JPH0417201Y2 - - Google Patents

Description

[Detailed explanation of the idea]

(Industrial Application Field) The present invention increases the evaporation area by centrifugally rotating the sample container, and pressurizes the sample solution by centrifugal force to distill the solution under reduced pressure without the risk of bumping. This invention relates to a double-shroud container for a rotor in a centrifugal rotary vacuum concentrator that performs concentration, drying, recovery, etc. with simple operations. (Prior art) Conventionally, in this type of device, there is a centrifugal rotary vacuum concentration device that heats the sample directly with a far-infrared heater or indirectly through a metal container [Reference: Taiyo Kagaku Kogyo Co., Ltd. centrifugal manufactured by Co., Ltd.
concentrator VC-36, VC-96 instruction manual and
catalog]. However, there are no centrifugal rotary vacuum concentrators in which heating of the sample to be concentrated is performed indirectly via a heat medium. (Problem that the invention aims to solve) When using conventional equipment, when the solution to be concentrated is an aqueous solution, the latent heat (heat of vaporization) of water is larger than that of other organic solvents, so water cannot be concentrated under reduced pressure. Accordingly, the temperature of the remaining aqueous solution decreases significantly, and the rate of subsequent vacuum concentration decreases rapidly.
Therefore, in order to continue concentrating the solution, it is necessary to raise the temperature of the remaining aqueous solution by heating. Sample heating methods using radiant heat from far-infrared heaters installed in conventional equipment include (1)
There are two methods: heating the sample solution directly through the glass sample container wall; and (2) heating the glass sample container wall through heating of the metal envelope container wall, thereby achieving heating of the sample solution. When heating is performed using these methods, the surface above the liquid surface on the wall of the sample container is heated quickly, but on the other hand, the temperature rises slowly below the surface of the liquid on the wall of the sample container due to the presence of supercooled aqueous solution. only is done. Therefore, when heating the aqueous solution until a sufficient vacuum concentration rate is obtained, the portion of the sample container wall above the liquid level reaches an overheated state. Generally, when a solution is concentrated, compounds in the concentrated solution are precipitated or concentrated on the container wall at the interface between the sample container wall and the liquid surface. In this case, if the sample to be concentrated is a thermally unstable compound, the sample will decompose, making it impossible for the experimenter to recover the necessary sample. The present invention was developed in view of the above points, and since the heating of the sample to be concentrated is performed indirectly through the heat medium contained in the double jacket container, uneven temperature rise on the sample container wall results. Therefore, the object of the present invention is to obtain a double jacket container for a rotor in a centrifugal rotary vacuum concentrator that does not involve loss of a required sample due to overthermal decomposition. (Means for Solving the Problems) In order to achieve the above object, the present invention provides two rotors for use in a centrifugal rotary vacuum concentrator that indirectly heats and concentrates a sample under vacuum and centrifugal rotation. A heavy mantle container, consisting of an inner mantle container that stores a sample container containing a sample to be concentrated, and an outer mantle container that stores the inner mantle container and is attached to the rotor of the centrifugal rotary vacuum concentrator, A double mantle container for a rotor in a centrifugal rotary vacuum concentrator, characterized in that a gap is formed between the outer mantle container and the inner mantle container, in which a heating medium for heating the sample to be concentrated is filled. was its gist. (Effects of the invention) As described above, in the present invention, the sample to be concentrated is heated not by direct radiation from a far-infrared heater, but indirectly by the heating medium in the double envelope for the rotor. Since this is carried out, there is no uneven temperature rise of the sample container wall, and therefore, the required sample is not lost due to overthermal decomposition. By using the double envelope container for the rotor in a centrifugal rotary vacuum concentrator according to the present invention, which allows heating of the sample to be concentrated to be performed indirectly via a heat medium,
Since the solution can be heated without decomposing the sample, vacuum concentration can be completed in a short time. Next, the double envelope container for the rotor in the centrifugal rotary vacuum concentrator of this invention will be explained in more detail by way of examples. (Example) An example of the present invention will be described based on FIGS. 1, 2, and 3. Fig. 1 is a top view showing a double outer envelope for the rotor in the centrifugal rotary vacuum concentrator of the present invention, Fig. 2 is a sectional view taken along the line A-B in Fig. 1, and Fig. 3 is a FIG. 2 is a cross-sectional view of a sample container and a state filled with a heat medium, viewed from the side. The names of the parts in FIG. 1 are as follows: outer mantle container 1, inner mantle container 2. The names of the parts in FIG. 2 are as follows: outer mantle container 1, inner mantle container 2, sample container 3, sample solution 4, heating medium 5. The outer mantle 1 and the inner mantle 2 are made of metal, glass, resin, or ceramic. It is also possible to color the outside with black to increase the absorption efficiency of far infrared rays. The space between the outer mantle container 1 and the inner mantle container 2 is filled with a heat medium. Examples of the heat medium that can be used include silicone oil, DMSO, DMF, glycerin, ethylene glycol, liquid paraffin, toluene, and xylene. For rotors in centrifugal rotary vacuum concentrators 2
