JPS62106802A - Residue extraction device - Google Patents

Abstract

PURPOSE:To automatically extract the residue product out of the sample in a short period of time and also always easily obtain accurate results of instrumentation by extracting residue product by means of supersonic process, condensation after separating the extracted liquid, and refining the said liquid in the chromatographic column. CONSTITUTION:The residue product is extracted by imparting supersonic out of the supersonic extraction device 9 to the sample and the solvent medium in the sample container. The extracted solution is sucked into the separating tank 11 through the filter 10. The said extracting process is repeated a required number of times. Next, the fixed quantity of common salt solution out of the common salt tank 2 and the fixed quantity of separated solvent medium out of the separating solvent medium tank 3 are added together to the separating tank 11, and after being mixed together thoroughly, are left at rest and the solution is separated into two phases, organic extracted liquid and residue water extract. Then the extracted liquid is charged into the condensation container 18, heated up under the reduced pressure and condensed by evaporating solvent medium. After completing condensing process, the fixed quantity of melt solvent medium out of the solvent medium tank 25 is charged into the condensation container 18 to solve the extract, and the solved extract is transferred into the chromatographic column 27 for instrumenting the residue product.

Description

DETAILED DESCRIPTION OF THE INVENTION [Industrial Application Field] The present invention relates to an apparatus for automatically extracting trace amounts of pesticide residues remaining in vegetables, fruits, and the like.

[Prior art]

Conventionally, the work of measuring the residue of drugs, etc. was done using a separating funnel,
This was done manually using test tubes, etc. As a result, work efficiency is low and costs are high, and even slight differences in operating methods can cause large variations in analysis results. Only experienced personnel can obtain appropriate results, making residue analysis easy and efficient. The problem was that it could not be done.

[Purpose of the invention]

The present invention has been made in order to solve the above-mentioned conventional problems, and it is possible to automatically extract residues from a sample in a short time, and also to easily extract residues from which accurate measurement results can always be obtained. The purpose is to provide an extraction device.

[Structure of the invention]

The residue extraction device according to the present invention includes an ultrasonic extractor that applies ultrasonic waves to a sample container containing a sample and an extraction solvent to extract a residual substance, and a saline solution added with an extraction solution. , and separation solvent, and then let stand to separate into extract liquid and raffinate liquid 5
Separation tank, said extraction solvent, saline solution and separation solvent)
1. A quantitative supply means for supplying a fixed amount of each, a separation means having an interface detection sensor for separating the separated extract solution, and 1. heating the extract solution under reduced pressure. It is equipped with a concentrator for concentrating /8 medium by threshold elution, a means for dissolving and extracting the concentrated extract, and a chromatography column for purifying the extracted extract solution. , extract quickly and efficiently with an extraction solvent using ultrasonic waves, separate the extract with a saline solution and a separation solvent, separate the extract solution (4 times), concentrate it, and store it in a container. It is characterized by being configured so that it can be easily and accurately measured by splitting the chroma 1-color LQ trowel 1n.

[) Drunken lineup]

Hereinafter, one embodiment of the present invention will be described based on the drawings. An extraction medium tank 1 containing an extraction solvent made of an organic solvent that is easily soluble in water, such as acetone or methanol, is connected to a sample container 8 via a measuring tube 4 and a cock TVI. The metering pipe 4 is connected to a pressure reducing pump 7 via a solenoid valve SVI,
The extraction solvent can be removed by suction. The sample container 8 is placed in the ultrasonic extractor 9 and subjected to ultrasound:! ').

The residue is extracted quickly and efficiently using an extraction solvent. Sample container 8 is passed through filter 10,
and is connected to the liquid separation tank 11. In this liquid separation tank 11,
A saline tank 2 containing a saline solution, and a separating solvent tank 3 containing a separating solvent made of an organic solvent that is difficult to dissolve in water such as n-hexane, ethyl acetate, dichloromethane, and chloroform.
are measuring tubes 5 and 6, cock'rV2 and T V 3 respectively.
In addition to being violated through , it is also agitating M-co! 1.2 and an interface detection sensor 13 are provided, and are further connected via a solenoid valve sv4 to a pressure reducing pump 7. The pre-measurement ports 5 and 6 are also connected to the decompression pump 7 via the electromagnetic valves sV2 and SV3. is connected to the extract liquid tank 16. In order to remove water in the extract liquid, a dehydrating agent such as anhydrous sodium sulfate or molecular sieves is stored between the cock MVI and the extract tank. It is preferable to install a dehydrator [15].

