CN114019054B - Method for calculating concentration of traditional Chinese medicine components in nanofiltration membrane interface layer - Google Patents
Method for calculating concentration of traditional Chinese medicine components in nanofiltration membrane interface layer Download PDFInfo
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Abstract
Description
技术领域technical field
本发明涉及一种中药成分在纳滤膜界面层浓度的计算方法，具体涉及基于中药成分纳滤分离通过界面传质实现分离的模式计算成分在纳滤膜界面层的浓度，属于医药领域。The invention relates to a method for calculating the concentration of traditional Chinese medicine components in the interface layer of nanofiltration membranes, in particular to calculating the concentration of components in the interface layer of nanofiltration membranes based on the mode of nanofiltration separation of Chinese medicine components to achieve separation through interface mass transfer, and belongs to the field of medicine.
背景技术Background technique
界面的存在是产生一切界面现象的根源，因此从19世纪Gibbs对界面层对非均匀相物质的平衡条件展开了讨论，也引起了两相界面、界面层(界面区)的分析方法和理论模型的的广泛关注。目前在界面化学领域，对两相界面层的成分浓度分布主要有三种主流认识，Gibbs分割表面型界面层模型：认为在不同的两相接触时，相交的两相的能量、熵、密度、浓度等性质参数在各相内部一直到物理界面都是均一的。Guggenheim过渡层型界面层模型：认为界面层是一个具有一定体积和一定内容的热力学实体。且界面层中物质的分布并不是均匀的。双界面层模型：相交的两相均有自己的界面层，且各自的热力学参数不同，相1中成分的浓度随着从相2内部向界面层过渡，其浓度发生变化，但是在靠近相2时浓度逐渐平稳。The existence of the interface is the root of all interface phenomena. Therefore, in the 19th century, Gibbs discussed the equilibrium conditions of the interface layer to the heterogeneous phase substance, which also led to the analysis methods and theoretical models of the two-phase interface and the interface layer (interface region). widespread attention. At present, in the field of interface chemistry, there are mainly three mainstream understandings of the composition concentration distribution of the two-phase interface layer. The Gibbs split surface interface layer model: it is considered that when two different phases are in contact, the energy, entropy, density, and concentration of the intersecting two phases The parameters of such properties are uniform within each phase up to the physical interface. Guggenheim transition layer interface layer model: the interface layer is considered to be a thermodynamic entity with a certain volume and a certain content. And the distribution of substances in the interface layer is not uniform. Double interface layer model: the two intersecting phases have their own interface layer, and their thermodynamic parameters are different. The concentration of the components in phase 1 changes with the transition from the interior of phase 2 to the interface layer, but when it is close to phase 2 concentration gradually stabilized.
不同相接触时，接触处存在一层为两相分子相互渗透的分子非均匀分布层，其中以合金为代表的两相界面层物化性质评价相对容易，因为合金的界面层相对固定。而液固两相产生的界面层是相对于正在流动的流体在固体周围或表面形成的一薄层流体，是溶液与固体接触后产生的过渡层，其物化性质有别于溶液与固体两相，厚度在几纳米到几微米之间，因难以直接获得界面层的流体，所以无法实现界面层成分组成的定量分析。When different phases are in contact, there is a layer of non-uniform distribution of molecules in which the molecules of the two phases penetrate each other. The physical and chemical properties of the two-phase interface layer represented by the alloy are relatively easy to evaluate because the interface layer of the alloy is relatively fixed. The interface layer produced by the liquid-solid two-phase is a thin layer of fluid formed around or on the surface of the solid relative to the flowing fluid. , the thickness is between several nanometers and several micrometers, because it is difficult to directly obtain the fluid of the interface layer, so the quantitative analysis of the composition of the interface layer cannot be realized.
