基于甘草配伍黄芩同时泡沫分离甘草酸和黄芩苷

为了同时分离甘草中有表面活性的甘草酸和黄芩中无表面活性的黄芩苷,开发了甘草配伍黄芩泡沫分离工艺。通过荧光光谱、紫外吸收光谱和红外吸收光谱分析表明,甘草酸与黄芩苷存在相互作用,并且甘草黄芩配伍强化了甘草酸和黄芩苷的提取。以甘草酸和黄芩苷的富集比和回收率为评价指标,当温度为40℃、气体体积流量为100 ml·min~(-1)、甘草酸初始浓度为0.2 g·L~(-1)、甘草黄芩质量比为3:1时,获得甘草酸的富集比和回收率分别为11.0和73.5%,黄芩苷的富集比和回收率分别为5.8和38.5%。通过甘草与黄芩配伍,利用泡沫分离获得黄芩中的黄芩苷。同时,与单独泡沫分离甘草中甘草酸相比,甘草酸的富集比提高了194.9%,回收率提高了23.3%。因此,甘草配伍黄芩能有效泡沫分离甘草酸和黄芩苷。     

麻黄强化泡沫分离甘草酸的工艺研究

为了提高泡沫分离甘草中甘草酸的分离效果,开发了甘草麻黄配伍泡沫分离工艺,并就麻黄对浸提液泡沫性能的影响进行了研究。结果表明,麻黄强化了甘草酸的提取,但降低了浸提液中甘草苷的浓度,使得浸提液的泡沫性能发生变化而影响泡沫分离甘草酸的分离效果。以甘草酸的富集比和回收率为评价指标,研究了温度、气体体积流量、甘草酸初始浓度和甘草麻黄质量配比对分离效果的影响。结果表明当温度为40℃、气体体积流量为100 m L×min~(-1)、甘草酸初始浓度为0.2 g×L~(-1)和甘草麻黄质量配比为5:3时,获得甘草酸的富集比和回收率分别为8.34和62.5%。与单独泡沫分离甘草中甘草酸相比,甘草酸的富集比提高了121.7%,而回收率并未明显降低。因此,麻黄的引入有效地提高了泡沫分离甘草酸的分离效果。     

分子荧光光度法测定黄芩中黄芩苷的含量

采用分子荧光光度法测定黄芩中黄芩苷的含量。结果表明,在硼砂浓度为0.020 moL·L^-1,pH值为12.5,黄芩苷溶液的荧光强度较大。黄芩苷溶液在0.50～2.5μg·mL^-1质量浓度范围内与其荧光强度呈现出良好的线性关系,线性方程为y=176.89+82.14x,R²=0.999 1。根据标准曲线计算得到黄芩药材中黄芩苷的含量。该方法具有选择性好、灵敏度高、操作简单的优点。     

生、炙百部分别与黄芩配伍后黄芩苷含量比较

采用RE-HPLC方法测定生、炙百部分别与黄芩配伍后化学成分含量进行比较。流动相为甲醇-水-磷酸（47∶53∶0.2）,流速：1.0 mL·min-1,检测波长：280 nm。生、炙百部分别与黄芩配伍后黄芩苷与其它成分分离度良好。高效液相色谱法（HPLC）测定黄芩苷,可达线分离,黄芩苷对照品进样量在0.069-0.299μg范围内呈线性关系,R=0.9997,平均回收率为96.93%,RSD=1.5%（n=6）。表明该方法简便快捷,结果准确,重现性好,生方中平均含量为47.5 mg·g-1;炙方中平均含量为60.0 mg·g-1。     

高效液相色谱法检测化妆品中黄芩苷、黄芩素和汉黄芩素

建立了高效液相色谱法检测化妆品中黄芩苷、黄芩素和汉黄芩素的方法。样品经磷酸甲醇溶液超声提取,以甲醇-磷酸溶液梯度洗脱和C18反相色谱柱分离,DAD检测器检测计算3种中药成分含量。黄芩苷在0.5~10μg/m L,黄芩素在0.5~10μg/m L及汉黄芩素在0.25~5μg/m L范围内浓度和278 nm紫外光吸收强度呈良好线性关系,相关系数大于0.999,方法检出下限分别为2、2和1 ng,方法回收率95.3%~112.7%,RSD为0.9%~5.2%。该方法适于快速、高效、准确对化妆品中黄芩苷、黄芩素和汉黄芩素进行测定。     

