Studies on determination of glucosamine by HPLC-ELSD

目的:建立氨基葡萄糖含量测定的高效液相色谱分析法。方法:样品采用高效液相色谱进行测定,使用Waters Carbohydrate色谱柱,流动相为乙腈-水=70:30,用蒸发光散射检测器(ELSD)检测。结果:方法的进样量线性范围为2.0～12.0μg,相关系数为0.9997,回收率为96.0%～97.7%。结论:此法简便、快速、准确,无需衍生反应,是测定氨基葡萄糖含量的有效方法,并可用于硫酸氨基葡萄糖含量的测定。Objective:A HPLC method for the determination of glucosamine was developed.Methods:The content of glucosamine was determined by HPLC on a water carbohydrate column(4.6 mm×250 mm,5 μm) with acetonitrile-water(70:30) as mobile phase and ELSD detector.Results:The linear range of calibration curve was 2.0～12.0 μg(r=0.9997),the recovery was 96.0%～97.7%.Conclusion:The method is simple,rapid,accurate and without derivation.It is a effective method for determination of glucosamine and can be used for determination of glucosamine sulfate.厦门市重大科技项目(3502Z20051025

Quantitative determination of arachidonic acid from microbial oil by gas chromatography

建立了快速、灵敏测定微生物油脂中花生四烯酸(AA)含量的气相色谱法(gC)。采用HP-InnOWAX毛细管柱,氢火焰离子化检测器(fId),优化了分析花生四烯酸酯化产物的色谱条件。结果表明:花生四烯酸甲酯(AA-ME)在0~1.00 Mg/Ml范围内具有较好线性,相关系数为0.999 6,检测限为0.000 5 Mg/Ml,相对标准偏差(rSd)为1.49%,回收率在95.86%~105.32%;花生四烯酸乙酯(AA-EE)在0~1.23 Mg/Ml范围内线性良好,相关系数为0.999 9,检测限为0.003 0 Mg/Ml,rSd为0.60%,回收率在97.79%~103.61%。A gas chromatography(GC) method for the determination of arachidonic acid(AA) in microbial oil was developed.Capillary column HP-INNOWAX with FID was used for detection.The parameters for analyzing esterfied AA were optimized and the method established was proved to be accurate and precise.The linearity range for methyl arachidonate was 0-1.00 mg/mL and the linear correlation coefficient was 0.999 6,the detection limit was 0.000 5 mg/mL,the relative standard deviation(RSD)was 1.49% and the recovery rate was 95.86%-105.32%.The linearity range for ethyl arachidonate was 0-1.23 mg/mL and the linear correlation coefficient was 0.999 9,the detection limit was 0.003 0 mg/mL,the RSD was 0.60% and the recovery rate was 97.79%-103.61%.厦门海洋研究开发院共建项

Methyl Esterification of Arachidonic Acid in Microbial Oil

作者简介：董宏祯(1988 —)，男，硕士研究生，研究方向为天然产物化学。E-mail：[email protected] 通信作者：许建中(1954 —)，男，高级工程师，本科，研究方向为生物化工。E-mai l：[email protected][中文文摘]以微生物油脂为原料,对其中花生四烯酸的甲酯化方法进行筛选和优化。在确定合适的花生四烯酸甲酯化方法基础上,考察酯化温度、酯化时间、催化剂体积分数及搅拌转速对花生四烯酸酯化效果的影响。结果表明:酯化温度80℃、酯化时间8h、浓硫酸体积分数2.0%、转速400r/min时,花生四烯酸甲酯质量分数达到37.75%,产率达到91.54%。甲酯化后的花生四烯酸沸点较低,适用于分子蒸馏。[英文文摘]In order to maximize arachidonic acid methyl ester production,the methyl esterification of microbial oil was optimized with respect to temperature,reaction time,catalyst(concentrated sulfuric acid) dosage and agitation speed using one-factor-a-at-a-time combined with orthogonal array design method.The highest yield of 91.54% was achieved after 8 h of reaction at 80 ℃ and an agitation speed of 400 r/min under the catalysis of 2.0% concentrated sulfuric acid.The obtained product contained 37.75% arachidonic acid methyl ester and its boiling point was lower than before the reaction, facilitating molecular distillation.厦门海洋研究开发院共建项目; 福建省海洋与渔业厅科技重点项目([2009]2-10);厦门市科技计划项目(3502Z20112005);福建省2010年第二批产业技术开发项目(5012060403