在中药成分纳滤分离过程中，纳滤膜的孔径分布在100～1000Da范围内，直径在纳米范围内，与两相接触后产生的界面层厚度接近，因此在进行纳滤分离时需要提供足够的跨膜压力差才能推动界面层进入膜孔径进而实现分离。因此纳滤分离是以界面传质为基础实现的分离过程，基于此为液-固两相界面层的溶质浓度计算提供了理论支撑。In the nanofiltration separation process of traditional Chinese medicine ingredients, the pore size distribution of the nanofiltration membrane is in the range of 100-1000 Da, the diameter is in the nanometer range, and the thickness of the interface layer produced after contacting with the two phases is close. Therefore, it is necessary to provide enough for nanofiltration separation. The transmembrane pressure difference is necessary to push the interface layer into the membrane pores to achieve separation. Therefore, nanofiltration separation is a separation process based on interfacial mass transfer, which provides theoretical support for the calculation of solute concentration in the liquid-solid two-phase interface layer.
基于上述背景，本发明提供一种中药成分在纳滤膜界面层浓度的计算方法，创新性地为解明液-固两相界面层溶质分布行为提供了技术手段，且有助于分析两相接触后，溶质分布的趋向性，从而阐明纳滤膜的污染机制。也有助于借助这种分布的趋向性对复杂溶液环境性下的成分进行定向分离、研发新颖的膜材质。Based on the above background, the present invention provides a method for calculating the concentration of traditional Chinese medicine ingredients in the interface layer of nanofiltration membranes, which innovatively provides a technical means for clarifying the solute distribution behavior of the liquid-solid two-phase interface layer, and is helpful for the analysis of two-phase contact. Finally, the tendency of the solute distribution can be used to clarify the fouling mechanism of the nanofiltration membrane. It is also helpful to use this distribution tendency to directional separate components in complex solution environments and to develop novel membrane materials.
发明内容Contents of the invention
发明目的：本发明的目的是提供一种中药成分在纳滤膜界面层浓度的计算方法，可用于分析液-固两相界面层溶质分布特征。Purpose of the invention: The purpose of the invention is to provide a method for calculating the concentration of traditional Chinese medicine components in the nanofiltration membrane interface layer, which can be used to analyze the distribution characteristics of the solute in the liquid-solid two-phase interface layer.
本发明的另一个目的是提供这种中药成分在纳滤膜界面层浓度的计算方法在分析膜污染机制、成分与膜材质的亲和性方面的应用。Another object of the present invention is to provide the application of the method for calculating the concentration of traditional Chinese medicine components in the interface layer of the nanofiltration membrane in the analysis of the membrane fouling mechanism and the affinity between the components and the membrane material.
技术方案：一种中药成分在纳滤膜界面层浓度的计算方法，包含以下步骤：a.将待评价的纳滤膜和中药成分置于分离系统中，检测溶液中待分析中药成分的浓度C0；b.将步骤a中的中药溶液采用膜分离，调节跨膜压力差在0.05～2.0MPa范围内，分别收集相应跨膜压力差下的膜通量(J)和成分截留率(R)数据；c.根据步骤b中系列跨膜压力差下的J和R，根据式(1)计算膜分离系数k，通过对ln[(1-R)·J/R]和J线性回归，其中为线性方程的截距，斜率为1/kTechnical solution: a method for calculating the concentration of Chinese medicine components in the nanofiltration membrane interface layer, comprising the following steps: a. placing the nanofiltration membrane and Chinese medicine components to be evaluated in a separation system, and detecting the concentration C of the Chinese medicine components to be analyzed in the solution 0 ; b. the traditional Chinese medicine solution in the step a is separated by a membrane, and the transmembrane pressure difference is adjusted within the range of 0.05 to 2.0 MPa, and the membrane flux (J) and component retention rate (R) under the corresponding transmembrane pressure difference are collected respectively Data; c. according to J and R under the series transmembrane pressure difference in step b, calculate membrane separation coefficient k according to formula (1), by linear regression to ln[(1-R) J/R] and J, wherein is the intercept of the linear equation with a slope of 1/k
d.根据步骤c中计算得到的分离系数k，根据式(2)计算膜界面层待分析中药成分的浓度Cm d. According to the separation coefficient k calculated in step c, calculate the concentration C m of the Chinese medicine component to be analyzed in the membrane interface layer according to formula (2)
所述步骤b中跨膜压力差需要选择3个以上跨膜压力差值。In the step b, the transmembrane pressure difference needs to select more than 3 transmembrane pressure difference values.
