CN219110887U

CN219110887U - Online small-size pressure membrane extraction module

Info

Publication number: CN219110887U
Application number: CN202222973836.2U
Authority: CN
Inventors: 赵梅; 宁霄; 曹进; 金绍明; 许鸣镝; 孙姗姗; 董喆
Original assignee: National Institutes for Food and Drug Control
Current assignee: National Institutes for Food and Drug Control
Priority date: 2022-11-09
Filing date: 2022-11-09
Publication date: 2023-06-02
Anticipated expiration: 2032-11-09

Abstract

The utility model discloses an online small pressure membrane extraction module, which relates to the technical field of food and environmental research, and is technically characterized in that: the device comprises a module body, wherein an extraction film is fixedly arranged in the module body, and the interior of the module body is divided into an extraction bin and an extraction bin by the extraction film; the side wall of the extraction bin is provided with a first injection port, a second injection port and a second outlet, and the extraction bin is internally provided with a solvent dispersion block and a blocking module; the solvent dispersion block is positioned at the joint of the first injection port and the module body, and the blocking module is positioned at the joint of the second outlet and the module body; and the side wall of the extraction bin is provided with an injection port III and an outlet I. The module can be used for efficiently extracting the weak polar and volatile components in a small amount of samples.

Description

Online small-size pressure membrane extraction module

Technical Field

The utility model relates to the technical field of food and environmental research, in particular to an on-line small pressure membrane extraction module.

Background

In the fields of food and environment, there are more parts with the distribution of the components to be detected in the sample in fat-soluble or fat-soluble parts, and the corresponding components are substances which are easy to be absorbed and contacted by human beings or animals and plants, and particularly a large number of dangerous substances such as organic pollutants, agricultural and veterinary drugs, natural hormones and the like exist. The above components are volatile or weakly polar components in terms of polarity and physicochemical properties. In the existing detection research and daily treatment, the common purification generally comprises the steps of homogenization, extraction, purification and detection, namely solid phase extraction, liquid-liquid extraction, solid-liquid extraction, physical phase separation and the like, however, the common extraction purification mode has the requirement of large sample demand due to the limitation and the trace requirement of taking samples, and the purification requirement of the trace samples is difficult to meet, so that under the condition of lower concentration of the detected target substances, the purification contradiction is particularly prominent, and the problems of inaccurate test value and larger test error are caused.

In recent years, the purification of a commonly used solid dispersion mode has certain requirements on the sample quantity, has limitation on the treatment of a trace amount of liquid sample, and is difficult to effectively recover or enrich corresponding target objects in a uniform environment completely, so that the detection is inaccurate. Non-porous membranes, which are a liquid or solid (e.g., polymer) phase, typically an aqueous phase, sandwiched between two other phases, one of which contains the component to be extracted, i.e., the donor phase, can be used to extract the weakly polar and non-polar compounds from the liquid sample with minimal amounts of organic solvents. The other side of the membrane is the receptor moiety. In most cases, the driving force for the extraction process on the membrane is the concentration gradient. If a small volume, stagnant receptor phase is used, a highly enriched fraction of the extracted components can be obtained. Thus, existing membrane extraction has the advantage over traditional liquid-liquid extraction (LLE) that less organic solvent is used, higher enrichment of species can be obtained, and it can be easily incorporated into a flow system and automatically coupled to HPLC, GC or capillary electrophoresis on-line. Different variations of the above techniques include support for liquid film extraction (SLM), microporous film liquid-liquid extraction (MMLLE), polymeric film extraction (PME) and membrane extraction with adsorbent interface (MESI). However, the existing researches have the problems that the extraction efficiency fluctuates and the sample treatment effect is poor.

Based on the above problems, the applicant devised an on-line small pressure membrane extraction module.

Disclosure of Invention

The utility model aims to provide an on-line small-sized pressure membrane extraction module which can be used for efficiently extracting weak polar and volatile components in a small quantity of samples.

The technical aim of the utility model is realized by the following technical scheme: an on-line small pressure membrane extraction module comprises a module body, wherein an extraction membrane is fixedly arranged in the module body, and the interior of the module body is divided into an extraction bin and an extraction bin by the extraction membrane;

the side wall of the extraction bin is provided with a first injection port, a second injection port and a second outlet, and the extraction bin is internally provided with a solvent dispersion block and a blocking module; the solvent dispersion block is positioned at the joint of the first injection port and the module body, and the blocking module is positioned at the joint of the second outlet and the module body;

and the side wall of the extraction bin is provided with an injection port III and an outlet I.

Further, a stop valve is arranged on the second outlet.

Further, the volume size of the extraction bin is 500-1000 mu L, and the volume size of the extraction bin is one third of the volume size of the extraction bin.