高效液相色谱法测定不同配伍比例甘草、威灵仙药对中甘草苷、甘草酸的含量

目的:建立测定不同配伍比例甘草、威灵仙药对中甘草苷、甘草酸的含量的方法,探讨不同配伍比例配伍的药对的合理性。方法:色谱柱Agilent 20RBAX XDB-C18(4.6 mm×250 mm,5μm)流动相为乙腈(B)-0.1%磷酸盐溶液(A),洗脱方式为梯度洗脱,0~10~19~20~24~70~75min,乙腈(B)为:15%~25%~25%~32%~80%~15%,0.1%磷酸盐溶液(A)为:85%~75%~75%~68%~20%~20%~85%。检测波长254 nm,流速为1 m L·min~(-1),柱温为室温,进样量20 L。结果:配伍比例为4∶1时,甘草苷、甘草酸含量分别为:10.67 mg·g~(-1)、30.54 mg·g~(-1)。甘草苷在0.0123~0.04305 mg·m L~(-1)浓度内呈良好线性关系,回归方程Y=509.31X-0.237,R2=0.9998;甘草酸在0.03684~0.12897 mg·m L~(-1)浓度范围呈良好线性关系回归方程Y=493X+0.6841,R2=0.9982。甘草苷、甘草酸平均回收率分别为97.50%,97.10%。结论:最佳的配伍比例为4∶1。     

HPLC法测定肺胀颗粒中橙皮苷和甘草苷的含量

建立同时测定肺胀颗粒中橙皮苷和甘草苷含量的方法。采用HPLC-UV法,Diamonsil C_(18)柱(4.6 mm×150 mm,5μm),流动相为0.2%磷酸水溶液-乙腈,梯度洗脱,检测波长为283 nm,柱温为30℃,流速为1 mL/min。橙皮苷和甘草苷分别在3.812¹14.36μg/mL和1.874114.36μg/mL和1.874⁵6.22μg/mL范围内线性关系良好,平均回收率分别为100.2%,98.87%,RSD分别为1.45%,1.15%。该法简便、准确、灵敏、重现性好,可用于肺胀颗粒中橙皮苷和甘草苷含量的同时测定。     

HPLC测定达原饮中的芍药苷和黄芩苷的含量

目的:建立同时测定达原饮中芍药苷和黄芩苷含量的方法。方法:采用双波长HPLC,Aglient ZORBAX SB-C_(18)柱(4.6×250mm,5μm);流动相:0.2%H3PO4溶液-甲醇(体积比50∶50);检测波长分别为230nm(芍药苷)和280nm(黄芩苷);柱温为30℃;流速为1m L·min~(-1)。结果:芍药苷和黄芩苷分别在9.69~155.04μg·m L~(-1),18.66~298.56μg·m L~(-1)线性关系良好,平均回收率分别为99.03%,98.98%,RSD分别为1.95%,1.67%。结论:该法简便、准确、灵敏、重现性好,可用于达原饮中芍药苷和黄芩苷含量的同时测定。     

温度对高浓度SDS水溶液泡沫稳定性及分离的影响

高浓度表面活性物质的分离是泡沫分离过程的难题,也是制约泡沫分离技术应用于工业化生产的瓶颈.为了解决高浓度表面活性物质泡沫分离的难题,以阴离子表面活性剂十二烷基硫酸钠(SDS)水溶液为体系,研究了在其临界胶束浓度(CMC)附近时,温度对SDS水溶液气泡直径、泡沫稳定性、富集比及回收率的影响.结果表明:温度对高浓度表面活性物质的泡沫分离有显著影响.当SDS水溶液浓度分别为1.2、2.3、3.5g·L-1,温度从30℃升高到70℃时,泡沫稳定性先增大后减小,在pH 6.9、表观气速2.4×10-3 m·s-1、装液量200 mL的操作条件下,气泡直径先减小后增大,富集比提高了3～5倍,回收率降低了34％～65％.     

Biosynthesis of glycyrrhetic acid 3-O-mono-β-D-glucuronide by whole cell in ionic liquid/water biphasic system

研究了水/离子液体两相体系中重组毕赤酵母Pichia pastoris GS115（r-PGUS-P）全细胞转化甘草酸（GL）生成单葡萄糖醛酸基甘草次酸（GAMG）的反应。确定最适反应体系为离子液体［BMIM］PF₆/水（2∶8,体积比）,最适缓冲液pH、反应温度、底物浓度和细胞加入量分别为5.4、45℃、6.0 mmol·L^-1和8.0 g·L^-1。在此条件下反应58 h,产物GAMG得率和化学键选择性分别为69.6%和67.2%,与纯水相反应体系相比,分别提高了12.4%和12.61%。离子液体循环使用7次后,回收利用率为93.47%。产物GAMG和副产物甘草次酸（GA）在此两相体系中得到有效分离,为后续产物分离带来便利。     

