Centrifugal partition chromatography extraction unit, rotor equipped with such extraction unit and use thereof in centrifugal partition chromatography device

Abstract

The invention relates to a centrifugal partition chromatography extraction unit structure (5) and a centrifugal partition chromatography extraction unit (1) comprising such an extraction unit wall structure, as well as to a method for manufacturing such a structure, in which each serrated member (6) is prismatic, preferably triangular-base prismatic; the centrifugal partition chromatography extraction unit structure (5) comprises at least two sawtooth-shaped components (6), and the sawtooth-shaped components (6) are arranged in the centrifugal partition chromatography extraction unit wall structure (5) in parallel. The invention also relates to a rotor of a centrifugal partition chromatography device comprising the centrifugal partition chromatography extraction unit (1), and to a centrifugal partition chromatography device comprising such a rotor.

Description

TECHNICAL FIELD

[0001] The present invention relates to a centrifugal partition chromatography extraction cell, in particular to a cell wall structure thereof.

[0002] The present invention also relates to a centrifugal partition chromatography rotor, a centrifugal partition chromatography apparatus comprising the rotor, a centrifugal partition chromatography extraction cell and use of the rotor in a centrifugal partition chromatography apparatus, and to a chromatographic method performed using a centrifugal partition chromatography extraction cell. BACKGROUND

[0003] In the chemical industry and other industries involving or using chemical materials, it is often necessary to separate mixtures into their constituent parts, such methods are collectively referred to as separation techniques.

[0004] It is important to note that the distinction between industrial and analytical methods is not absolute: analytical methods can be applied partially or completely to industrial methods, and vice versa. Analytical separation techniques encompass physicochemical methods, including chromatography. Chromatography is a separation technique based on the difference in the transfer of substances between a stationary phase and a mobile phase. The components of the mixture to be separated (i.e. the sample) can interact differently with the stationary and mobile phases, in other words, each component has a different retention characteristic in the stationary phase and in the mobile phase.

[0005] The present specification relates to liquid-liquid chromatography, in particular centrifugal partition chromatography, and is mainly concerned with the extraction cell used in this method. In liquid-liquid chromatography (LLC for short in the literature), both the stationary and mobile phases are liquids, and the two liquids are essentially immiscible. The components of the sample to be separated also differ in their distribution between the two liquids; the transfer of matter occurs at the interface between the two liquids.

[0006] Liquid-liquid chromatography in which the liquid phase solvent or multi-component solvent mixture is formed into a stationary phase by the action of centrifugal force, and the mobile phase is also a liquid, is called centrifugal partition chromatography, abbreviated to CPC in the literature.

[0007] The original form of partition chromatography was the Craig apparatus invented by Lyman C. Craig in 1943, which is based on the principle of countercurrent distribution, abbreviated to the CCD apparatus [Craig, L.C.; Post, O., Anal. Chem., 1949, 21(4), 500-504.].

[0008] Droplet countercurrent chromatography technology emerged in the 1970s, in which the liquid stationary phase is placed in a series of vertically connected glass columns, and the mobile phase flows through the columns in the form of droplets [Tanimura, T.; Pisano, J. J.; Ito, Y.; Bowman, R. L., 1970, Droplet countercurrent chromatography, Science, 169(3940), 54-56.]. Initially, the stationary phase was immobilized by gravity.

[0009] It was not until the 1980s that centrifugal force was first used to form an immobilized stationary phase in a liquid-liquid separation device. Through centrifugal partition chromatography technology, higher flow rates were achieved, resulting in a separation method that is faster and more efficient in production, which can also be applied to industrial fields.

[0010] A variety of chromatography devices using centrifugal force are known in the art.

[0011] Patent application WO21259577A1 discloses a universal rotor that can be applied to all systems that perform liquid centrifugal acceleration. The rotor contains a plurality of cells arranged in a radial (i.e., the cell longitudinal axis is consistent with the radius) or inclined (i.e., the cell longitudinal axis is at an angle to the radius) manner.

[0012] Patent application EP3204136A1 discloses an extraction cell that can be used for centrifugal partition chromatography and a method for manufacturing the same. The extraction cell has a tubular structure, and a liquid inlet plug and a liquid outlet plug are connected to the inlet and outlet ends of the cell, respectively. A liquid-permeable insert can be placed in the extraction cell, which can reduce the harmful turbulence caused by the Coriolis force and increase the mass transfer surface area between the two phases (stationary phase and mobile phase). The insert can have a regular or irregular structure, and can also be a monolithic insert. According to one embodiment of the extraction cell, the opposite walls of the cell are roughened (e.g., in a stepped or jagged structure). It should be noted that the insert placed in the cell can be compressed by the centrifugal force, resulting in a decrease in separation efficiency.

[0013] Patent application WO2017072542A1 discloses a method for purifying cyclosporin. The patent application Figure 5 It can be seen that the walls of the extraction cell are roughened, and the rough structure is preferably a stepped or jagged structure.

[0014] Patent application US2013005556AA relates to a device and a method in which immiscible liquid phases are brought into contact under the action of centrifugal force. The device contains at least one cell for contacting the liquids, and according to the description, the cell can be rotated about the X'X axis and contains a plurality of cells.

[0015] Patent application WO13036803A discloses a coated rotor that can be used for preparative centrifugal thin-layer chromatography.

[0016] Patent application number US2008035546A1 relates to a method for optimizing the size design of the unit chamber of a centrifugal partition chromatograph.

[0017] The centrifugal partition chromatograph rotor disclosed in patent application number US2004173534AA comprises at least one thick-walled cylinder containing multiple units connected in series (even hundreds of long units). This rotating device can withstand pressures exceeding 100 bar, meaning it can also function well in industrial applications.

[0018] European Patent EP1166100B1 relates to a centrifugal partition chromatography apparatus comprising at least one rotor disk rotatable about an axis, wherein a plurality of units are connected in series via channels within the rotor disk.

[0019] Patent application FR2883770A1 differs from the former (EP1166100B1) in its internal structure. Opposite baffles are formed inside the unit, oriented perpendicular to the unit's longitudinal axis. In other words, due to the presence of the baffles, the liquid flowing through the unit no longer follows the hollow unit space, but flows along channels formed by the internal shape (see Figures 15 and 16 of patent application FR288377A1), thereby improving the separation effect. The device disclosed in this application can achieve not only preparative liquid-liquid separation but also industrial-scale applications. The baffles within the extraction unit are designed to extend the liquid flow path, thereby improving the separation effect.