Further, the extraction membrane comprises two porous metal sieve plates and a thin membrane plate, wherein the thin membrane plate is filled between the two porous metal sieve plates, and the two porous metal sieve plates are fixedly connected with the inner side wall of the module body.

Further, the blocking module is a porous stainless steel sieve plate.

In summary, the utility model has the following beneficial effects:

1. the extraction module is suitable for extracting substances in a small amount of liquid samples or suspension extracting solution, and compared with a conventional micro-extraction device, the extraction module can realize batch processing of samples, and related operations can realize an automatic function and online;

2. the thin film plate is made of organic materials, so that the thin film plate is suitable for passing weak polar substances to realize extraction;

3. a blocking module is arranged at the joint of the second outlet and the module body and can be used for blocking the solution, so that the time of the second outlet in the extraction bin is delayed;

4. a stop valve is arranged on the second outlet, so that the retention time of the solution with low viscosity in the extraction bin can be prolonged;

5. the solvent dispersing block is arranged at the joint of the first injection port and the extraction bin, so that the solvent can be uniformly dispersed and injected into the extraction bin, and the real-time mixing with the sample solution is ensured.

Drawings

FIG. 1 is a schematic diagram of an on-line small-scale pressure membrane extraction module according to embodiment 1 of the present utility model;

fig. 2 is a schematic structural diagram of an on-line small-sized pressure membrane extraction module in embodiment 2 of the present utility model.

In the figure: 1. an injection port I; 2. a solvent dispersion block; 3. an injection port II; 4. an injection port III; 5. an extraction membrane; 6. an extraction bin; 7. an outlet I; 8. an outlet II; 9. a blocking module; 10. a module body; 11. an extraction bin; 12. and a stop valve.

Detailed Description

The present utility model will be described in further detail with reference to fig. 1 and 2.

Example 1: an on-line small pressure membrane extraction module is shown in fig. 1, and comprises a module body 10, wherein an extraction membrane 5 is fixedly arranged in the module body 10, and the extraction membrane 5 divides the interior of the module body 10 into an extraction bin 11 and an extraction bin 6;

the side wall of the extraction bin 11 is provided with an injection port I1, an injection port II 3 and an outlet II 8, wherein the injection port II 3 is connected with an injection pump, and the injection pump is used for injecting sample suspension or liquid sample into the extraction bin 11; the first injection port 1 is connected with a solvent pump, and the extraction solvent is injected into the extraction bin 11 through the solvent pump, so that the liquid sample and the extraction solvent are fully mixed in the extraction bin 11; the extraction bin 11 is also fixedly provided with a solvent dispersion block 2 and a blocking module 9; the solvent dispersion block 2 is positioned at the joint of the injection port I1 and the module body 10, and the blocking module 9 is positioned at the joint of the outlet II 8 and the module body 10; the solvent dispersing block 2 is arranged to realize the uniform dispersion and injection of the solvent into the extraction bin 11, so that the real-time mixing with the sample solution is ensured; in development, experiments prove that under the three conditions of solution samples, extract suspension samples and extract samples, the dispersing blocks are added and the dispersing blocks are not added, and table 1 shows that after the dispersing blocks are added, the samples can be uniformly mixed in real time, so that the effective extraction of the samples is ensured.

TABLE 1

The blocking module 9 is arranged to provide a certain back pressure and form a blocking of the solvent; the pressure in the extraction chamber 11 is provided by a solvent pump connected to the inlet one 1.

The side wall of the extraction bin 6 is provided with an injection port III 4 and an outlet I7, the injection port III 4 is used for injecting the receiving solvent, and the outlet I7 is used for collecting the receiving solution for detection.

In this embodiment, preferably, the volume size of the extraction bin 11 is 500-1000 μl, the volume size of the extraction bin 6 is one third of the volume size of the extraction bin 11, and the efficient extraction of the weak polar substances in the sample is realized through the small-volume extraction module.

In this embodiment, the extraction membrane 5 preferably includes two porous metal sieve plates and a thin membrane plate, the thin membrane plate is filled between the two porous metal sieve plates, and the two porous metal sieve plates are fixedly connected with the inner side wall of the module body 10, wherein the thin membrane plate is made of extraction materials such as polyester, fiber, and the like.

In this embodiment, the thin film plate is preferably made of an organic material.

In the preferred embodiment, the blocking module 9 is an inert porous stainless steel sieve plate; in this example, the thickness, average pore size, etc. of the porous stainless steel sieve plate were compared, and the results are shown in table 2 (the injected samples are peony extract and alcohol extract).

TABLE 2

From the results, it is shown that the sample can be effectively mixed in the extraction chamber 11 with a certain residence time, the system pressure is achieved, and in practice, the second outlet 8 can be cut off to achieve an effective mixing and residence time.