所述的步骤b中成分截留率(R)的计算方法为R＝截留液溶质浓度/原液溶质浓度。The calculation method of the component rejection rate (R) in the step b is R=retentate solute concentration/stock solution solute concentration.
所述步骤c中线性方程的回归系数≥0.99。The regression coefficient of the linear equation in the step c is ≥0.99.
一种中药成分在纳滤膜界面层浓度的计算方法，可以用于分析中药成分的膜污染特征、中药成分与膜材质的亲和性。A method for calculating the concentration of traditional Chinese medicine ingredients in the interface layer of nanofiltration membranes can be used to analyze the membrane fouling characteristics of traditional Chinese medicine ingredients and the affinity between traditional Chinese medicine ingredients and membrane materials.
一种中药成分在纳滤膜界面层浓度的计算方法，适用于水溶液和有机溶液。A method for calculating the concentration of traditional Chinese medicine ingredients in the interface layer of nanofiltration membranes is applicable to aqueous solutions and organic solutions.
有益效果：(1)解决液-固两相界面层因无法直接获取，难以进行溶质成分浓度分析的技术瓶颈。(2)根据界面层成分浓度分布情况，直观分析成分与膜材质的亲和性，以及分析膜产生污染的根本原因。(3)有助于研发新的膜材质，调整不同中药成分在界面层分布的浓度差异，放大分离差异，进行目的性分离。Beneficial effects: (1) Solve the technical bottleneck that the liquid-solid two-phase interface layer cannot be directly obtained and it is difficult to analyze the concentration of solute components. (2) According to the concentration distribution of the interface layer components, intuitively analyze the affinity between the components and the membrane material, and analyze the root cause of the membrane fouling. (3) It is helpful to develop new membrane materials, adjust the concentration difference of different traditional Chinese medicine components distributed in the interface layer, amplify the separation difference, and perform purposeful separation.
具体实施方式Detailed ways
以下通过实施例形式，对本发明的上述内容再作进一步的详细说明，但不应将此理解为本发明上述主题的范围仅限于以下的实例，凡基于本发明上述内容所实现的技术均属于本发明的范围。Below by embodiment form, above-mentioned content of the present invention is described in further detail again, but this should not be interpreted as the scope of the above-mentioned theme of the present invention being limited to following examples, all technologies realized based on the above-mentioned content of the present invention all belong to this invention the scope of the invention.
实施例1金银花水提取液中绿原酸在复合聚酰胺纳滤膜界面层中的浓度The concentration of chlorogenic acid in the composite polyamide nanofiltration membrane interface layer in the honeysuckle water extract of embodiment 1
称取金银花水提液，采用高效液相色谱法检测，色谱条件如下：Waters e2695高效液相色谱仪，全波长紫外检测器，Welch ultimate C18色谱柱，乙腈-0.5％磷酸(v/v 30∶70)，体积流量1.0mL/min，柱温30℃，检测波长340m，采用外标一点法计算金银花药材水提液中绿原酸浓度为112.02μg/mL，将300Da的复合聚酰胺纳滤膜和金银花水提液置于分离系统中，调节跨膜压力差为0.2、0.5、0.8、1.0、1.5、2.0MPa，分别收集相应跨膜压力差下的膜通量(J)和成分截留率(R)数据。Take honeysuckle aqueous extract, adopt high performance liquid chromatography to detect, chromatographic condition is as follows: Waters e2695 high performance liquid chromatography, full-wavelength ultraviolet detector, Welch ultimate C 18 chromatographic column, acetonitrile-0.5% phosphoric acid (v/v 30 : 70), volumetric flow rate 1.0mL/min, column temperature 30°C, detection wavelength 340m, using the external standard point method to calculate the concentration of chlorogenic acid in the water extract of honeysuckle medicinal material to be 112.02μg/mL, the 300Da composite polyamide nanofiltration The membrane and honeysuckle water extract were placed in the separation system, and the transmembrane pressure difference was adjusted to 0.2, 0.5, 0.8, 1.0, 1.5, 2.0MPa, and the membrane flux (J) and component rejection rate were collected under the corresponding transmembrane pressure difference (R) Data.