[0020] Patent application number US4877523A relates to a centrifugal countercurrent partition chromatography apparatus. This apparatus is suitable for the detection, separation, and purification (i.e., quantitative or qualitative analysis) of biochemical materials or natural organic compounds, as well as the purification of raw material samples. Its subject matter is highly similar to patent application number JP56016868A2.

[0021] The invention described in patent application number US2009173680 relates to a continuous countercurrent chromatography system suitable for substance separation and / or purification. The core of this invention lies in making the then-known countercurrent chromatography technology continuous. It solves the technical challenge by arranging multiple interconnected rotating units in a ring on a disk-like structure. The two liquids used within the unit are delivered in a countercurrent manner, thereby improving separation efficiency.

[0022] Japanese Patent Application No. JPS629270A relates to a subunit that can be used in a centrifugal partition chromatograph. The rotor of the device is cylindrical, with multiple so-called column units formed on its circumference, and adjacent units are interconnected.

[0023] Patent application number US2010200488A1 discloses a centrifugal partition chromatography column composed of stacked disks. The disks contain a three-dimensional network structure connected in series.

[0024] Currently, there are no centrifugal partition chromatography devices containing extraction units, whose extraction unit wall structures can more effectively mitigate the negative effects of tangential forces during industrial-scale purification. Therefore, this invention aims to provide a centrifugal partition chromatography device whose extraction unit employs a novel unit wall structure, achieving more efficient separation compared to existing extraction units and their unit wall structures.

[0025] The present invention also aims to create a centrifugal partition chromatography apparatus suitable for analytical and industrial-scale separation, wherein the ratio of stationary phase to mobile phase in the centrifugal partition chromatography extraction unit does not decrease even during scale-up production, and the ratio is maintained at at least 80%.

[0026] The above objectives were achieved by using a centrifugal partition chromatography apparatus with serrated components as the wall structure of the cavity unit. The function of the serrated components of this invention is to improve chromatographic separation efficiency by increasing the interfacial contact area for interphase mass transfer; at the same time, its structure reduces the "dead zone" that has no practical effect in the separation process, thereby reducing the amount of stationary phase required.

[0027] The serrated component placed within the extraction unit is key to achieving efficient chromatographic separation in the centrifugal partition chromatography apparatus of this invention.

[0028] We recognize that if the serrated components force the mobile phase flowing through the centrifugal partition chromatography extraction unit to flow along a trajectory different from the existing path, the length of the material flow path through the centrifugal partition chromatography device will increase, thereby improving production efficiency.

[0029] In other words, compared to existing centrifugal partition chromatography devices, the significant advantage of this invention lies in the increased material transfer surface area resulting from the serrated components. The extraction unit structure formed by the serrated components helps improve chromatographic efficiency. Existing extraction unit structures (mostly inserts) include metal mesh, steel wool, glass fiber, and silica gel packing materials. However, given the limited lifespan, cleaning difficulty, and potential breakage due to centrifugal forces in some cases, the serrated components of this invention are more advantageous—they do not deform under centrifugal forces. Furthermore, another significant advantage of this invention is that, compared to solutions disclosed in existing technical literature, the centrifugal partition chromatography extraction unit of this invention can achieve a longer material flow path length, thereby improving production efficiency, achieving a faster and more economical separation process, supporting process scale-up without affecting pressure resistance. The wall structure of the extraction unit in this invention gives the flow within the unit a distinct laminar flow characteristic, i.e., backmixing does not occur. Attached Figure Description

[0030] Figure 1 A perspective view showing a preferred embodiment of the wall structure of the centrifugal partition chromatography extraction unit in a centrifugal partition chromatography apparatus (extraction unit not shown).

[0031] Figure 2 This is a cross-sectional schematic diagram of the extraction unit in a centrifugal partition chromatography apparatus, wherein the wall structure of the extraction unit described in this invention is located inside the unit body.

[0032] Figure 3 A top view of a centrifugal partition chromatography extraction unit (excluding unit wall structure).

[0033] Figure 4 A perspective view of a preferred embodiment of the external and internal structure of a centrifugal partition chromatography extraction unit (excluding the unit wall structure).

[0034] Figure 5 A perspective view of a preferred embodiment of the external structure of a centrifugal dispensing chromatography extraction unit.

[0035] Figure 6 The results show a comparison between the centrifugal partition chromatography extraction unit and the tubular structure (including the unit wall structure formed by the serrated member of the present invention) disclosed in European patent application No. EP3204136A1 in the separation of p-hydroxybenzoic acid esters. Summary of the Invention

[0036] This invention relates to the structure of the wall of a centrifugal partition chromatography extraction unit, the extraction unit having at least two planar sidewalls, and i) The unit wall structure includes prismatic sawtooth members, preferably triangular-base prismatic members; ii) The wall structure of the centrifugal partition chromatography extraction unit contains at least two serrated members, and iii) Each serrated component is arranged parallel to the sidewall of any plane of the centrifugal partition chromatography extraction unit.

[0037] The number of serrated components in the wall structure of the centrifugal partition chromatography extraction cell is at least 2, at most 8, and preferably 6.

[0038] According to a preferred embodiment of the centrifugal partition chromatography extraction unit wall structure of the present invention, the serrated members are triangular-based prisms, and the prism sides of all the serrated members are located in the same plane as the triangular base, thereby forming one side plane of the centrifugal partition chromatography extraction unit wall.

[0039] In another preferred embodiment of the fine unit structure of centrifugal partition chromatography extraction according to the present invention, the serrated member is a triangular-base prism, wherein the included angle between the base of the triangle and any edge is between 40° and 80°, preferably 47.54°.

[0040] In another preferred embodiment of the centrifugal partition chromatography extraction unit wall structure according to the present invention, the serrated member is a triangular-base prism with a prism height between 160 mm and 200 mm, preferably 185 mm.

[0041] The present invention also relates to a centrifugal partition chromatography extraction unit having an internal structure in the shape of a racetrack prism, wherein the base of the racetrack prism preferably has a ratio of its major axis to its minor axis of at least 3:1, more preferably a major axis of 180 mm and a minor axis of 50 mm, and furthermore, the unit includes the unit wall structure described in the present invention on one of its two planar sides.

[0042] According to a preferred embodiment of the centrifugal partition chromatography extraction unit of the present invention, the top view section of the unit wall structure, when such a structure is not present, constitutes at least 68% and / or at most 90%.

