A rapid detection device for food additives in pre-prepared dishes

Abstract

The present application discloses a rapid detection device for food additives in pre-prepared dishes, and relates to the technical field of food additive detection devices, including: a modularly arranged high-performance liquid chromatography device and a detection system, wherein the high-performance liquid chromatography device is stacked and connected in sequence from top to bottom and is provided with a vacuum degassing system, an injection system, a mobile phase delivery system and a separation system, wherein the detection system comprises a detector and a workstation connected to the high-performance liquid chromatography device; the injection system comprises a plurality of groups of sample liquid processing components, wherein the sample liquid processing components integrate mutually nested ultrasonic microwave extraction components and a centrifuge, wherein the centrifuge is provided with an accommodation hole for accommodating a sample liquid storage bottle; the mobile phase delivery system comprises an integrated processing component and a plurality of mobile phase storage tubes that are interconnected; and the separation system comprises a plurality of groups of elution components, so as to cope with the problem of low detection efficiency due to the wide variety of additives in pre-prepared dishes.

Description

Technical Field

[0001] The present application relates to the technical field of food additive detection equipment, and in particular to a rapid detection equipment for food additives in pre-prepared dishes. Background Art

[0002] Pre-prepared meals are finished or semi-finished dishes that are produced by pre-processing, pre-cooking, and pre-packaging food ingredients in a standardized assembly line. Due to the short development time of pre-prepared meals and the lack of a unified standard and other regulatory systems, the quality of pre-prepared meals varies greatly. In addition, based on the long-term storage requirements of pre-prepared meals, most of the dishes on the market today are heavy-tasting home-cooked meat dishes that are high in oil and salt.

[0003] Preservatives are usually added to prepared meat dishes to inhibit microorganisms, antioxidants are added to reduce fat oxidation, and sweeteners are added for seasoning. However, in order to improve the taste and shelf life, there is a phenomenon of manufacturers abusing additives. Long-term consumption of excessive amounts of food additives such as preservatives and sweeteners will seriously damage liver and kidney function and affect physical health. Testing is needed to determine whether there is a problem of abuse of additives or excessive use.

[0004] There are various methods for testing food additives, including spectroscopy, gas chromatography, liquid chromatography, etc. Considering the resistance to matrix and the requirements for physical properties of samples, high performance liquid chromatography is the most suitable method for testing meat food additives. In order to improve the detection efficiency, there is a high performance liquid chromatography method that can quickly detect multiple food additives at the same time. However, in actual production, different manufacturers and different foods have different types of food additives added. It is unrealistic to cover the content of all additives in a single test. Multiple tests require sample pretreatment and the selection of chromatographic conditions. The process is complicated and it is difficult to ensure detection efficiency.

[0005] Therefore, it is necessary to provide a rapid detection device for food additives in pre-prepared dishes to solve the problems raised in the above background technology. Summary of the invention

[0006] To achieve the above-mentioned purpose, the present application provides the following technical solutions: a rapid detection device for food additives in pre-prepared dishes, comprising: a modularly arranged high-performance liquid chromatography device and a detection system, wherein the high-performance liquid chromatography device is stacked and connected in sequence from top to bottom and is provided with a vacuum degassing system, a sample injection system, a mobile phase delivery system and a separation system, and the detection system comprises a detector and a workstation connected to the high-performance liquid chromatography device;

[0007] The sample injection system comprises a plurality of sample liquid processing components, wherein the sample liquid processing components integrate mutually nested ultrasonic microwave extraction components and centrifuges, wherein the centrifuge is provided with a placement hole for placing a sample liquid storage bottle, and a filter screen is arranged in the sample liquid storage bottle;

[0008] The mobile phase delivery system comprises an integrated processing unit and a plurality of mobile phase storage tubes that are interconnected;

[0009] The separation system comprises a plurality of elution components, and the elution components are composed of an adjusting clamping plate, a heat preservation ring and a chromatographic column.

[0010] Furthermore, preferably, the sample injection system further comprises: a module square shell for accommodating the sample liquid processing components, and a delivery pipeline and a distribution slide member are also arranged in the module square shell, and a single distribution slide member corresponds to two sample liquid processing components.