根据系列跨膜压力差下的J和R，根据式(1)计算膜分离系数k。According to J and R under a series of transmembrane pressure differences, the membrane separation coefficient k is calculated according to formula (1).
通过对ln[(1-R)·J/R]和J线性回归，其中为线性方程的截距，斜率为1/k。拟合ln[(1-R)·J/R]和J的线性方程为：/>回归系数为0.9920。By linear regression on ln[(1-R) J/R] and J, where is the intercept of the linear equation with a slope of 1/k. The linear equation for fitting ln[(1-R) J/R] and J is: /> The regression coefficient is 0.9920.
根据计算得到的分离系数k，根据式(2)计算膜界面层绿原酸的浓度Cm。According to the calculated separation coefficient k, the concentration C m of chlorogenic acid in the membrane interface layer was calculated according to formula (2).
Cm＝115.02μg/mL，说明界面层中绿原酸浓度高于溶液本体浓度，绿原酸易接近复合聚酰胺材质纳滤膜。C m =115.02 μg/mL, indicating that the concentration of chlorogenic acid in the interface layer is higher than that of the bulk solution, and chlorogenic acid is easily accessible to the nanofiltration membrane made of composite polyamide.
实施例2绿原酸单体化合物在复合聚酰胺纳滤膜界面层中的浓度The concentration of embodiment 2 chlorogenic acid monomer compound in composite polyamide nanofiltration membrane interface layer
配制浓度为112.0μg/mL的绿原酸水溶液采用300Da的复合聚酰胺纳滤膜进行分离，调节跨膜压力差为0.2、0.5、0.8、1.0、1.5、2.0MPa，分别收集相应跨膜压力差下的膜通量(J)，并采用实施例1中的液相检测方法测定并计算成分截留率(R)数据。Prepare a chlorogenic acid aqueous solution with a concentration of 112.0 μg/mL and use a 300 Da composite polyamide nanofiltration membrane for separation, adjust the transmembrane pressure difference to 0.2, 0.5, 0.8, 1.0, 1.5, and 2.0 MPa, and collect the corresponding transmembrane pressure differences Under the membrane flux (J), and using the liquid phase detection method in Example 1 to measure and calculate the component rejection rate (R) data.
根据系列跨膜压力差下的J和R，根据式(1)计算膜分离系数k。According to J and R under a series of transmembrane pressure differences, the membrane separation coefficient k is calculated according to formula (1).
通过对ln[(1-R)·J/R]和J线性回归，其中为线性方程的截距，斜率为1/k。拟合ln[(1-R)·J/R]和J的线性方程为：/>回归系数为0.9908。By linear regression on ln[(1-R) J/R] and J, where is the intercept of the linear equation with a slope of 1/k. The linear equation for fitting ln[(1-R) J/R] and J is: /> The regression coefficient is 0.9908.
根据计算得到的分离系数k，根据式(2)计算膜界面层绿原酸的浓度Cm。According to the calculated separation coefficient k, the concentration C m of chlorogenic acid in the membrane interface layer was calculated according to formula (2).
Cm＝143.02μg/mL，说明界面层中绿原酸浓度高于溶液本体浓度，对比实施例1中金银花提取液在纳滤膜界面层的浓度，可以看出单一化合物的绿原酸在界面层中的浓度高于金银花提取液，说明金银花提取液中其他成分低于绿原酸进入界面层具有竞争作用。C m =143.02 μg/mL, indicating that the concentration of chlorogenic acid in the interface layer is higher than the concentration of the solution body, and comparing the concentration of the honeysuckle extract in the interface layer of the nanofiltration membrane in Example 1, it can be seen that the chlorogenic acid of a single compound is at the interface The concentration in the layer is higher than that of the honeysuckle extract, indicating that other components in the honeysuckle extract are lower than the chlorogenic acid and have a competitive effect in entering the interface layer.