[0043] In another preferred embodiment of the centrifugal partition chromatography extraction unit according to the present invention, at least one of the serrated members of the unit wall structure extends beyond the centerline of the unit body, and the direction of extension is parallel to the longitudinal edge of the member (here understood as the state without the unit wall structure).

[0044] The centrifugal partition chromatography extraction unit of the present invention, after removing the unit wall structure, has a volume of at least 1.5 ml and / or up to 1.3 liters.

[0045] The present invention also relates to a rotor for a centrifugal partition chromatography apparatus, the rotor comprising the centrifugal partition chromatography extraction unit of the present invention.

[0046] According to a preferred embodiment of the invention, one or more rotors include centrifugal partition chromatography extraction units, wherein the number of centrifugal partition chromatography extraction units on each rotor is between 30 and 100, and the total length of the chromatographic column is between 2.5 and 4.1 meters.

[0047] The present invention also relates to a centrifugal partition chromatography apparatus comprising one or more rotors designed according to the present invention.

[0048] The present invention also relates to a method for manufacturing a centrifugal partition chromatography extraction unit for use in a centrifugal partition chromatography apparatus, wherein the unit wall structure described in the present invention is placed inside or formed therein within the extraction unit. Detailed Implementation

[0049] In this specification, if a numerical value is given, it should be understood that the last digit of the value represents a precision range determined according to rounding rules. For example, 99.0% should be understood as a range of 98.95% to 99.04%.

[0050] In liquid-liquid chromatography (LLC), both the stationary phase and the mobile phase are liquids and are essentially immiscible. The components of the sample to be separated are distributed differently in the two phases, and mass transfer occurs at the interface between the two phases (stationary and mobile phases).

[0051] When the stationary phase is a denser phase and the mobile phase is a less dense phase, it is called ascending chromatography—in this case, the mobile phase flows from the outer edge of the rotation towards the center. Conversely, it is called descending chromatography—the stationary phase is a less dense phase and the mobile phase is a denser phase, and the mobile phase flows towards the center.

[0052] Liquid-liquid chromatography, which uses a centrifugal force field to form a stationary phase from a liquid solvent or a mixture of multiple components, and where the mobile phase is liquid, is called centrifugal partition chromatography (CPC). The apparatus that utilizes a centrifugal force field for separation (purification) is called a centrifugal partition chromatography apparatus. In this invention, a series of centrifugal partition chromatography extraction units located within the centrifugal partition chromatography apparatus are responsible for chromatographic separation.

[0053] The separation principle lies in the fact that when different components in a solution have different partition coefficients at the interface between the mobile and stationary phases, their mass transfer (adsorption / desorption) tendencies differ, resulting in different residence times for each component in different phases. In other words, chromatographic separation efficiency mainly depends on the size of the mass transfer surface between the stationary and mobile phases. If this transfer surface increases, the chromatographic separation efficiency also increases.

[0054] Figure 2 A cross-sectional view of the extraction unit of the present invention is shown. In the present invention, the centrifugal partition chromatography extraction unit 1 refers to a cavity unit enclosed by a unit wall, which includes one or more outlet pipe ends 3 and one or more inlet pipe ends 4, wherein two liquid phases are mixed therein, thereby achieving the separation of sample components. Figure 2 The unit wall structure 5 is shown, which is placed or processed within the centrifugal partition chromatography extraction unit 1.

[0055] like Figure 4 As shown, in terms of its design, the centrifugal partition chromatography extraction unit 1 of the present invention, when viewed from the outside, is preferably a prism with a rectangular base, and its interior has a cylindrical cavity shaped like a racetrack. That is, the part of the centrifugal partition chromatography extraction unit 1 that actually participates in separation, i.e., its internal structure, is precisely this racetrack-shaped cylindrical cavity. The so-called racetrack-shaped cylindrical internal structure refers to a prism with a racetrack-shaped base, whose height is preferably greater than the minor and major axes of the racetrack, and more preferably at least 2.7% greater than the major axis of the racetrack's base. The racetrack shape refers to a geometric shape formed by two parallel straight line segments connecting two relatively curved segments. The radius of the curved segments is variable, corresponding to the size of the extraction unit. The racetrack shape has two mutually perpendicular axes of symmetry, which, for simplicity, are referred to as the major axis and minor axis based on the principles of elliptical geometry.

[0056] The centrifugal partition chromatography extraction unit 1 can be made of the following materials: stainless steel and acid-resistant steel; polytetrafluoroethylene (PTFE); polyvinylidene fluoride (PVDF); polyether ether ketone (PEEK); high-density polyethylene (HDPE); titanium; graphite and carbon fiber composite materials. The extraction unit 1 described in this invention can typically withstand a maximum pressure of approximately 100 bar, and its operating pressure is typically between 5 and 50 bar. As those skilled in the art know, the centrifugal partition chromatography extraction units 1 connected in series are interconnected by pipes suitable for conveying liquids, i.e., the unit has an outlet pipe end 3 and an inlet pipe end 4 (opening). The inlet pipe end 4 and the outlet pipe end 3 are preferably tapered (see...). Figure 2 ).

[0057] A series of units arranged in this way in the rotor are suitable for allowing the solvent to flow under high pressure.

[0058] Compared with existing technical solutions, the significant advantage of the present invention is that by using the centrifugal partition chromatography extraction unit wall structure 5 in the extraction unit, a more efficient separation effect can be achieved.

[0059] This invention relates to, for example Figure 1 The shown structure is the wall structure 5 of the centrifugal partition chromatography extraction unit. This structure can be used in the centrifugal partition chromatography extraction unit 1, wherein the extraction unit has two planar walls, and i) The unit wall structure includes prism-shaped sawtooth members 6, preferably triangular-base prisms; ii) The wall structure 5 of the centrifugal partition chromatography extraction unit includes at least two serrated members 6, and iii) Each of the serrated components 6 is arranged parallel to one of the two planes of the centrifugal partition chromatography extraction unit.

[0060] like Figure 1 As shown, each serrated member 6 is prismatic. In this specification, "serrated" means that the part of the member protruding into the unit space has one or more edges, and the edges are not in close contact with the edges or sides of adjacent members, that is, the centrifugal partition chromatography extraction unit wall structure 5 is independently and freely positioned in space relative to other members. Figure 1 A centrifugal partition chromatography extraction unit wall structure 5 consisting of six serrated members 6 is shown. Although the number of serrated members 6 can be adjusted, it must be ensured that the centrifugal partition chromatography extraction unit wall structure 5 includes at least two serrated members 6 to achieve the effects described in this invention. Figure 1 As shown, the serrated members 6 are arranged in parallel on the unit wall structure, forming a plane ( Figure 1The sides of the left-hand side are in contact with each other. When using the centrifugal separation extraction unit wall structure 5 of the present invention, this structure is attached to the unit wall along this plane. It should be noted that the scope of protection of the present invention covers the case where there are gaps between the serrated members 6—in this case, the aforementioned plane may be formed not only by specific sides of the serrated members 6, but also by other structural elements (such as plate structures).