The raffinate liquid tank 14 and the extract liquid tank 16 each have a solenoid valve SV.
5 and SV6, and the raffinate tank 14 is opened to the outside of the system via a cock M V 2. The extract liquid tank 16 has a liquid level sensor I7 and a cock MV.
3 to the concentration container 18. a tank container 1
8 is a condenser 2 which is disposed in a constant temperature water bath 19 and is configured to be stirred by a magnetic stirrer 20, and which condenses the evaporated solvent and stores it in a trap 22 at the lower part.
Connected to 1. In addition, the concentration container 18 is connected to a solenoid valve SV.
The concentrating container 18 and condenser 21 are connected to a vacuum pump 23 with a high blade clearance via a solenoid valve SV8 to evaporate under reduced pressure. ing. The raffinate tank 14 and the separation tank 11 are connected through a return passage 24 . Further, a melting solvent tank 25 containing a melt is connected to the tank a container 18 via a metering tube 26 and a cock TV4, and a metering tube 2G is connected to the pressure reducing pump 7 through a solenoid valve 5VIO. ing. And t! ! A chromatography column 27 is connected to the compression vessel 18 via a solenoid valve 5VII. A vacuum pump 7 is connected to the chroma 1 column 27 via a solenoid valve SV9, and a developing solution tank 28 containing a developing solution for chromatography is connected via a metering pump 29 and a solenoid valve 5V12. There is. At the bottom of the chromatography column 27, there are discharge/& tank 30 and eluate tank 3 through a three-way cock TV4.
1 is connected to the liquid level sensor 3 which further controls the amount of liquid released.
2 is arranged in the chromatography column 27.

In the above configuration, when a predetermined amount of the sample that has been cut and homogenized by the homogenizer is put into the sample container 8 and activated, the solenoid valve SVI is fixed in the direction of the pressure reduction pump 7 so that the measuring tube 4 becomes a pressure reduction system. Open for a time, extraction solvent is drawn into the metering tube 4 from the extraction solvent tank 1 . After a predetermined period of time has elapsed, the solenoid valve SV1 cuts off communication with the pressure reducing pump 7 and opens the metering tube 4 system to atmospheric pressure. Therefore, over 1,000 f of the extraction solvent introduced into the nine pipes 4 is returned to the extraction solvent tank 1, and by maintaining a constant liquid level, the amount of extraction solvent can be accurately measured. . The conocooler vi is then opened and the extraction solvent is injected into the sample container 8. Here, the sample container 8 has a small hole in its upper lid and is kept open. The sample and extraction solvent in the sample container 8 are subjected to ultrasonic waves from the ultrasonic extractor 9, and residues attached to or incorporated into the sample are quickly and efficiently extracted with the extraction solvent. The extraction solution is sucked into the separation tank 11 through the filter 10 by opening the solenoid valve SV4. This extraction operation is repeated as many times as necessary.

Next, the solenoid valve SV2 and the cock TV2 are activated to draw a predetermined amount of saline water from the saline tank 2 into the measuring pipe 5 in the same manner as in the case of the measuring pipe 4 described above, and then into the separating tank 11. Similarly, solenoid valve SV3 and cock TV3
A predetermined amount of the separating solvent is drawn into the measuring tube 6 from the separating solvent tank 3 and then added into the separating tank 11. Thereafter, the stirrer 12 is operated for a predetermined period of time to sufficiently mix the solution, and then the solution is allowed to stand still, and the solution is separated into two phases: an aqueous extract and an aqueous raffinate. Next, so that the raffinate tank 14 becomes a pressure reducing system, the solenoid valve SV5 opens in the direction of the pressure reducing pump 7, and the cock MVI opens the raffinate tank 14+14, and the raffinate flows into the raffinate tank 14. be extracted. Then, similarly, solenoid valve S
When V6 opens in the direction of the vacuum pump 7, the cock MVI opens toward the extract tank 1G, and the extract is drawn out to the extract tank 1G via the dehydration tank 15 as necessary. When the interface between the raffinate liquid phase and the extract liquid phase is detected by the interface detection sensor 13 due to the difference in the electrical transmission of both phases, the solenoid valve S
V5, SV6 and cock MVI are controlled to accurately separate the raffinate and extract.

When all the waves are removed, the solenoid valve SV4 is opened again and the raffinate in the raffinate pq14 is returned to the separation tank 11 through the return passage 24, Liquid manipulation is performed and this is repeated as many times as necessary. Thereafter, the raffinate liquid is discharged outside the system by opening the cock MV2, and the extract liquid is supplied little by little into the concentration container 18 by opening the solenoid valve SV8 toward the pressure reducing pump 23 and opening the cock MV3. and a constant temperature water bath 19 in the concentration container 18.
Teka? mixed with magnetic stirrer 20,
The solvent is then evaporated and concentrated while the pressure is reduced by the reduced JI pump 23. When the extract liquid runs out, its state is detected by the liquid level sensor 17, and the pot MV3 is closed after a certain period of time. The emitted solvent is condensed in a condenser 21 and stored in a trap 22. After the concentration operation is completed in this way, next, the solenoid valve 5VIO is opened in the direction of the pressure reducing pump 7, and a predetermined amount of the melt is transferred from the melting solvent tank 25 to the measuring pipe 266 in the same manner as in the case of the measuring pipe 4 described above. After the solvent is sucked, the cock TV4 is opened and the extract is supplied into 1 g of the concentration container, and the extract is dissolved with the minimum necessary amount of solvent. After that, solenoid valve S
V9 is depressurized and opened in the direction of pump 7, and 5VII is opened to transfer the decomposed extract into the chromatography column 27. After the transfer is completed, the MV4 is opened to the effluent tank 30 side and a part of the solvent is released into the effluent liquid +! It will be released for ¥30.