Separation of Tea Saponin by Two-Stage Continuous Foam Fractionation

A technology of two-stage continuous foam fractionation for tea saponin recovery was studied for increasing both the enrichment ratio and the recovery percentage. In the first stage, the effect of air flow rate, the initial pH, the feed flow rate, and the feed position were studied at a temperature of 60°C. The results showed that when the conditions of the first stage were at a temperature of 60°C, air flow rate 150 mL/min, pH 5.3, feed flow rate 1.92 mL/min, and feed position at the interface between the liquid phase and the foam phase, the enrichment ratio, and the recovery percentage of tea saponin were 4.02 and 56.4%, respectively, and the effluent solution was added to the second stage as the initial solution. When the conditions of the second stage were at a temperature of 30°C and an air flow rate of 300 mL/min, the recovery percentage of tea saponin reached 47.6%, and the foamate was added to the first stage as feed solution. The total recovery percentage of tea saponin reached 86.3% by the two-stage continuous foam fractionation.     

Foam fractionation for effective recovery of leaf protein from alfalfa (Medicago sativa L.)

ABSTRACT

Foam fractionation for recovering leaf protein from alfalfa (Medicago sativa L.) has been investigated. The extraction yield of alfalfa leaf protein (ALP) from the dried alfalfa leaves reached 71.90% under the extraction conditions of pH 8.0, temperature 70°C, and extracting time 40 min. For strengthening foam drainage at room temperature, a novel foam fractionation column with a cross-internal component covered superhydrophobic coating was developed. By using the extraction liquor as the feeding solution, a two-stage foam fractionation had been performed. Under the suitable operation conditions, the enrichment ratio and the recovery percentage of ALP were 4.33 and 89.0%, respectively.     

Separation of Bovine Serum Albumin by Foam Fractionation with Sieve Tray Column

A batch foam fractionation column with sieve trays was developed for enhancing the foam drainage. Effects of feeding concentration, air flow rate, number of stages, and sieve pore size on foam fractionation performances were investigated. The results indicated that the sieve trays enhanced the foam drainage effectively and improved enrichment ratio. At the liquid loading volume 490 mL, feeding concentration 0.1 g L^?1, and air flow rate 300 mL min^?1, the enrichment ratio reached 7.56 by using 10 stages of sieve trays with opening ratio of 38.25%, which was 1.84 times of that obtained by the control column.     

Purification and Concentration of the Total Saikosaponins Extracted from Radix Bupleuri using Foam Fractionation

The purpose of this study was to investigate the use of foam fractionation to recover saikosaponins. First, the solvent extraction method was applied for the extraction of saikosaponins from radix bupleuri using ethanol or deionized water. Then, the foam fractionation technique in batch mode was used for the recovery of the total saikosaponins from the extract. The effects of initial concentration, air flow rate, liquid loading volume, pH, and operating time on the process performance were investigated. The recovery percentage 77.2% and an enrichment ratio 3.68 of total saikosaponins with one-stage separation were obtained under the optimal conditions of initial saikosaponin concentration 0.18 mg/mL, air flow rate 50 mL/min, liquid loading volume 200 mL, pH 5.5, and operating time of 2 h. A two-stage foam fractionation technology was also designed, which was effective for improving both the recovery percentage and enrichment ratio simultaneously.     

Concentration and separation of glycyrrhizic acid by foam separation

By the aid of the surface activities of glycyrrhizic acid, foam separation can be used to extract and concentrate it. The effects of operating parameters such as flow rate of air, initial feed concentration, pH and ionic strength on the enrichment ratio and recovery yield of glycyrrhizic acid are investigated in detail. In addition, the influences of other surface‐active substances in solution, such as proteins, on the separation of glycyrrhizic acid are also discussed. The experimental results show that foam separation is a simple and effective method to separate and concentrate glycyrrhizic acid. © 2002 Society of Chemical Industry     