[0061] According to a preferred embodiment of the present invention, the serrated member 6 is in the shape of a triangular-based prism. This is because a triangular-based prism is the simplest geometric shape that enables the centrifugal partition chromatography extraction unit wall structure 5 to achieve the purpose of the invention. However, it should be noted that if the serrated members conform to the above definition when positioned relative to each other in the centrifugal partition chromatography extraction unit wall structure 5, then prisms based on other two-dimensional shapes can also be used as serrated members 6. Therefore, serrated members with rectangular, pentagonal, hexagonal, and star-shaped bases are also applicable.

[0062] The advantage of the centrifugal partition extraction unit wall structure 5 of this invention is that the above-described structure eliminates backmixing in unfilled extraction units, thereby improving chromatographic separation efficiency. Furthermore, if the material transfer surface area within the extraction unit is sufficiently increased, a smaller number of centrifugal partition extraction units 1 are needed to achieve the same separation efficiency. In this case, the serrated structure 6 prevents the mobile phase from adhering to the inner wall of the centrifugal partition extraction unit 1, thus expanding the mass transfer interface. These effects result in a reduction in the required number of centrifugal partition extraction units 1, making this approach even more advantageous—as it reduces the pressure drop experienced by the rotor.

[0063] An unexpected discovery regarding this invention is that when at least two serrated members 6 are arranged in parallel as the wall structure 5 of the centrifugal partition chromatography extraction unit, the negative impact of tangential forces during operation can be mitigated. As mentioned above, this centrifugal partition chromatography extraction unit wall structure 5 increases the internal surface area of ​​the unit by approximately 35-70%, and the mass transfer interface area also increases accordingly. Therefore, the extraction unit using serrated members 6 can achieve more efficient separation. In other words, the core understanding of this invention is that the volume of the centrifugal partition chromatography extraction unit 1 that does not participate in separation can be reduced by using the centrifugal partition chromatography extraction unit wall structure 5. Therefore, in this specification, the centrifugal partition chromatography extraction unit wall structure specifically refers to a structure that can partially fill the volume of the extraction unit. By employing the wall structure of the centrifugal partition chromatography extraction unit 1 with serrated members 6 and applying this wall structure in the extraction unit, our goal is not to divide the centrifugal partition chromatography extraction unit 1 into smaller units, but, as detailed above, to reduce the unused portion of the extraction unit volume (i.e., the area of ​​the extraction unit filled with the stationary phase) from the perspective of separation operation through the unit wall structure described in this invention. In the centrifugal partition chromatography extraction unit 1, the wall structure 5 of the extraction unit increases the interfacial area between the stationary phase and the mobile phase during operation, compared to extraction units without this wall structure. Furthermore, the wall structure 5 increases the flow path length of the mixture to be separated within the extraction unit. The mobile phase, after passing through the serrated member 6, is atomized and moved away from the unit wall, significantly increasing its specific surface area before completely re-entering the stationary phase, thus further increasing the phase interface between the stationary and mobile phases. During chromatographic separation, increasing the interfacial area improves the efficiency of substance transfer between phases; in other words, a larger interfacial area results in higher separation efficiency.

[0064] Compared to existing plug-in and extraction unit wall structures, the centrifugal partition chromatography extraction unit wall structure 5 used in this invention has significant advantages: it is not deformed by centrifugal force during separation and remains stable even when subjected to centripetal force during rotation. The centrifugal partition chromatography extraction unit wall structure 5 functions through a dual mechanism: on the one hand, it re-atomizes condensed large droplets and prevents the mobile phase from penetrating the unit due to compression by the extraction unit wall (this reduces the mass transfer surface area); on the other hand, it extends the flow path length within the unit—these effects increase the specific surface area of ​​the internal volume of the centrifugal partition chromatography extraction unit 1 of this invention—that is, it improves the production efficiency of this type of extraction unit.

[0065] Each extraction unit is equipped with a centrifugal distribution extraction unit wall structure 5. During the unit cleaning process, the solvent used can flow through the entire volume of the extraction unit without dead angles, thereby reducing the amount of cleaning solvent required. In addition, the wall structure can be selectively replaced due to its design characteristics, so the extraction unit can also be cleaned separately.

[0066] Viewed from above, the interior of the centrifugal partition chromatography extraction unit 1 of this invention is shaped like a racetrack, with a symmetrical structure, so it can operate in both ascending and descending modes without reinstallation.

[0067] The turbulence generated during centrifugal partition chromatography separation can create circulation within a conventional centrifugal partition chromatography extraction unit with inserts, leading to backmixing—a negative effect from a chromatographic separation efficiency perspective. This backmixing can cause separated substances to mix again, thus reducing separation efficiency. On the other hand, during separation, the two liquids should have as large a contact area as possible to improve surface substance transfer efficiency. The centrifugal partition chromatography extraction unit wall structure 5, located within the centrifugal partition chromatography extraction unit 1 as described in this invention (see...) Figure 1 and Figure 2 This can mitigate the negative impact of backmixing. Besides backmixing, in centrifugal partition chromatography extraction units without the plug-in or without the unit wall structure of this invention, the negative effect of the Coriolis force causes the material flow to deflect towards the extraction unit wall. At this time, the liquid phase surface in contact with the extraction unit wall cannot contact the other liquid phase, resulting in a reduction in the mass transfer surface area between the two liquid phases, directly causing a decrease in chromatographic separation efficiency. In chromatography, the mass transfer surface area is directly proportional to the separation efficiency. In other words, if the mass transfer surface area can be sufficiently increased within the extraction unit, then fewer centrifugal partition chromatography extraction units or a smaller extraction unit volume are needed to achieve the same separation efficiency. Reducing the number of extraction units is even more advantageous because it reduces the pressure drop within the rotor of the centrifugal partition chromatography apparatus.