The heavy overcoat container is attached to a rotor in the state shown in Figure 3, and concentrated in a centrifugal rotary vacuum concentrator. FIG. 4 shows the appearance of the centrifugal rotary vacuum concentrator. The names of the parts in Figure 4 are as follows:
Vacuum rotor chamber 6, rotor chamber lid 7, suction nozzle 8 (to vacuum pump or aspirator), vacuum gauge 9, operation panel 10, power switch 11, centrifuge switch 12, far infrared heater switch 1
3. Far-infrared heater adjustment dial 14 and centrifuge rotation speed adjustment dial 15. FIG. 5 is a cross-sectional view showing the centrifugal rotary vacuum concentrator in a state in which a double outer rotor container is attached to the centrifugal rotary vacuum concentrator. The names of the parts in Figure 5 are as follows: vacuum rotor chamber 6;
Rotor chamber lid 7, suction nozzle 8 (to the vacuum pump or aspirator), centrifuge rotating shaft 16, centrifuge rotor 17, double jacket container 18 in the state shown in FIG. 2, magnet rotor 19, vacuum leak Valve 20, rotating shaft support part 21, centrifugal motor 22
and far infrared heater 23. The vacuum rotor chamber 6 becomes a closed system by closing the rotor chamber lid 7. Vacuum leak valve 2
0 is closed and suction is applied from the suction nozzle 8 with a vacuum pump or an aspirator, thereby making the vacuum rotor chamber 6 evacuated. The double jacket container 18 of the present invention attached to the centrifuge rotor 17 is connected to the centrifuge rotation shaft 1.
6 starts rotating at a speed of about 0-3000 rpm. Rotation is transmitted to the rotary shaft by a sealless structure between the vacuum rotor chamber 6 and the rotary shaft 16 to prevent vacuum leakage, and therefore by a magnetic drive system. The magnetic drive system is a magnet rotor 19 directly connected to the centrifuge rotating shaft 16 which is rotated by the rotation of the centrifuge motor 22 in response to the rotating magnetic field generated by this rotor. By transmitting the rotational motion to the container 19, the centrifugal rotation of the double-walled container 18 of the present invention is realized. The sample solution in the double-mantle container 18 is concentrated in vacuum in the vacuum rotor chamber 6 and heated by heat conduction from the heating medium in the double-mantle container heated by a far-infrared heater. that time,
By undergoing centrifugation, the sample liquid is pressurized and stirred, and bumping is suppressed even under vacuum and heating conditions, making it possible to perform safe concentration operations.
Furthermore, safe operation is achieved in that necessary and sufficient heating by indirect heat transfer from the heating medium prevents sample components from decomposing. Comparative Example It is known that red cabbage contains more than 10 types of acylated anthocyanins (Reference: E.ldaka et al, Chemistry Letter, 145-
148pp, 1213-1216pp (1987)). It was divided into 60 fractions by HPLC preparative analysis. The volume of each is 30ml. The eluent composition is a mixed solvent of acetic acid/acetonitrile/water. Fraction 1-3 is 3-O-[2-O-
{β-D-glucopyranosyl}-β-D-glucopyranosyl]-5-O-(β-D-glucopyranosyl)cyanidin (3-0-[2-0-{β-D-
glucopyranosyl}-β-D-glucopyranosyl]-
5-0-(β-D-glucopyranosyl)cyanidin
()), fraction 17-21 is 3-O-[2-O-{β-D
-glucopyranosyl}-6-O-p-coumaryl-
β-D-glucopyranosyl]-5-O-(β-D-
glucopyranosyl) cyanidin (3-0-[2-
0-{β-D-glucopyranosyl}-6-0-p-
coumaryl-β-D-glucopyranosyl]-5-0-
(β-D-glucopyranosyl)cyanidin()), fractionation
35-37 is 3-O-[2-O-{2-O-sinapyr-
β-D-glucopyranosyl}-6-O-p-coumaryl-β-D-glucopyranosyl]-5-O-(β
-D-glucopyranosyl)cyanidin (3-0-
[2-0-{2-0-sinapyl-β-D-
glucopyranosyl}-6-0-p-coumaryl-β-
D-glucopyranosyl]-5-0-(β-D-
glucopyranosyl) cyanidin ()), fractions 41-45 are 3-O-[2-O-{2-O-sinapyr-β-D-
glucopyranosyl}-6-O-ferryl-β-
D-glucopyranosyl]-5-0-(β-D-glucopyranosyl)cyanidin (3-0-[2-0-
{2-0-sinapyl-β-D-glucopyranosyl}-
6-0-ferulyl-β-D-glucopyranosyl]-5
-0-(β-D-glucopyranosyl)cyanidin())
And fraction 50-54 is 3-0-[2-O-{2-O-
Sinapyr-β-D-glucopyranosyl}-6-O
-Sinapyr-β-D-glucopyranosyl]-5-
O-(β-D-glucopyranosyl)cyanidin (3-0-[2-0-{2-0-sinapyl-β-D-
glucopyranosyl}-6-0-sinapyl-β-D-
glucopyranosyl]-5-0-(β-D-
glucopyranosyl)cyanidin()). ()
-() decomposes in the presence of acid at temperatures above 35°C to gradually produce (). Each fraction containing ()-() was divided into 15 ml portions and subjected to centrifugal rotary vacuum concentration using three methods. That is, () when concentrated using a centrifugal rotary vacuum concentrator without heating; () when concentrated at a liquid temperature of 20°C using a centrifugal rotary vacuum concentrator equipped with a conventional far-infrared heater;
This is a case of concentration at a liquid temperature of 20° C. using the centrifugal rotary vacuum concentrator of the present invention, which is equipped with a double outer envelope for the rotor of the centrifugal rotary vacuum concentrator. For each compound ()-(), ()
- The required time for concentration using method () and the decomposition rate of each compound to () are shown in the table below.