连续泡沫分离塔回收水溶液中钼(Ⅵ)的研究

以十六烷基三甲基氯化铵为表面活性剂,在连续稳态操作条件下,研究了泡沫塔和填料泡沫塔回收水溶液中微量Mo(Ⅵ)的分离性能。结果表明:随鼓泡区高度的增加,泡沫塔的富集率逐渐增加,回收率逐渐减小;随填料层高度的增加,填料泡沫塔的回收率增加,富集率减小;随泡沫层高度的增加,两种塔的富集率均逐渐增加,回收率均逐渐减小。泡沫塔内的浓度分布基本一致,表明泡沫塔存在较大的液相返混,填料泡沫塔内浓度分布随填料层高度的增加而增大,表明填料泡沫塔的液相返混程度较泡沫塔小。填料的加入有效增大了气液传质面积,提高了气液传质速率。填料泡沫塔的回收率远高于泡沫塔,但富集比略有下降。在实验条件范围内,填料泡沫塔中Mo(Ⅵ)的回收率可达99.8%,富集率可达12.2。     

泡沫分离法回收酶法生产生物柴油中的液体脂肪酶

采用泡沫分离法对酶法生产生物柴油过程中的水相脂肪酶进行回收并富集. 通过正交实验考察了液体脂肪酶溶液中pH值、通气速度、初始酶浓度对富集比、酶蛋白回收率和酶活回收率的影响. 结果表明,气速10 L/(L×h)、进料酶浓度0.2 g/L及pH 7.0时蛋白回收率和酶活回收率接近100%,相应的富集比为3.67;初始酶浓度对富集比和蛋白回收率有显著影响,回收过程中脂肪酶活性无损失. 甲醇的存在能显著提高回收速率,甘油的存在降低了富集比,而生物柴油的存在影响了泡沫的稳定性,要形成稳定的泡沫,生物柴油含量需小于0.01%.     

Intensified Effect of Reduced Pressure on the Foam Fractionation Process of Bovine Serum Albumin

A novel method to intensify the foam fractionation process by operating the column under reduced pressure was reported in this paper. It was found that a poorer foam stability, a bigger mean bubble size and a wider bubble size distribution in the foam layer, a less upward liquid flux and volumetric liquid fraction at the top of the foam layer, and a higher enrichment ratio but a lower mass recovery of the foam fractionation process were obtained under reduced pressures compared to the ones under atmospheric pressure. The most important effect of the reduced pressure on the foam layer during the foam fractionation process is the encouraged bubble coalescence process which was exhibited by those unusual foam properties discussed above. The limitations of this new method were also discussed.     

Removal of Trace Cd2+ Using Continuous Multistage Ion Foam Fractionation: Part II—The Effects of Operational Parameters

A multistage ion foam fractionation column with bubble-cap trays was employed to study the removal of cadmium ions from simulated wastewater having low Cd concentrations (10–30 mg/L), examining the effects of foam height, air flow rate, feed flow rate, and feed Cd concentration. Sodium dodecyl sulfate (SDS) was used to generate foam in this study. An increase in foam height, which reduces liquid hold-up in the generated foam, resulted in the enhancement of the enrichment ratios of both SDS and Cd while the removal and residual factor of Cd showed insignificant change. An increase in air flow rate increased the foam generation rate, foamate volumetric ratio, and the removal efficiency of Cd but decreased the enrichment ratios of both Cd and SDS. The separation factors of both Cd and SDS decreased with increasing feed flow rate, which is mainly attributable to both the effects of the enhancement of foamate volumetric ratio and the increases in both SDS and Cd input rates. An increase in feed Cd concentration was found to increase Cd effluent concentration and SDS removal but to decrease the enrichment ratios of both Cd and SDS because of the increasing liquid entrainment in the produced foam.     

泡沫相塔壁对泡沫分离牛血清蛋白分离性能的影响

In order to enhance foam drainage, the column with an inner sleeve in the foam phase was designed for studying effect of the column wall of foam phase on foam separation performances using bovine serum albumin(BSA) as the research system. The effects of the wall on the liquid holdup out of the top column, bubble size, enrichment and recovery percentage were investigated. The results indicated that the experimental column with the inner sleeve decreased the liquid holdup, accelerated the coarsening and coalescence of bubbles and increased enrichment of BSA compared the contrasted column without the inner sleeve. Under the conditions of the initial concentration 0.2 g?L-1 of BSA, air flow rate 400 ml?min-1, the experimental column achieved up to a 2.06 fold increase in enrichment compared to the contrasted column. The enrichment of BSA increased with the increase of inner sleeve length. Channel theoretical analysis showed that the ratio of exterior channels to interior channels increased with the increase of bubble diameter. So the experiment column obtained the better performances at the lower concentration and the lower air flow rate. The better performances obtained by experimental column showed that the drainage rate of plateau borders on wall was greater than that of plateau borders between bubbles. So the inner sleeve provided more plateau borders on wall and improved foam drainage.