[0068] In general, the centrifugal partition chromatography extraction unit wall structure 5 described in this invention makes the manufacture and use of centrifugal partition chromatography apparatus more efficient and less costly, as the required pore size and reinforcing rib structure are easier to form. Furthermore, the centrifugal partition chromatography extraction unit wall structure 5 can be linearly scaled up while maintaining its proportions, as can the extraction units of its components—that is, the mass of the mixture to be separated can exceed the gram level, and it is also suitable for separating mixtures with masses above the gram level.

[0069] Based on the research findings, the number of serrated components in the wall structure of the centrifugal partition chromatography extraction unit of this invention is at least 2, at most 8, and preferably 6. This is because, while keeping other parameters constant, this number maximizes separation efficiency. The number of serrated components (6) was determined through simulation. Experiments show that when the number of serrated structures exceeds 8, the separation efficiency no longer significantly improves but instead shows a decreasing trend. If the number of serrated structures is increased by 50% (i.e., from 4 to 6), the interfacial area can be increased by 16%.

[0070] The effect produced by the unit wall structure 5 of the centrifugal partition chromatography extraction device is significantly different from the unit wall roughening effect caused by the serrated member 6 structure. Compared with an extraction unit without inserts, the significant advantage of the extraction unit of the present invention is that, through the action of the centrifugal partition chromatography extraction unit wall structure 5, the mobile phase in the extraction unit 1 is forced to the side of the extraction unit, which was previously only filled with stationary phase. In other words, compared with an unfilled extraction unit (which was previously mainly filled with stationary phase that does not participate in separation), when equipped with the centrifugal partition chromatography extraction unit wall structure 5, more than 80% of the extraction chamber volume is actually utilized. As a result, a material flow rate two to three times higher than that of an unfilled extraction unit can be achieved, that is, the load capacity of the centrifugal partition chromatography extraction unit 1 of the present invention is greater than that of the prior art, and the production efficiency is higher.

[0071] The serrated components 6 constituting the unit wall structure 5 of the centrifugal partition chromatography extraction unit are all triangular-based prisms. The prism lateral faces of all components are coplanar with the triangular bases, thus forming the planar lateral faces of the unit wall constructed by the serrated components (see [link]). Figure 1 and Figure 2 ).

[0072] According to another preferred embodiment of the centrifugal partition chromatography extraction unit wall structure 5, the serrated member 6 is a triangular-base prism, with the included angle between its base and any side face between 40° and 80°, preferably 47.54°. The included angle between the base and the side face of the triangle depends on the size of the centrifugal partition chromatography extraction unit 1 and the number of serrated members 6. The principle is that, as those skilled in the art know, the more members there are within the unit wall, the sharper the included angle of the prism triangle.

[0073] According to another preferred embodiment of the centrifugal partition chromatography extraction unit wall structure 5 of the present invention, the serrated member 6 constituting the extraction unit wall structure is a prism with a triangular base, and the height of the prism is between 160 mm and 200 mm, preferably 185 mm.

[0074] It will be apparent to those skilled in the art that the common contact area with the unit wall depends on the geometry of the serrated member 6. If the serrated member 6 contacts the unit wall along the side corresponding to the base of the triangle, the contact area is larger than when it contacts along the shorter (shortest) base of the triangle. According to... Figure 2It can be clearly observed that the serrated member 6 is in close contact with the wall surface of the centrifugal partition chromatography extraction unit 1. According to a more preferred embodiment of the centrifugal partition chromatography extraction unit wall structure 5 than the previous embodiment, this unit wall structure 5 contacts one-third of the total area of ​​the wall surface of the centrifugal partition chromatography extraction unit 1. This contact method is achieved when the centrifugal partition chromatography extraction unit wall structure 5 is formed by the serrated member 6, which is a base prism of an equilateral triangle. It will be apparent to those skilled in the art that this unit wall structure 5 can increase the effective area of ​​the inner wall of the centrifugal partition chromatography extraction unit 1, thereby expanding the mass transfer interface within the unit.

[0075] The present invention also relates to a centrifugal partition chromatography extraction unit 1, the internal structure of which is a racetrack-shaped prism, wherein the base of the racetrack-shaped prism satisfies a ratio of at least 3:1 between its major axis and minor axis, more preferably its major axis is 180 mm and its minor axis is 50 mm. Furthermore, the extraction unit has a centrifugal partition chromatography extraction unit wall structure 5 as described in the present invention on one of its two planar sidewalls, the planar sidewall of which contacts and supports the unit body. Figure 5 The centrifugal partition chromatography extraction unit 1 includes a lower cover 7a and an upper cover 7b, which together enclose the housing 8 (i.e., the outer covering structure of the racetrack-shaped cylindrical cavity 2). It should be noted that the shape of this housing 8 (i.e., the outer covering layer of the extraction unit) may differ from the prism shape of a racetrack; it can also be a prism shape with a rectangular base (see [reference]). Figure 4 and Figure 5 When performing numerical fluid simulation analysis, a prismatic shell with a rectangular base is more ideal; if the raw material is sheet metal or a stretched prism, this structure also has significant advantages in manufacturing test cells. Figure 5 As shown, the lower cover 7a has an outlet pipe end 3, and the upper cover 7b has an inlet pipe end 4. In this specification, the major axis 9a of the racetrack-shaped lower cover 7a and upper cover 7b is the major axis of reflection, and the minor axis 9b is the minor axis of reflection. This structure... Figure 3 This is also indicated in the text. It should be specifically noted that the lengths of the major axis 9a and minor axis 9b of the lower cover 7a and upper cover 7b are completely consistent with the lengths of the primary and secondary axes of the bottom surface of the racetrack-shaped prism. According to the preferred embodiment of the centrifugal partition chromatography extraction unit 1, the length of the major axis 9a (top view) of the racetrack-shaped extraction unit is 180 mm, and the length of the minor axis 9b is 50 mm, thus satisfying the requirement that the ratio of the lengths of the major axis 9a to the minor axis 9b is at least 3:1. When the aforementioned centrifugal partition chromatography extraction unit wall structure 5 is placed inside the centrifugal partition chromatography extraction unit 1, its position is located on one of the longer straight edges of the two parallel sides of the racetrack-shaped base (e.g., ...). Figure 4 The longer straight side of the racetrack-shaped main body marked 10 is shown (the unit wall structure is not drawn for simplicity), but the curved side of the racetrack-shaped centrifugal partition chromatography extraction unit 1 is not included.