Effects of Acid Extraction Parameters on Properties of Pectin from Pomelo Peel

作者简介：林晓锋(1986 —)，男，硕士研究生，研究方向为化学工程。E-mail：[email protected] 通信作者：许建中(1953 —)，男，高级工程师，研究方向为生物化工。E-mail：[email protected][中文文摘]选用福建特产琯溪蜜柚果皮为原料,考察酸提工艺条件对果胶的酯化度、黏均分子质量和半乳糖醛酸含量的影响,设计正交试验L9(34)考察各因素的影响。结果表明:在试验范围内,酸提工艺条件对果胶的酯化度基本无影响,对半乳糖醛酸的含量有明显的影响,对果胶的分子质量影响最显著。9个不同试验条件下,酸提果胶的酯化度63.5%～63.8%,半乳糖醛酸含量74.2%～88.5%,果胶的黏均分子质量101～202ku。[英文文摘]The effects of process parameters such as temperature,solid/liquid ratio,extraction time and pH for pectin extraction from Guanxi honey pomelo peel with dilute hydrochloric acid on degree of esterification(DE),viscosity-average molecular mass and galacturonic acid content of pectin were investigated using an L9(34) orthogonal array design.The results showed that the process parameters had little effect on pectin DH,remarkable effect on galacturonic acid content,and the largest effect on viscosity-average molecular mass and galacturonic acid content of pectin were investigated using an L9(34) orthogonal array design. The results showed that the process parameters had little effect on pectin DH, remarkable effect on galacturonic acid content, and the largest effect on viscosityaverage molecular mass. The 9 orthogonal array runs resulted in a DH of 63.5%-63.8%, a galacturonic acid content of 74.2%－88.5% and a viscosity-average molecular weight of 101－202 ku.福建省科技计划重点项目(2010Y0035

Separation and Purification of Naringin by Solid Phase Extraction Using Strong Anion Exchange Cartridge

作者简介：宁方刚(1986 —)，男，硕士研究生，研究方向为天然产物化学。E-mail：[email protected] * 通信作者：许建中(1954 —)，男，高级工程师，本科，研究方向为生物化工。E-mail：[email protected][中文文摘]目的:建立固相萃取分离纯化柚皮苷的方法。方法:以强阴离子交换(strong anion exchange,SAX)填料为吸附材料,利用柚皮苷与填料的功能基团之间的静电作用将柚皮苷吸附在填料上,考察洗脱液离子强度、洗脱液体积,洗脱流速对洗脱效果的影响。结果:选用5mL碳酸氢钠溶液(0.1mol/L,pH9.0)为洗脱液,以0.5mL/min的流速进行洗脱,回收率达到91%以上。结论:本方法简单、高效,选择性好,可为柚皮苷样品的纯化提供理论依据。 [英文文摘]Purpose: A solid-phase extraction procedure for the separation and purification of naringin(NG) was developed using strong anion exchange(SAX) cartridge.Method: Naringin was adsorbed onto the cartridge by electrostatic interaction between naringin and functional groups.Several variables affecting the elution performance of SAX,such as ionic strength of elution,elution volume and elution rate,were studied.Results: The application of 5 mL of sodium bicarbonate solution(0.1 mol/L,pH = 9.0) to elute SAX cartridge at a flow rate of 0.5 mL/min resulted in a recovery rate of 91%.Conclusions: The established method is simple and efficient.福建省科技计划重点项目(2010Y0035

CO-OFDM DWDM系统非线性容限的仿真研究

为了提高光传输容量,提出了一种四进制正交幅度调制相干光检测正交频分复用系统与密集波分复用系统平行复用的超信道系统。利用Optisystem软件和Matlab软件搭建仿真平台,采用非线性分离模型控制四波混频噪声的加入,并使用误差向量幅度来测量误码率。在不同的传输速率、复用间隔和信道数下,通过仿真不同的循环前缀、入纤功率来研究四波混频对系统的影响和系统的非线性容限。仿真结果表明,随着循环前缀的增大,误码率先减小后增大,有最优取值,一般为快速傅里叶变换窗口长度的1/8。新型光纤链路超信道系统的误码率总是比常规光纤链路的小,且有更好的非线性容限

Simultaneous Determination of Glucuronic Acid and Glucuronolactone Using Ion-exclusion Chromatography