At this time, the discharge amount is controlled by the liquid level sensor 32. Next, the metering pump 29 is activated and the solenoid valve 5 is activated.
VI2 was opened and the developing solution was supplied from the developing solution tank 28 to the chromatography column 27, and the cock MV4 was opened again to the effluent tank 30 side, and a predetermined amount of the first effluent was discharged to the effluent tank 30. The cock M4 is opened on the side of the eluate tank 3I, and a predetermined amount of eluate is taken out into the eluate tank 31.This eluate is analyzed by an analytical means such as gas chromatography or liquid chromatography to determine the residue. measurements are taken.

In the above embodiment, in the case where the separation solvent is one having a specific gravity smaller than water, such as Normanhexane or ethyl acetate, the raffinate is first taken out to the raffinate tank 14,
After that, we have explained the case where the above extract liquid is taken out to the extraction tank 16, but conversely, when using a separation solvent with a higher specific gravity than water, such as dichloromethane or chloroform,
First, pour the extract liquid into the extract tank 16 (cut it into the extraction tank 1).
The structure is such that it can be avoided.

Furthermore, in the dual embodiment, only one system is installed, but it is also possible to install multiple systems in parallel so that multiple extractions can be performed at the same time.

In addition, in the apparatus of the present invention as described above, each component can be adjusted by using, for example, a grinder 12, etc.
It is designed to be extremely easy to attach and detach.

〔Effect of the invention〕

According to the residue extraction device of the present invention, as described above, the ultrasonic extractor extracts the residue by applying ultrasonic waves to the sample container containing the sample and extraction solvent, and the extraction solution and the added a separation tank that mixes a saline solution and a separation solvent and then leaves it to stand to separate the liquid into an extract liquid and a raffinate liquid; a quantitative supply means that supplies a fixed amount of each of the extraction solvent, the saline solution, and the separation solvent; A separation means having an interface detection sensor that separates the separated extract liquid, a concentrator that heats the extract liquid under reduced pressure and evaporates the solvent to concentrate it, and a concentrator that melts the concentrated extract liquid. and a chromatography column for roughly purifying the extracted extract solution.This allows the residue to be quickly and efficiently extracted from the sample using an extraction solvent using ultrasonic waves. After separating the sample with saline and a separating solvent to obtain 1 fraction of the extract, it can be condensed by 1 and then passed through the Chroma 1 column to obtain the necessary fractions.Therefore, the sample This system has the following effects: residues can be automatically extracted in a short time, the extraction process becomes easier, there is no variation in extraction, and the measurement of residues can be easily and always accurately carried out. .

[Brief explanation of drawings]

The figure is a schematic configuration diagram of an embodiment of the present invention. ■ is an extraction solvent tank, 2 is a saline tank, 3 is a separation solvent tank, 4.
5.6.26! ;! : Total 9 tubes, 8 is test T-↓ container, 9
is an ultrasonic extractor, 10 is a filter, 11 is a separation tank, 1
2 is stirring υ■, 13 is an interface detection sensor, 14 is a raffinate tank, 15 is a dehydration tank, 16 is an extract tank, 17 and 32 are liquid level sensors, 1B is a concentration container, and 19 is a constant temperature water bath. , 20 is Magnetifuku Stara, 21 is Fuku F? 4 vessels, 22 is a trap, 7 and 23 are vacuum pumps, 25 is a dissolving solvent tank, 27 is a chromatography column, 28 is a developing liquid tank, 29 is a metering pump, 3
0 is a discharge liquid tank, 31 is an eluate tank, SVI to 12 are solenoid valves, and TVI to iMV1 to 4 are cocks.

Claims (1)

[Claims] 1. An ultrasonic extractor that applies ultrasonic waves to the sample container containing the sample and extraction solvent to extract the residue, and mixes the extraction solution, added saline, and separation solvent, and then leaves it still. a separation tank that separates the extract into an extract liquid and a raffinate; a quantitative supply means that supplies a fixed amount of the extraction solvent, the saline solution, and the separation solvent, respectively;
A separation means having an interface detection sensor that separates the separated extract, a concentrator that heats the extract under reduced pressure and evaporates the solvent to concentrate it, and melts and extracts the concentrated extract. 1. A residue extraction device comprising: a means for extracting a residue; and a chromatography column for purifying the extracted extract solution.