[0076] Comparing the inner surface of centrifugal partition chromatography extraction unit 1 with that of an empty unit reveals that using the serrated component 6 as the unit wall structure increases the mass transfer interface within the unit. According to preliminary model experiments, the structure of centrifugal partition chromatography extraction unit 1—due to the presence of the centrifugal partition chromatography extraction unit wall structure 5—increases the interfacial area by 35-70% compared to an extraction unit without any inserts (i.e., without an extraction unit wall structure). It should be noted that the interfacial size measured in an extraction unit without any inserts or unit wall structures is taken as a 100% baseline value, and this experiment used an ethyl acetate-water solvent system.

[0077] Experiments show that when the number of serrated components 6 increases from four to six (using two sample extraction units with a diameter of 10 mm and a length of 32 mm as a baseline), increasing the number of serrations by two increases the interfacial area of ​​the serrated components 6 by 16%. Therefore, it can be inferred that when more than eight serrations are used as the unit wall structure, the resulting liquid-liquid interface cannot be increased proportionally, and thus increasing the number of serrations will not significantly improve the separation efficiency.

[0078] In the centrifugal partition chromatography extraction unit 1, the area of ​​the centrifugal partition chromatography extraction unit wall structure 5 should occupy at least 68% of the top view cross-section of the unit without this structure, and at most no more than 90%. Thus, compared to a unit without any inserts or unit wall structures, the fine unit wall structure of the present invention significantly reduces the internal volume of the centrifugal partition chromatography extraction unit 1. The top view cross-section of the centrifugal partition chromatography extraction unit described in this invention refers to the cross-section perpendicular to the direction of the lower cover 7a and upper cover 7b inside the unit body, i.e., the cross-section of a horseshoe-shaped prism. In the context of this invention, the concept of top view cross-section specifically refers to a "hollow" unit that does not contain the serrated elements of the present invention. This definition allows for precise quantification of the proportion of the volume occupied by the component relative to the top view cross-section. As detailed above, the volume of the centrifugal partition chromatography extraction unit 1 is reduced due to the space portion not involved in separation. According to another preferred embodiment of the centrifugal partition chromatography extraction unit 1 of the present invention, its unit wall structure 5 can occupy up to 90% of the total volume of the extraction unit. As described above, the centrifugal partition chromatography extraction unit wall structure 5 constitutes an important component of the extraction unit of the present invention, but does not obstruct the material flow path within the extraction unit.

[0079] According to another preferred embodiment of the centrifugal partition chromatography extraction unit 1 of the present invention, at least one serrated member 6 in the wall structure 5 of the centrifugal partition chromatography extraction unit extends beyond the unit centerline 11, and the direction of extension is parallel to the longitudinal edge of the member (here it is understood that it does not include the unit wall structure), and its extension amplitude relative to the unit centerline 11 can reach 80-90% of the distance between the unit centerline 11 and the opposite unit wall (see Figure 2 ). Figure 2The tip (side view) of the triangular serrated member 6 is clearly shown to extend beyond the unit centerline 11, and those skilled in the art can see that... Figure 2 It can be clearly seen that the longitudinal edge of the serrated member 6 is parallel to the center line of the extraction unit, which is perpendicular to the final flow direction of the mobile phase during operation.

[0080] The centrifugal partition chromatography extraction unit 1 according to the present invention, without including any inserts or unit wall structures, has a volume of at least 1.5 mL and / or up to 1.3 L. For example, a centrifugal partition chromatography extraction unit 1 with a volume of 1.5 mL is suitable for separating gram-level samples. As mentioned above, the centrifugal partition chromatography extraction unit wall structure 5 can be linearly scaled up proportionally, and the centrifugal partition chromatography extraction unit 1 including this component can also be scaled up synchronously. Furthermore, the maximum volume of the centrifugal partition chromatography extraction unit 1 of the present invention is 1.3 L. By connecting an appropriate number of units and optional rotors in series, the separation of ton-level mixtures can be achieved with a volume of 1.3 L.

[0081] This invention also relates to a rotor for a centrifugal partition chromatography apparatus, the rotor comprising the centrifugal partition chromatography extraction unit 1 described herein. The extraction units 1 on the rotor are connected in series and, when arranged on the rotor of the centrifugal partition chromatography apparatus, can move around the rotor axis as the rotor rotates. This series of units is arranged in a ring on the rotor, achieving effective transfer of substances between phases through rotor rotation. The tangential force generated by rotation acts on the centrifugal partition chromatography extraction unit, causing the mobile phase entering the extraction unit to deflect. For units without inserts or unit wall structures, mobile phase droplets will be pushed against the unit sidewalls, thereby reducing the contact area between the mobile phase and the stationary phase. The centrifugal partition chromatography extraction unit wall structure 5 of this invention significantly mitigates this adverse effect because it does not allow the mobile phase to flow along the extraction unit wall, but instead guides it back towards the opposite sidewall, thereby increasing the interface area between the stationary and mobile phases. Furthermore, from the perspective of separation efficiency, the use of centrifugal partition extraction unit wall structure 5 can reduce the idle volume of centrifugal partition extraction unit 1. In other words, this unit wall structure increases the proportion of the actual utilized unit volume, and the utilization rate of a single unit can reach more than 80%. Thus, the separation efficiency is also improved.

[0082] The rotor preferably contains between 30 and 100 centrifugal partition chromatography extraction units 1, at which point the total column height is between 2.5 meters and 4.1 meters. It will be apparent to those skilled in the art that a higher number of centrifugal partition chromatography extraction units (i.e., a taller total column height) results in higher separation efficiency; conversely, a higher efficiency of the centrifugal partition chromatography extraction units requires fewer extraction units. It is recommended to arrange at least 30 centrifugal partition chromatography extraction units on the rotor. However, there is an upper limit to the increase in the number of extraction units, which can be determined experimentally. One reason for this upper limit is that more extraction units mean more connecting tubing, leading to pressure loss, requiring higher operating pressure, and reducing load capacity. When the rotor is equipped with more than 100 extraction units, the chromatographic separation efficiency does not significantly improve, but the rotor installation difficulty and cost increase significantly.

[0083] The present invention also relates to a centrifugal partition chromatography apparatus comprising one or more rotors conforming to the requirements of the present invention, namely rotors connected in series with the centrifugal partition chromatography extraction unit 1 of the present invention.