建立了同时检测葡萄糖醛酸和葡萄糖醛酸内酯的离子排斥色谱法。采用bOSTOn HC-b75 H+色谱柱进行分离,以5 MMOl/l H2SO4水溶液为流动相,流速0.6 Ml/MIn,柱温25℃,紫外检测波长220 nM;根据外标法定量,葡萄糖醛酸和内酯分别在10~1200 Mg/l和5~600 Mg/l范围内线性良好(r>0.9999);葡萄糖醛酸、葡萄糖醛酸内酯的最低检测限及定量限均分别为0.1和0.3 Mg/l,精密度实验rSd分别为1.00%和0.35%,平均回收率分别为99.69%和98.21%。该检测方法简便、快速、灵敏,可用于葡萄糖醛酸和葡萄糖醛酸内酯的同时测定。温度、PH值和溶剂对葡萄糖醛酸稳定性有影响,可为葡萄糖醛酸的分析与制备研究提供参考依据。An analytical method was established for the simultaneous determination of glucuronic acid and glucuronolactone using ion-exclusion chromatography.The separation was performed on a Boston HC-B75 H+ column at 25 ℃ by HPLC equipped with an ultraviolet detector at the wavelength of 220 nm.The mobile phase is 5 mmol / L sulfuric acid with a flow rate of 0.6 mL / min.The quantification was performed by an external standard.The linear ranges for glucuronic acid and glucuronolactone are 10 ~ 1200 mg / L and 5 ~ 600 mg / L( r > 0.9999),respectively.The detection and quantification limits for the two compounds are 0.1 mg / L and 0.3 mg / L,respectively.The standard deviations for glucuronic acid and glucuronolactone are 1.00% and 0.35%,respectively.The recovery ratios for glucuronic acid and glucuronolactone are 99.69% and 98.21%,respectively.This method is convenient,rapid,sensitive and suitable for the simultaneous determination of glucuronic acid and glucuronolactone.Temperature,pH and solvent affected the stability of glucuronic acid.国家海洋公益性行业专项(201005022); 中国大洋矿产资源研究开发协会专项(DY125-15-T-01)资助~

Purification of Naringin by simulated moving bed chromatography

通过四区模拟移动床色谱制备纯化柚皮苷。采用高效液相色谱测试单柱的相关参数,通过三角形方法,确定线性条件下的完全分离操作范围。在该范围中选取操作条件进行柚皮苷的制备纯化。实验结果表明,当选取的一至四区流速分别为2Ml/MIn,1.35Ml/MIn,1.69Ml/MIn,0.69Ml/MIn,切换时间为35.5MIn时,通过面积归一法计算出,该系统制备的柚皮苷纯度可从粗品的82%提升到98%左右,主要杂质峰基本消失,满足柚皮苷的高纯度制备要求。柚皮苷的回收率为97%,产率为0.33Mg/MIn,溶剂耗量为4.85Ml/Mg。The naringing was purified by four-zone simulated moving bed.The relative parameters were determined by HPLC and the complete separation region was found under linear condition with triangle theory.In this region,the oparation conditions were set.As the result,according to the area normalization method,the naringin purity increased to appoximate 98% from the 82% in crude sample by this system when flow rates of the four zone were 2mL/min,1.35 mL/min,1.69 mL/min,0.69 mL/min respectively and switching time was 35.5min.The main impurity was disappeared and this process could reach the separation requirment.The naringin recovery was 97%,productivity was 0.33mg/mL and desorbent consumption was 4.85mL/mg

Isolation and Identification of Two Terphenyl Compounds fromAspergillus candicus Metabolites

对深海来源真菌亮白曲霉(ASPErgIlluS CAndIduS)进行固体发酵,并采用浸泡萃取法和中高压制备柱对代谢产物进行提取分离,从中分离得到化合物1和2,通过波谱解析确定化合物1为三联苯曲霉素(TErPHEnyllIn),化合物2为2,4-二甲氧基-1,10-二羟基对联三苯.对6种不同菌株进行抑菌实验,表明两化合物均具有抗菌活性.本实验是首次报道化合物2(2,4-二甲氧基-1,10-二羟基对联三苯),也是第一次从海洋真菌中分离得到化合物2.The vast ocean area is a great treasure trove of resources,but the research and utilization is not enough,especially for deep-sea microorganisms.Deep-sea has specific environments,and the chance of obtaining novel structure is big.Deep-sea microorganisms have been focused on its significant economic value.Solid fermentation was performed using Aspergillus candicus from deepsea.The solid fermentation was extracted using soaking method and the metabolites were separated using medium-pressure preparative liquid chromatography column.Two compounds of antifungal bioactivity were obtained.Based on their spectroscopic data,their structures were elucidated.Compound 1 is terphenyllin.It′s a antioxidant and has cytotoxicity.Compound 2 is 2,4-dimethyl-1,10-dihydroxy-p-terphenyl,apotential antioxidant.It is the first report of compound 2,especially fromAspergillus candicus of deep-sea.国家海洋公益性行业专项(201005022); 中国大洋矿产资源研究开发协会专项(DY125-15-T-01