[0011] Further, as a preference, a mechanical arm is provided on the distribution slide member, and the mechanical arm clamps a blender and a liquid adding tube connected to the conveying pipeline.

[0012] Furthermore, preferably, the robotic arm also clamps a sample liquid extraction connector, and the blender, liquid adding tube and sample liquid extraction connector are adjusted to move to above different sample liquid storage bottles through the distribution slide and the robotic arm, and the adjustment method also includes height adjustment.

[0013] Furthermore, preferably, the mobile phase delivery system further comprises: a stand provided with a plurality of sockets, wherein the sockets are used to accommodate the mobile phase storage tubes, the integrated processing unit is also arranged on the stand, and a metering pump is also arranged on the stand.

[0014] Further, as a preference, the lower end of the mobile phase storage tube is connected to the integrated processing unit, and the upper end of the mobile phase storage tube is connected to the metering pump via a hose.

[0015] Further, preferably, the separation system also includes a plurality of constant flow plunger pumps, one end of a single constant flow plunger pump is connected to a group of the elution components, and the other end is correspondingly connected to a mobile phase storage tube and an injection loop tube.

[0016] Further, preferably, the insulation rings are symmetrically arranged at both ends of the chromatographic column, and an insulation sleeve is sleeved on the outside of the chromatographic column, both ends of the insulation sleeve contact the insulation rings, and the adjustment clamp clamps the insulation sleeve for deflection.

[0017] Compared with the prior art, the present application provides a rapid detection device for food additives in pre-prepared dishes, which has the following beneficial effects:

[0018] 1. The sample injection system in this application uses an ultrasonic microwave extraction unit for microwave treatment and a centrifuge for centrifugal treatment, and at the same time, the sample is filtered and stored in a sample storage bottle. The entire processing process is integrated and automated, and the crushing, extraction, centrifugation, filtration, storage and cleaning are integrated into a process, which reduces the difficulty of repeated operations and refined operations, improves sample processing efficiency, and provides guarantees for subsequent batch testing;

[0019] 2. The mobile phase delivery system and separation system in this application can adjust the mobile phase ratio and flow rate independently and conveniently, and adapt to multiple detection methods at the same time, so as to achieve simultaneous detection of additives covering the product at the same time, avoid the phenomenon of additional detection of single additives, and achieve the purpose of reducing detection time and improving detection efficiency. BRIEF DESCRIPTION OF THE DRAWINGS

[0020] Other features, objects and advantages of the present application will become more apparent by reading the detailed description of non-limiting embodiments with reference to the following drawings:

[0021] Figure 1 The figure is a schematic diagram of the overall structure of a rapid detection device for food additives in pre-prepared dishes;

[0022] Figure 2 The schematic diagram of the structure of the sampling system of a rapid detection device for food additives in pre-prepared dishes is shown;

[0023] Figure 3 This is a schematic diagram of the structure of a sample liquid processing component of a rapid detection device for food additives in prepared dishes;

[0024] Figure 4 A schematic diagram of the structure of a sampling system for a rapid detection device for food additives in prepared dishes;

[0025] Figure 5 It is a schematic diagram of the structure of a mobile phase delivery system of a rapid detection device for food additives in prepared dishes;

[0026] Figure 6 The schematic diagram of the separation system structure of a rapid detection device for food additives in pre-prepared dishes is shown in FIG.

[0027] In the figure: 1. Vacuum degassing system; 2. Sampling system; 21. Module square shell; 22. Sample liquid processing component; 221. Ultrasonic microwave extraction component; 222. Centrifuge; 223. Placement hole; 23. Delivery pipeline; 24. Distribution slide plate; 25. Blender; 26. Liquid adding tube; 27. Sample liquid storage bottle; 28. Filter; 3. Mobile phase delivery system; 31. Stand; 311. Socket; 32. Integrated processing component; 33. Metering pump; 34. Mobile phase storage tube; 4. Separation system; 41. Adjustment splint; 42. Insulation ring; 43. Chromatographic column; 44. Constant flow plunger pump; 5. Detector. DETAILED DESCRIPTION