[0084] In the method of manufacturing the centrifugal partition chromatography extraction unit 1, which can be used in the centrifugal partition chromatography apparatus of the present invention, the centrifugal partition chromatography extraction unit wall structure 5 of the present invention is positioned or formed inside the extraction unit. Here, "formed" means that during the manufacturing process of the extraction unit (e.g., by 3D printing), the centrifugal partition chromatography extraction unit wall structure is irreversibly fixed inside the extraction unit. "Positioned" means that there is a possibility of positioning the serrated member 6 or the centrifugal partition chromatography extraction unit wall structure 5 in a detachable (reversible) manner.

[0085] The present invention will be described below with reference to specific embodiments.

[0086] Example 1: In a centrifugal partition chromatography apparatus including the centrifugal partition chromatography extraction unit 1 of the present invention, a mixture of ethyl p-hydroxybenzoate and methyl p-hydroxybenzoate was separated by centrifugal partition chromatography. A mixture containing 100 µg of ethyl paraben and methyl paraben, in a mass ratio of 50–50% (Sigma-Aldrich, methyl paraben CAS No.: 99-76-3; Sigma-Aldrich, ethyl paraben CAS No.: 120-47-8), was separated. The mixture of ethyl paraben and methyl paraben was dissolved in 50 µl of a solvent mixture stationary phase in equilibrium (components described below) and injected.

[0087] The separation parameters for centrifugal partition chromatography are as follows: The component ratios of the solvent mixture under equilibrium conditions are as follows (Note: the solvent mixture is brought to equilibrium by mixing the stationary phase and the mobile phase and then shaking): Hexane: 135; Ethyl acetate: 15; Acetonitrile: 60; Water: 240; Phosphoric acid: 0.1.

[0088] Stationary phase retention rate during chromatographic separation: 91%.

[0089] Operating mode of centrifugal partition chromatography apparatus: descending range method.

[0090] Rotor speed of the centrifugal partition chromatography apparatus: 1000 rpm.

[0091] The flow rate for the centrifugal partition chromatography extraction apparatus is 1 ml / min.

[0092] The operating pressure of the centrifugal partition chromatography extraction device is 25 bar.

[0093] Number of centrifugal partition chromatography extraction units: 80.

[0094] Centrifugal partition chromatography extraction unit size: 4 mm in diameter Centrifugal partition chromatography extraction unit length: 40 mm Number of serrated components in the wall structure of the centrifugal partition chromatography extraction unit: 8. Temperature during chromatographic separation: room temperature.

[0095] The above separation operation was previously performed in a centrifugal partition chromatography apparatus containing a tubular extraction unit (disclosed in European patent application EP3204136A1). In the comparative experiment, the parameters were kept consistent; the differences between the two centrifugal partition chromatography extraction apparatuses lay in the inserts, unit wall structure, and shape of the extraction unit. The comparative experimental results are shown below. Figure 6 Among the components containing ethyl parabens and methyl parabens, the best separation effect was achieved by a centrifugal partition chromatography extraction device with a unit wall structure. This conclusion is also supported by numerical data (see Table 1 for details).

[0096] Table 1 As can be clearly seen from the data in the table, when using the centrifugal partition chromatography extraction device described in this invention (which includes an extraction unit with a centrifugal partition chromatography extraction unit wall structure), the yields of ethyl p-hydroxybenzoate and methyl p-hydroxybenzoate are both increased by nearly 4%.

[0097] Example 2 - Simulation Through simulation, we compared the performance of the hollow cylindrical extraction unit with that of the extraction unit described in this invention.

[0098] The simulation parameters are as follows: Reference measurement: A cylindrical extraction unit without lining or partition structure is used.

[0099] Centrifugal partition chromatography extraction unit diameter: 1.75 mm.

[0100] Centrifugal partition chromatography extraction unit length: 36 mm.

[0101] Equilibrium solvent mixture: ethyl acetate / water.

[0102] Centrifugal partition chromatography apparatus operating mode: Ascending mode.

[0103] The rotor speed of the centrifugal partition chromatography device is 1200 rpm.

[0104] The flow rate for the centrifugal partition chromatography extraction apparatus is 2 mL / min.

[0105] Specific interfacial area of ​​the centrifugal partition chromatography extraction unit: 344 m² 2 / m 3 (100%).

[0106] Measurements were performed using a horseshoe-shaped centrifugal partition chromatography extraction unit, which includes the wall structure of a centrifugal partition chromatography extraction unit. Long axis of centrifugal partition chromatography extraction unit: 14 mm.

[0107] Equipped with a centrifugal partition chromatography extraction unit: Short axis of centrifugal partition chromatography extraction unit: 3 mm.

[0108] Centrifugal partition chromatography extraction unit length: 14 mm.

[0109] Number of serrated components: 4.

[0110] Equilibrium solvent mixture: ethyl acetate / water.

[0111] Centrifugal partition chromatography apparatus operating mode: Ascending mode.

[0112] The rotor speed of the centrifugal partition chromatography device is 1200 rpm.

[0113] The flow rate for the centrifugal partition chromatography extraction apparatus is 2 mL / min.

[0114] Specific interfacial area of ​​the centrifugal partition chromatography extraction unit: 441 m² 2 / m 3 (128%).

[0115] Measurements were performed using a horseshoe-shaped centrifugal partition chromatography extraction unit, which includes the wall structure of a centrifugal partition chromatography extraction unit. Long axis of centrifugal partition chromatography extraction unit: 14 mm.

[0116] Equipped with a centrifugal partition chromatography extraction unit: Short axis of centrifugal partition chromatography extraction cell: 3 mm.

[0117] Centrifugal partition chromatography extraction cell length: 14 mm.

[0118] Number of serrated components: 6.

[0119] Equilibrium solvent mixture: ethyl acetate / water.

[0120] Centrifugal partition chromatography apparatus operating mode: Ascending mode.

[0121] The rotor speed of the centrifugal partition chromatography device is 1200 rpm.

[0122] The flow rate for the centrifugal partition chromatography extraction apparatus is 2 mL / min.

[0123] Specific interfacial area of ​​the centrifugal partition chromatography extraction unit: 471 m² 2 / m 3 (137%).

[0124] In other words, based on the simulation results shown in Example 2 above, it is clear that if the wall structure of the centrifugal partition chromatography extraction unit is used instead of the tubular structure unit for separation in the centrifugal partition chromatography extraction unit, the specific interface area can be increased by 28-37%, and this ratio can be further increased by increasing the number of serrated components.