实施例3苦参中苦参碱和氧化苦参碱在纳滤膜界面层中的浓度The concentration of matrine and oxymatrine in the interface layer of nanofiltration membrane in embodiment 3 Sophora flavescens
称取苦参药材1.0kg，分别加10倍水提取2次，每次1小时，合并提取液，微孔滤膜过滤，得苦参提取液，采用高效液相色谱法检测，色谱条件如下：Waters e2695高效液相色谱仪，全波长紫外检测器，Agilent NH2色谱柱，乙腈-无水乙醇-3％磷酸(v/v/v 80∶10∶10)，体积流量1.0mL/min，柱温25℃，检测波长220nm，采用外标一点法计算苦参药材水提液中苦参碱浓度为0.46μg/mL、氧化苦参碱浓度为0.53μg/mL。Weigh 1.0 kg of Sophora flavescens medicinal material, add 10 times of water to extract twice, each time for 1 hour, combine the extracts, and filter through a microporous membrane to obtain Sophora flavescens extract, which is detected by high performance liquid chromatography, and the chromatographic conditions are as follows: Waters e2695 high-performance liquid chromatography, full-wavelength UV detector, Agilent NH 2 chromatographic column, acetonitrile-absolute ethanol-3% phosphoric acid (v/v/v 80:10:10), volume flow 1.0mL/min, column The temperature is 25°C, the detection wavelength is 220nm, and the concentration of matrine in the water extract of Sophora flavescens medicinal materials is calculated by using the external standard one-point method to be 0.46 μg/mL, and the concentration of oxymatrine to be 0.53 μg/mL.
采用500Da的聚丙烯腈纳滤膜进行分离，调节跨膜压力差为0.2、0.5、0.8、1.0、1.5、2.0MPa，分别收集相应跨膜压力差下的膜通量(J)并计算苦参碱和氧化苦参碱的截留率(R)数据。A 500Da polyacrylonitrile nanofiltration membrane was used for separation, and the transmembrane pressure difference was adjusted to 0.2, 0.5, 0.8, 1.0, 1.5, and 2.0 MPa, and the membrane flux (J) under the corresponding transmembrane pressure difference was collected and calculated for Sophora flavescens Retention (R) data for base and oxymatrine.
根据系列跨膜压力差下的J和R，根据式(1)计算膜分离系数k。According to J and R under a series of transmembrane pressure differences, the membrane separation coefficient k is calculated according to formula (1).
通过对ln[(1-R)·J/R]和J线性回归，其中为线性方程的截距，斜率为1/k。拟合ln[(1-R)·J/R]和J的线性方程为：By linear regression on ln[(1-R) J/R] and J, where is the intercept of the linear equation with a slope of 1/k. The linear equation for fitting ln[(1-R) J/R] and J is:
苦参碱：回归系数为0.9910。Matrine: The regression coefficient is 0.9910.
氧化苦参碱：回归系数为0.9906。Oxymatrine: The regression coefficient is 0.9906.
根据计算得到的分离系数k，根据式(2)计算膜界面层苦参碱和氧化苦参碱的浓度Cm。According to the calculated separation coefficient k, the concentration C m of matrine and oxymatrine in the membrane interface layer was calculated according to formula (2).
苦参碱Cm＝0.41μg/mL，氧化苦参碱Cm＝0.36μg/mL，在苦参水提液中，聚丙烯腈纳滤膜界面层中苦参碱浓度高于氧化苦参碱，说明苦参碱更容易进入界面层，从而透过纳滤膜。Matrine C m =0.41μg/mL, oxymatrine C m =0.36μg/mL, in the water extract of matrine, the concentration of matrine in the interface layer of polyacrylonitrile nanofiltration membrane is higher than that of oxymatrine , indicating that matrine is more likely to enter the interface layer, thereby passing through the nanofiltration membrane.