[0028] See also Figure 1-6 In an embodiment of the present application, a rapid detection device for food additives in pre-prepared dishes comprises: a modularly arranged high-performance liquid chromatography device and a detection system, wherein the high-performance liquid chromatography device is stacked and connected in sequence from top to bottom and is provided with a vacuum degassing system 1, a sampling system 2, a mobile phase delivery system 3 and a separation system 4, and the detection system comprises a detector 5 and a workstation connected to the high-performance liquid chromatography device, and the specific vacuum degassing system 1 has a built-in vacuum degasser for vacuum degassing the inside of containers and pipelines, and the detector 5 and the workstation are used for sample signal recognition, signal recording and data acquisition output;

[0029] The sample injection system 2 includes a plurality of sample liquid processing components 22, wherein the sample liquid processing components 22 integrate mutually nested ultrasonic microwave extraction components 221 and centrifuges 222, wherein the centrifuges 222 are provided with placement holes 223 for placing sample liquid storage bottles 27, and the sample liquid storage bottles 27 are provided with filter screens 28;

[0030] The mobile phase delivery system 3 comprises an integrated processing unit 32 and a plurality of mobile phase storage tubes 34 which are interconnected;

[0031] The separation system 4 comprises a plurality of elution components, and the elution components are composed of an adjustment clamp 41 , a heat preservation ring 42 and a chromatographic column 43 .

[0032] It should be explained that during the working process, the inside of the container and the pipeline are first vacuum degassed by the vacuum degassing system 1, and the sample processing is completed in the injection system 2 and the mobile phase is prepared in the mobile phase delivery system 3. Then, a suitable chromatographic column 43 is installed in the separation system 4. After the preparation is completed, the power supply of each module is started, the communication is established between the high-performance liquid chromatography device and the detection system, and the pipeline is cleaned by the mobile phase delivery system 3;

[0033] After cleaning, according to the existing method of simultaneously detecting multiple additives, automatically compare and cover all or as many types of additives in the samples as possible, and select multiple suitable methods based on the shortest time as the screening condition, automatically set up the complete method editing at the workstation, set the flow rate, temperature and other parameters, and record the batch information;

[0034] Then, the system is started and waited for stable operation, and the sample liquid is transported through the sample injection system 2. After the analysis, the chromatographic column 43 is flushed with an appropriate solvent, and the system is exited and closed. Finally, qualitative analysis is performed based on the retention time of the liquid chromatogram, and quantitative analysis is performed based on the peak area and peak height.

[0035] It should be explained that the following is an explanation of the relevant contents using two liquid chromatography methods for detecting multiple food additives running simultaneously:

[0036] Scheme 1: Eight additives including acesulfame potassium, benzoic acid, tartrazine, amaranth, caffeine, sunset yellow, sorbic acid and saccharin sodium were determined simultaneously. Methanol-ammonium acetate (20 mmol / L, pH = 7.0) was used as the mobile phase. The flow rate was 0.8 ml / min-1.0 ml / min, the injection volume was 5 μL, and gradient elution was performed. The chromatographic column was Diamomsil Plus-C18 column (4.6 mm × 250 mm × 5 μm) and the temperature was 30 °C.

[0037] Scheme 2: Simultaneous measurement of four additives: benzoic acid, sorbic acid, dehydroacetic acid, and saccharin sodium. Using 0.2 mmol / L ammonium acetate-methanol (97:3), a flow rate of 1.0 ml / min, an injection volume of 20 μL, and isocratic elution. The chromatographic column is XDB-C18 (4.6 mm×250 mm×5 μm) and the temperature is 35°C.

[0038] In this embodiment, as shown in the figure, the injection system 2 also includes: a module square shell 21 for accommodating the sample liquid processing component 22, and a delivery pipeline 23 and a distribution slide 24 are also arranged in the module square shell 21. The specific distribution slide 24 is a controllable movable platform composed of a support plate, a base plate and a screw. The delivery pipeline 23 integrates an injection valve, an injection loop tube, an initial sample liquid input tube and a preparation liquid delivery tube. A single distribution slide 24 corresponds to two sample liquid processing components 22.

[0039] As a preferred embodiment, a mechanical arm is provided on the distribution slide member 24 , and the mechanical arm clamps a blender 25 and a liquid adding pipe 26 connected to the conveying pipeline 23 .