[0125] The centrifugal partition chromatography extraction unit 1 of this invention has a maximum pressure resistance of approximately 150 bar, meaning it possesses pressure resistance characteristics. This is mainly attributed to two aspects: firstly, the components are precisely assembled through a heat treatment process; secondly, the specific interface area inside the centrifugal partition chromatography extraction unit 1 (including the serrated component 6) is increased, enhancing its pressure resistance. Therefore, it can be concluded that a smaller number of centrifugal partition chromatography extraction units 1 can achieve efficient separation; in other words, reducing the number of units can reduce the pressure drop.

[0126] Compared to existing centrifugal partition chromatography extraction units, the centrifugal partition chromatography extraction unit 1 of this invention does not require a component for distributing the liquid flow at the extraction unit inlet, nor does it require a component for collecting the liquid flow at the outlet. In other words, the centrifugal partition chromatography extraction unit 1 of this invention consists of fewer components, and based on the above characteristics, the number of extraction units required for the entire device is reduced, thereby making the centrifugal partition chromatography apparatus simpler in structure, faster in manufacturing process, and more cost-effective.

[0127] The centrifugal partition chromatography extraction unit 1 of this invention does not have a component for distributing the liquid flow at the inlet of the extraction unit, nor does it have a component for collecting the liquid flow at the outlet. The unit itself has a symmetrical structure, meaning it can operate in both ascending and descending modes without reinstallation, thereby shortening the separation operation interval (downtime) and improving production efficiency.

[0128] The present invention employs a centrifugal partition chromatography extraction unit wall structure 5 located within the centrifugal partition chromatography extraction unit 1, which has the following advantages: it can prevent material flow deviation caused by tangential force along the unit wall direction; its design increases the material transfer surface area within the centrifugal partition chromatography extraction unit 1; and it can avoid backmixing caused by turbulence within the extraction unit. In other words, the use of the centrifugal partition chromatography extraction unit wall structure 5 can improve chromatographic separation efficiency.

[0129] The centrifugal partition chromatography extraction unit wall structure 5 used in the centrifugal partition chromatography extraction unit 1 of this invention has significant advantages: it remains stable even under centripetal forces, has a longer service life, and is easy to clean. The centrifugal partition chromatography extraction unit wall structure 5 allows for precise geometric definition and design, thus its effects can be clearly defined and quantified. This structure can re-atomize large droplets condensed during separation and, through its structural design, extend the path length of the sample during separation, thereby increasing the specific interface area between the liquid phases. Furthermore, centrifugal partition chromatography apparatuses using this type of centrifugal partition chromatography extraction unit wall structure 5 have the advantage of easy scale-up in production, and adjustments to production scale are simpler. In the centrifugal partition chromatography unit 1 formed according to this invention, the ratio of stationary phase to mobile phase is at least 80%, and the larger the specific interface size between the stationary phase and mobile phase, the higher the separation efficiency. This objective can also be achieved by using an extraction unit containing serrated members 6 as the extraction unit wall structure.

Claims

1. A centrifugal partition chromatography extraction unit wall structure (5), the extraction unit having at least two planar walls, characterized in that: i) The unit wall structure includes prism-shaped sawtooth members (6), which are preferably triangular-base prisms; ii) The wall structure (5) of the centrifugal partition chromatography extraction unit contains at least two serrated members (6), and iii) Each serrated component (6) is arranged in parallel along one of the two planar sides of the centrifugal partition chromatography extraction unit.

2. The wall structure (5) of the centrifugal partition chromatography extraction unit according to claim 1, characterized in that... The number of its serrated components (6) is at least 2, at most 8, and preferably 6.

3. The centrifugal partition chromatography extraction unit wall structure (5) according to any one of claims 1 to 2, characterized in that: The serrated component (6) is a triangular-base prism, and the prism sides of all the serrated components (6) are located in the same plane, thus forming one side plane of the centrifugal partition chromatography extraction unit wall.

4. The centrifugal partition chromatography extraction unit wall structure (5) according to claim 3, characterized in that: The serrated member (6) is a triangular-base prism, wherein the angle between the base of the triangle and any edge is between 40° and 80°, preferably 47.54°.

5. The centrifugal partition chromatography extraction unit wall structure (5) according to any one of claims 1 to 4, characterized in that: The serrated member (6) is a prism with a triangular base, and the height of the prism is between 160 mm and 200 mm, preferably 185 mm.

6. Centrifugal partition chromatography extraction unit (1), characterized in that The extraction unit comprises a centrifugal partition chromatography extraction unit wall structure (5) according to any one of claims 1 to 5, and its internal structure is a racetrack-shaped prism, wherein the bottom surface of the racetrack-shaped prism preferably forms a ratio of its major axis (9a) to its minor axis (9b) of at least 3:1, more preferably, its major axis (9a) is 180 mm and its minor axis (9b) is 50 mm, and the extraction unit is provided with the centrifugal partition chromatography extraction unit wall structure (5) according to any one of its two planar sides.

7. The centrifugal partition chromatography extraction unit (1) according to claim 6, characterized in that: The centrifugal partition chromatography extraction unit wall structure (5) according to any one of claims 1 to 5 constitutes at least 68% of the area of ​​the top view section of the centrifugal partition chromatography extraction unit (1) (when the unit wall structure (5) is not included), and / or constitutes at most 90% of it.

8. The centrifugal partition chromatography extraction unit (1) according to any one of claims 6 to 7, characterized in that: At least one of the serrated members (6) in the centrifugal partition chromatography extraction unit wall structure (5) according to any one of claims 1 to 5 extends beyond the unit centerline (11), and the direction of extension is parallel to the longitudinal edge of the member, which is understood to exclude the longitudinal edge of the unit wall structure (5).

9. The centrifugal partition chromatography extraction unit (1) according to any one of claims 6 to 8, characterized in that: Its volume (excluding the unit wall structure) is at least 1.5 ml and / or up to 1.3 liters.

10. A rotor for a centrifugal partition chromatography apparatus, characterized in that... It includes a centrifugal partition chromatography extraction unit (1) according to any one of claims 6 to 9.

11. The rotor of the centrifugal partition chromatography apparatus according to claim 10, characterized in that... Each rotor contains 30 to 100 centrifugal partition chromatography extraction units (1), and the total length of the chromatographic column is between 2.5 and 4.1 meters.

12. A centrifugal partition chromatography apparatus, characterized in that... It includes one or more rotors according to claim 10 or 11.

13. A method for manufacturing a centrifugal partition chromatography extraction unit (1) used in a centrifugal partition chromatography apparatus, characterized in that: The centrifugal partition chromatography unit wall structure (5) according to any one of claims 1 to 5 is placed inside or formed therein in the extraction unit.

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