实施例4乙醇溶液环境下苦参中苦参碱和氧化苦参碱在纳滤膜界面层中的浓度The concentration of matrine and oxymatrine in the interface layer of nanofiltration membrane in Sophora flavescens under the environment of embodiment 4 ethanol solution
称取苦参药材1.0kg，分别加10倍乙醇提取2次，每次1小时，合并提取液，微孔滤膜过滤，得苦参乙醇提取液，采用高效液相色谱法检测，色谱条件如下：Waters e2695高效液相色谱仪，全波长紫外检测器，Agilent NH2色谱柱，乙腈-无水乙醇-3％磷酸(v/v/v 80∶10∶10)，体积流量1.0mL/min，柱温25℃，检测波长220nm，采用外标一点法计算苦参药材水提液中苦参碱浓度为0.54μg/mL、氧化苦参碱浓度为0.61μg/mL。Weigh 1.0 kg of Sophora flavescens medicinal material, add 10 times of ethanol to extract twice, each time for 1 hour, combine the extracts, and filter through a microporous membrane to obtain Sophora flavescens ethanol extract, which is detected by high performance liquid chromatography, and the chromatographic conditions are as follows : Waters e2695 high performance liquid chromatograph, full-wavelength UV detector, Agilent NH 2 chromatographic column, acetonitrile-absolute ethanol-3% phosphoric acid (v/v/v 80:10:10), volume flow rate 1.0mL/min, The column temperature is 25°C, the detection wavelength is 220nm, and the concentration of matrine and oxymatrine in the aqueous extract of Sophora flavescens is calculated as 0.54 μg/mL and 0.61 μg/mL by the external standard one-point method.
采用500Da的聚丙烯腈纳滤膜进行分离，调节跨膜压力差为0.2、0.5、0.8、1.0、1.5、2.0MPa，分别收集相应跨膜压力差下的膜通量(J)并计算苦参碱和氧化苦参碱的截留率(R)数据。A 500Da polyacrylonitrile nanofiltration membrane was used for separation, and the transmembrane pressure difference was adjusted to 0.2, 0.5, 0.8, 1.0, 1.5, and 2.0 MPa, and the membrane flux (J) under the corresponding transmembrane pressure difference was collected and calculated for Sophora flavescens Retention (R) data for base and oxymatrine.
根据系列跨膜压力差下的J和R，根据式(1)计算膜分离系数k。According to J and R under a series of transmembrane pressure differences, the membrane separation coefficient k is calculated according to formula (1).
通过对ln[(1-R)·J/R]和J线性回归，其中为线性方程的截距，斜率为1/k。拟合ln[(1-R)·J/R]和J的线性方程为：By linear regression on ln[(1-R) J/R] and J, where is the intercept of the linear equation with a slope of 1/k. The linear equation for fitting ln[(1-R) J/R] and J is:
苦参碱：回归系数为0.9908。Matrine: The regression coefficient is 0.9908.
氧化苦参碱：回归系数为0.9924。Oxymatrine: The regression coefficient is 0.9924.
根据计算得到的分离系数k，根据式(2)计算膜界面层苦参碱和氧化苦参碱的浓度Cm。According to the calculated separation coefficient k, the concentration C m of matrine and oxymatrine in the membrane interface layer was calculated according to formula (2).
苦参碱Cm＝0.47μg/mL，氧化苦参碱Cm＝0.72μg/mL，相较于水溶液环境，在苦参乙醇提液中，苦参碱和氧化苦参碱的k值相对下降，均聚丙烯腈纳滤膜界面层中氧化苦参碱浓度明显高于苦参碱，说明乙醇溶液环境与聚丙烯腈构成的界面层，氧化苦参碱更容易进入而透过纳滤膜。Matrine C m ＝0.47μg/mL, oxymatrine C m ＝0.72μg/mL, compared with the aqueous solution environment, in the matrine ethanol extract, the k value of matrine and oxymatrine decreased relatively , the concentration of oxymatrine in the interface layer of polyacrylonitrile nanofiltration membrane was significantly higher than that of matrine, indicating that the interface layer composed of ethanol solution environment and polyacrylonitrile, oxymatrine is more likely to enter and pass through the nanofiltration membrane.
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