、质谱和核磁共振谱(nMr)以及单晶衍射等方法进行结构确证。样品分装成400瓶后,采用离子色谱法进行均匀性、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。在40℃下,经过24个月稳定性考察,结果表明样品稳定性良好。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,海藻糖标准样品定值结果为99.72%,扩展不确定度为0.26%(k=1.96)。该标准样品达到国家标准样品的技术要求,可用于有关海藻糖的方法校正和质量控制。Trehalose certified reference material was developed.Trehalose was purified from the crude product.The structure of trehalose certified reference material was comfirmed by infrared spectroscopy(IR),mass spectrometry,NRM and XRD.Trehalose was divided into 400 bottles.The homogeneity and stability testing and quantitative analysis were evaluated by ion chromatography method.According to analysis procedure of homogeneity,15 bottles of sample were randomly taken from 400 bottles,and the results were validated by F-test statistical methods.The stability inspection was carried on the long-term(24 months),and the results indicated that the period for trehalose storage was 24 months at 40 ℃.A cooperative certification was conducted by 8 qualified laboratories.The certified purity value of the reference material of trehalose was 99.72%with relative expaned uncertainty of 0.26%(k=1.96).The reference material can conform to the technical requirement of the certified reference material,and it can be used for validation and quality control regarding trehalose.福建省科技计划项目(2013N01010205); 厦门市海洋经济创新发展区域示范项目(12PZP001SF10); 海洋公益行业科研专项(201005020–1); 厦门市科技计划项目(3502Z20122009