脂肪醇类溶剂对青霉素的萃取

研究了不同醇类及醇酯混合体系对青霉素的萃取. 在pH=4的条件下脂肪醇及醇酯混合体系的萃取能力均高于乙酸丁酯. 具有相同碳原子数、带支链的脂肪醇对青霉素的萃取能力比直链醇强,平衡后的有机相水含量下降. 红外光谱分析表明：乙酸丁酯的加入使脂肪醇羟基谱带变宽且明显向高波数方向位移,能阻止醇的多聚,使羟基活性增强. 激光拉曼光谱结果证明：青霉素是以反相微乳液的形式进入脂肪醇相的;支链的存在使体系的有序性和极性都明显增加.     

Investigation of Three-liquid-phase Extraction Systems for Simultaneous Separation of Emodin and Rhein

Several three-liquid-phase extraction systems comprised of organic extractant,polymer and salt aqueous solution were applied to isolate and purify simulated herbal extract containing emodin and rhein.Some influential factors on the partitioning behaviors were studied.The results revealed that extractant type and solution pH value were crucial factors for improving the separation performance.The optimal separation results were obtained at pH 8.00 with methyl isobutyl ketone as the extractant,10%（ω） polyethylene glycol with the molecular weight 4000 Da,and 10%（ω） ammonium sulphate.Under the optimized conditions,95%emodin and 97%rhein were simultaneously extracted into the organic phase and polymer-rich phase from simulated herbal solution with the initial concentration of 100×l0^-6（ω）,respectively,and their separation factor of over 10000 was achieved.By adjusting pH value,back extraction rate of both emodin and rhein could be up to about 99%.With the assistance of molecular simulation program XLOGP3 and molecular orbital package,the possible mechanism of extraction was analyzed,and hydrophobic interaction and hydrogen-bonding interaction might be the major driving forces affecting the partitioning behaviors of emodin and rhein.     

青霉素RSE—POD机串联萃取工艺探索与应用

RSE离心机（固-液-液三相萃取分离机）为固-液-液三相立式分离机,是德国生产的新型离心机,具有处理量大、分离因数高、能够自动排渣的特点;美国生产的液-液卧式离心分离萃取机（POD机）,具有处理量大、萃取级数高（可达4级）、收率高的特点。在青霉素新萃取工艺开发中,充分利用这2种设备的优点,开发了RSE与POD机串联逆流萃取生产工艺,该工艺具有连续稳定、劳动强度小、产品质量好、收率高等优点。     

Partitioning Behavior of Penicillin G in Aqueous Two Phase System Formed by Ionic Liquids and Phosphate

Abstract

An aqueous two‐phase system (ATPS) was presented with hydrophilic ionic liquid 1‐butyl‐3‐methylimidazolium chloride ([Bmim]Cl) and NaH₂PO₄ aqueous solution in this paper. The partitioning behavior of penicillin G in the ATPS was investigated. Concentrations of NaH₂PO₄, penicillin G, and [Bmim]Cl were evaluated to determine their effects on the partition coefficient and extraction yield of penicillin G. It was found that both of partition coefficient and extraction yield strongly depended on the concentration of [Bmim]Cl, penicillin and NaH₂PO₄. A high extraction yield of 93% was achieved with the following parameters: NaH₂PO₄ · 2H₂O 40% (wt%), penicillin 45000～50000 u/ml, [Bmim]Cl 20～21% (wt%). The [Bmim]Cl/NaH₂PO₄ system was also applied in a real filtration of penicillin G fermentation broth and the extraction yield was averaged at 91.5%. It is worthy noting that the working pH value of ATPS was at the range of 5～6, no emulsification and protein denaturation could be observed.     

替考拉宁在不同液液萃取体系中分配系数的测定

Teicoplanin is one of the macrocyclic glycopeptide antibiotics, which is active against Gram-positive bacteria, and has attracted a lot of attention in the field of chiral separation recently. In this work, the partition coefficients and extraction ratio of teicoplanin in three different solvent systems were studied: conventional extraction, reactive extraction and reverse micelle extraction. With conventional solvent extraction, n-butanol demonstrated high partition coefficient for teicoplanin, but low extraction ratio because of its high solubility in water. Reactive extraction of teicoplanin showed the highest partition coefficient with almost 100% recovery in organic phase when tri-n-octylmethyl ammonium chloride (TOMAC) was used as extractant and pH value was above 5.0. A reverse micelle system, consisted of isooctane 10 mmol-L^-1 TOMAC -t-1% n-octanol, also offered high separation factor for teicoplanin. The results are beneficial for the design of teicoplanin separation and purification process.     