In this example, the results of the hydrothermal liquid extraction and the extraction after passing through the membrane plate were compared by the test, the weight of the volatile substances in the latter was increased by 30% compared with the former, which means that the extraction efficiency can be improved more under the pressure condition, and the dynamic extraction condition of the lower extraction chamber 6 was compared, and the results are shown in table 3 (taking paeoniflorin body fluid as an example, the middle pore fiber membrane plate, and the upper pressure is 100 psi).

TABLE 3 Table 3

The results show that in the general extraction state, the complete extraction can be obtained by 2-3 extraction bins and 6 volumes, and after dynamic extraction, less solvent volume and faster time can be realized.

Working principle: the injection pump is used for injecting sample suspension or liquid sample into the extraction bin 11, meanwhile, the solvent pump is used for pumping extraction solvent which can be mixed with the sample solution, the connection part of the first injection port and the module body 10 is connected through the solvent dispersion block 2, the solvent can be uniformly dispersed and injected into the extraction bin 11, real-time mixing with the sample solution is guaranteed, after the sample solution is injected, the second injection port 3 is cut off, the pressure in the extraction bin 11 is provided by the solvent pump externally connected with the first injection port 1, the output port on the extraction bin 11 is fixedly connected with the blocking module 9 and communicated with waste liquid, the blocking module 9 is used for providing certain back pressure and forming blocking of the solvent, the sample solution fully contacts with the pre-injected receiving solvent in the extraction bin 6 through the extraction membrane 5, extraction of weak polar substances is provided, the output port of the extraction bin 6 is not cut off in the extraction process, and after a certain time, the receiving solution is collected by the first outlet 7 for detection.

Example 2: as shown in fig. 2, the on-line small-sized pressure membrane extraction module is different from the embodiment 1 in that a shut-off valve 12 is installed on the outlet two 8; in this way, the retention time of the solution in the extraction chamber 11 can be further prolonged for the solution with a lower viscosity and under a certain pressure.

Example 3: a method for using the miniature pressure membrane extraction module on line includes such steps as filling 200 microliter of fluid extract of notoginseng into 1.5 ml of extraction chamber 11, cutting off the injection port of sample, filling the alcohol of extraction solvent at 500 microliter/min, cutting off the liquid outlet, using hollow fibrous plate with 1 mm thickness, continuously filling ethyl acetate as extraction solvent into lower extraction chamber 6, extracting for three min, dynamic collecting 600 microliter solution, measuring total saponins of notoginseng, and comparing with alcohol extraction method.

Example 4: a method for using an on-line miniature pressure membrane extraction module includes such steps as connecting the sample injection pump, extracting solvent and receiving solvent pump to be connected, injecting 200 microliter of meat slurry containing inosine into 1.5 ml of extraction bin 11, cutting off sample injection port, injecting acetonitrile as extracting solvent at 500 microliter/min, cutting off waste liquid port, using hollow fibrous plate with thickness of 1 mm, continuously injecting acetone as extracting solvent into lower extraction bin 6, extracting for three min, dynamically collecting 600 microliter of solution, measuring inosine content, comparing with alcohol extraction method, and increasing inosine result by 30%.

The present embodiment is only for explanation of the present utility model and is not to be construed as limiting the present utility model, and modifications to the present embodiment, which may not creatively contribute to the present utility model as required by those skilled in the art after reading the present specification, are all protected by patent laws within the scope of claims of the present utility model.

Claims

1. An on-line small-sized pressure membrane extraction module comprises a module body (10), and is characterized in that: an extraction film (5) is fixedly arranged in the module body (10), and the extraction film (5) divides the interior of the module body (10) into an extraction bin (11) and an extraction bin (6);

the side wall of the extraction bin (11) is provided with an injection opening I (1), an injection opening II (3) and an outlet II (8), and the extraction bin (11) is internally provided with a solvent dispersion block (2) and a blocking module (9); the solvent dispersion block (2) is positioned at the joint of the injection port I (1) and the module body (10), and the blocking module (9) is positioned at the joint of the outlet II (8) and the module body (10);

the side wall of the extraction bin (6) is provided with an injection port III (4) and an outlet I (7).

2. An on-line mini-size pressure membrane extraction module as in claim 1, wherein: and a stop valve (12) is arranged on the second outlet (8).

3. An on-line mini-size pressure membrane extraction module as in claim 1, wherein: the volume size of the extraction bin (11) is 500-1000 mu L, and the volume size of the extraction bin (6) is one third of the volume size of the extraction bin (11).

4. An on-line mini-size pressure membrane extraction module as in claim 1, wherein: the extraction membrane (5) comprises two porous metal sieve plates and a thin membrane plate, wherein the thin membrane plate is filled between the two porous metal sieve plates, and the two porous metal sieve plates are fixedly connected with the inner side wall of the module body (10).

5. An on-line mini-size pressure membrane extraction module as in claim 1, wherein: the blocking module (9) is a porous stainless steel sieve plate.