[Table] Regarding the thermal stability of the compounds, ()-() is relatively stable, and each has the same degree of stability. ()
is an unstable compound compared to ()-(). HPLC preparative separation uses stepwise elution, and the content of acetonitrile increases in the later fractions, so ()
Concentration time is relatively short in the order of →(). () has a longer concentration time than (), but
This seems to be due to the fact that the upper part of the sample container is heated higher than the set temperature, but the liquid temperature is lower.
Therefore, this overheating of the upper part of the sample container is the main reason why the decomposition rate of the compound is higher in () than in (). Therefore, when concentrating using the centrifugal rotary vacuum concentrating device of the present invention equipped with a double rotor envelope container, it is possible to concentrate using the centrifugal rotary vacuum concentrating device of the present invention. It has become clear that unstable samples can be concentrated more safely and quickly compared to conventional methods.

[Brief explanation of the drawing]

Fig. 1 is a top view showing the double envelope container for the rotor in the centrifugal rotary vacuum concentrator of the present invention, Fig. 2 is a sectional view taken along the line A-B in Fig. 1, and Fig. 3 4 is a cross-sectional view from the side of the sample container and the rotor double jacket container in the centrifugal rotary vacuum concentrator filled with a heating medium, and FIG. 4 shows the external appearance of the centrifugal rotary vacuum concentrator of the present invention. FIG. 5 is a cross-sectional view showing the centrifugal rotary vacuum concentrator filled with a heat medium and equipped with a double outer rotor container. Explanation of symbols, 1...Outer mantle container, 2...Inner mantle container, 3...Sample container, 4...Sample solution, 5
...Heating medium, 6...Vacuum rotor chamber, 7...Rotor chamber lid, 8...Suction nozzle, 9...Vacuum gauge,
10...Operation panel, 11...Power switch, 1
2... Centrifuge switch, 13... Far infrared heater switch, 14... Far infrared heater adjustment dial, 15... Centrifuge rotation speed adjustment dial, 16
... Centrifuge rotation shaft, 17 ... Centrifuge rotor, 1
8...Double mantle container, 19...Magnetic rotor, 20
... Vacuum leak valve, 21 ... Rotating shaft support part, 22 ... Centrifugal motor, 23 ... Far infrared heater.

Claims (1)

[Scope of Claim for Utility Model Registration] A double jacket container for the rotor of a centrifugal rotary vacuum concentrator that indirectly heats and concentrates the sample under vacuum and centrifugal rotation, which contains the sample to be concentrated. an outer mantle container that houses the inner mantle container and is attached to the rotor of the centrifugal rotating vacuum concentrator, and a space between the outer mantle container and the inner mantle container. 1. A double-sheathed container for a rotor in a centrifugal rotary vacuum concentrator, characterized in that a space is formed for filling a heating medium for heating a sample to be concentrated.