Determination of Teicoplanin A2's Partition Coefficient in Different Liquid-Liquid Extraction Systems

Teicoplanin is one of the macrocyclic glycopeptide antibiotics, which is active against Gram-positive bacteria, and has attracted a lot of attention in the field of chiral separation recently. In this work, the partition coefficients and extraction ratio of teicoplanin in three different solvent systems were studied: conventional extraction, reactive extraction and reverse micelle extraction. With conventional solvent extraction, n-butanol demonstrated high partition coefficient for teicoplanin, but low extraction ratio because of its high solubility in water. Reactive extraction of teicoplanin showed the highest partition coefficient with almost 100% recovery in organic phase when tri-n-octylmethyl ammonium chloride (TOMAC) was used as extractant and pH value was above 5.0. A reverse micelle system, consisted of isooctane 10mmol-L-1 TOMAC 1% n-octanol, also offered high separation factor for teicoplanin. The results are beneficial for the design of teicoplanin separation and purification process.     

The Extraction of Penicillin G with Aliphatic Amines in Organic Solvents of Different Polarities

The equilibrium constants of the extraction, the molar ratios of amines to penicillin G in the extract and the bonding structures of the extracted species were studied with chemical analysis and the absorbance shift of FT-IR spectra of the functional groups in penicillin G. Extraction of penicillin G from the filtrate of fermentation broth indicates that amines will be difficult to use as the industrial solvent for the production of penicillin G because of the poor quality of the final crystalline product obtained and the difficulties involved in the stripping and solvent recovery.     

Novel Gas-assisted Three-liquid-phase Extraction System for Simultaneous Separation and Concentration of Anthraquinones in Herbal Extract

abstract Gas-assisted three-liquid-phase extraction (GATE), which has the advantages of both three-liquid-phase extrac-tion and solvent sublation, is a novel separation technique for separation and con...     

新型高效破乳剂在青霉素生产中的应用

本文介绍了我国青霉素征税中使用的破乳剂现状，对破乳机理进行了比较详细的阐述，新型高效破乳剂Ｄ９２５ｍ采用了混合的表面活性剂体系，可调性好，适应性强，已受到国内主要青霉素生产厂家的关注。     

青霉素钾,青霉素亚砜和青霉素砜的薄层色谱法分离和鉴别

用薄层色谱法分离和鉴别青霉素钾、青霉素亚砜、青霉素砜，斑点清晰，重现性好，可作为中间体的检测。     

青霉素G钾/钠在含乙酸丁酯混合溶剂中的溶解度

测定了青霉素G钾在乙酸丁酯与水混合溶剂100mL中,其中含水0．6mL至9．0mL,温度为23.5℃、46．7℃和52．0℃时的溶解度;以及青素霉G钾和钠在含乙酸丁酯、水、乙酸和乙醇等几个特定组成溶剂中,温度范围27．0至50．0℃的溶解度。试验结果可用于青霉素G钾或青霉素G钠结晶过程。     

高效青霉素萃取助剂的合成研究

对发酵青霉素萃取助剂的种类及效果进行了综述,重点介绍了乙氧基脂肪二胺和脂肪酰胺复配破乳剂,并以牛油二胺和环氧乙烷为原料,氢氧化钾为催化剂,合成了乙氧基脂肪二胺,环氧乙烷反应率可达79.5%;用大豆植物油和三乙醇胺合成了油酰胺,以乙氧基脂肪二胺为主、油酰胺为辅制备了破乳剂,该破乳剂用于青霉素的提取,使用量300ppm,溶解情况良好,萃取液界面清晰,界面层厚度0.9~1.2mm,离心分层时间35s,青霉素提取收率（两步,二次结晶）90.6%,性能优于市售同类产品。     

青霉素制备青霉素亚砜的研究

以青霉素G钾盐与低质量分数过氧乙酸为原料氧化制备青霉素亚砜 ,其最佳工艺条件为 :n(C16 H18N2 O4 SK)∶n(CH3CO3H) =1 .0∶( 1 1～ 1 2 ) ,反应温度 0～ 5℃ ,反应时间 2 .0～ 2 5h ,w(CH3CO3H) =8 5% ,w(CH3CO2 H) =1 0 %。青霉素亚砜收率达 96 8%。同时建立了青霉素亚砜的半定量分析方法 ,以硅胶G为固定相 ,以V(CH3CO2 C4 H9 n)∶V(CH3CO2 H)∶V(NaH2 PO4 -H2 O)∶V(C4 H9OH n) =6.0∶2 .0∶1 .0∶0 5为流动相 ,用TLC法对产品进行半定量分析检测 ,并经IR、MS谱图验证了产品结构。     

Separation of Penicillin G from Fermentation Broth Using N,N-Dioctyloctan-1-amine Extractant in Different Diluents

The extraction of penicillin G was investigated using N,N-Dioctyloctan-1-amine (TOA) with different diluents having distinct functional groups. Nine diluents were used in the study, namely, octan-1-ol, nonan-1-ol, isoamyl alcohol, ethyl ethanoate, propyl ethanoate, methyl iso butyl ketone(MIBK), octan-2-one, octane, and decane. The measurements were performed at a temperature of 298.2 K. The experimental results of batch extractions were used to calculate distribution coefficients (K_D), loading factors (Z), and extraction efficiency (E). The highest distribution coefficient (K_D = 5.79) was obtained with isoamyl alcohol, and its extraction efficiency was 85.27%. Further, the highest loading factor was reached to a value of 0.130 at 0.374 mol.kg^?1 amine concentration. Overloading was not observed at any amine concentration. Solvatochromic model (Linear solvation Energy Relationship (LSER)) for data which obtained from alcohols experiments gives the good results as near as same to experimental results. Suitability of data between experiments and model predictions have been tested with root main square deviation (RMSD) with 0.99.     

青霉素G亚砜的合成

以青霉素G钾盐为原料,采用15%左右低浓度过氧乙酸为氧化剂合成青霉素G亚砜,反应时间2～2.5h,n(过氧乙酸):n(青霉素G钾盐)=(1.1～1.2):1.0,反应温度和结晶温度在0～5℃,总收率可达96%以上。所得青霉素G亚砜可直接从溶液中结晶析出,解决了产物与反应体系的分离。产品纯度较高。     

青霉素G亚砜对-硝基苄酯的制备研究

对青霉素G钾制备青霉素G亚砜对-硝基苄酯工艺进行了研究。在青霉素G钾:过氧乙酸(mol)为1∶1.15,氧化温度<5℃,反应时间2 h的条件下,青霉素G亚砜收率为89.0%。酯化反应最佳反应条件为:DMF的用量为4.28 mL/1 g青霉素亚砜,反应温度为室温,青霉素亚砜与对-硝基氯苄的投料比(mol)为1∶1.15,反应时间为24 h,在此条件下酯化收率为80.23%。此方法对于控制产品品质和确保操作安全简便,对工业化生产具有参考意义。     

Partition Behavior of Drug Molecules in Cholinium-Based Ionic Liquids

In this paper, a series of ionic liquids (ILs) contains cholinium as cations were prepared. These ILs were used as extractants to separate some model drug molecules. The partition coefficients of these drug molecules between ILs and aqueous solutions were determined. Furthermore, the influence of different extraction parameters was investigated: volume ratio, equilibrium time, pH values, temperature, and ILs structure. It is shown that these ILs are highly effective materials for the extraction of drug molecules. The results imply that these ILs may have potential in drug extraction or separation as a new type of media.     

青霉素G亚砜二苯甲酯的合成研究

以青霉素G钾为原料制备青霉素G亚砜二苯甲酯。氧化反应优化条件为:n(过氧乙酸)∶n(青霉素G钾)=1.2∶1.0,氧化温度0～5℃,反应时间2h,青霉素G亚砜酸收率为97.3%;酯化反应优化条件为:二氯甲烷的用量为17mL/g青霉素G亚砜,投料比n(二苯甲醇)∶n(青霉素G亚砜)=1.8∶1.0,反应温度为-15℃,反应时间为60min,酯化收率为79.5%,反应总收率为77.4%。此工艺成本低廉,操作安全简便,对工业化生产具有积极意义。     

青霉素发酵过程精细化控制

青霉素发酵生产水平一方面取决于菌种的生产能力,另一方面取决于发酵过程的控制。青霉素发酵周期长,影响因素多,加大了工艺控制的难度。同一个菌种,同样的设备,由于过程控制的不同,发酵水平可以相差15%以上。通过对青霉素发酵过程中种子质量的控制,移种过程的精细操作和检查,pH值、氨氮等重要参数的控制,补料的动态调整等方面的精细化控制,可以有效地控制代谢方向,避免代谢异常,防止出现低水平罐批,使发酵罐批之间的差异降低,整体发酵水平提高5%左右。     

Penicillin G extraction from model media using an emulsion liquid membrane: Determination of optimum extraction conditions

Penicillin G extraction by an emulsion liquid membrane (ELM) was investigated. The effects of surfactants, diluents, and carrier mixtures, together with their combined effects on the initial extraction rate and the emulsion stability were examined. Surfactants, diluents, and carriers used were Span80 (sorbitan monooleate)/ECA4360J (nonionic polyamine), n-butyl acetate/kerosene, and DOA (dioctylamine)/Amberlite LA-2 (secondary amine), respectively. The optimum extraction conditions were found to be 20% (v/v) of Span80 in ECA4360J as a surfactant, kerosene as a diluent and Amberlite LA-2 as a carrier.