[0040] As a preferred embodiment, the robotic arm also clamps a sample liquid extraction connector, and the distribution slide 24 and the robotic arm are used to adjust the blender 25, the liquid adding tube 26 and the sample liquid extraction connector to move to different sample liquid storage bottles 27, and the adjustment method also includes height adjustment. The specific sample liquid extraction connector can pass through the filter net 28 to control the extraction of the processed sample liquid through the injection valve, and the sample liquid extraction connector has a built-in replaceable filter membrane for subsequent sample liquid transportation through the injection loop tube; the blender 25 further crushes the original sample liquid transmitted through the initial sample liquid input tube, and adds the sample liquid to the sample liquid storage bottle 27, and the liquid adding tube 26 is used to add reagents for adjustment or cleaning.

[0041] It should be explained that after the initial sample liquid is initially crushed, it is transported into the sampling system 2 for further processing, including microwave treatment with the help of an ultrasonic microwave extraction element 221 and centrifugal treatment with a centrifuge 222, and at the same time filtering and storing in a sample liquid storage bottle 27. The entire processing process is integrated and automated, and crushing, extraction, centrifugation, filtration, storage and cleaning are processed in an integrated process, which reduces the difficulty of repeated operations and refined operations, improves sample processing efficiency, and provides guarantees for subsequent batch testing.

[0042] In this embodiment, the mobile phase delivery system 3 further comprises: a stand 31 with a plurality of sockets 311 , wherein the sockets 311 are used to place the mobile phase storage tubes 34 , and the integrated processing unit 32 is also placed on the stand 31 , and a metering pump 33 is also provided on the stand 31 .

[0043] As a preferred embodiment, the lower end of the mobile phase storage tube 34 is connected to the integrated processing unit 32. Specifically, the integrated processing unit 32 includes multiple eluent raw material storage tanks, cleaning liquid storage tanks and matching delivery pumps, and a single mobile phase storage tube 34 is connected to each storage tank. The upper end of the mobile phase storage tube 34 is connected to the metering pump 33 by means of a hose.

[0044] It should be explained that inappropriate mobile phase and elution method may result in some additives not being separated or the elution time being too long. For different additive combinations, the existing additive combination determination generally has an adapted elution method;

[0045] The integrated processing unit 32 can provide different raw materials in different proportions in different mobile phase storage tubes 34 to construct different mobile phases and adapt to different elution methods;

[0046] There are two different mobile phases and elution modes:

[0047] Method 1: Acesulfame potassium, benzoic acid, tartrazine, amaranth, caffeine, sunset yellow, sorbic acid and saccharin sodium were determined simultaneously, (20mmol / L, pH=7.0) methanol-ammonium acetate was used as the mobile phase, wherein the ratio of methanol to ammonium acetate varied from 2:23, 1:9, 3:7, 3:2, at a flow rate of 0.8ml / min-1.0ml / min, with an injection volume of 5μL, and gradient elution was performed.

[0048] Method 2: Mixed measurement of benzoic acid, sorbic acid, dehydroacetic acid and saccharin sodium, using 0.2mmol / L ammonium acetate-methanol (97:3), 1.0ml / min flow rate, 20μL injection volume, and isocratic elution.

[0049] The gradient elution method and isocratic elution method adopted in the above two methods can be controlled and adjusted by controlling the proportion of raw materials transported into the mobile phase storage tube 34 through the integrated processing unit 32, and multiple mobile phase storage tubes 34 support independent provision of different mobile phases, supporting the above two methods to run simultaneously in the device to detect samples.

[0050] In this embodiment, as shown in the figure, the separation system 4 also includes a plurality of constant flow plunger pumps 44, one end of a single constant flow plunger pump 44 is connected to a group of the elution components, and the other end is correspondingly connected to a mobile phase storage tube 34 and an injection loop tube, and a valve is also provided between the specific constant flow plunger pump 44 and the mobile phase storage tube 34.

[0051] As a preferred embodiment, the insulation ring 42 is symmetrically arranged at both ends of the chromatographic column 43, and the chromatographic column 43 is externally sleeved with an insulation sleeve, both ends of the insulation sleeve contact the insulation ring 42, and the adjustment clamp 41 clamps the insulation sleeve for deflection. Specifically, the chromatographic column 43 can be installed and replaced by deflecting the insulation sleeve upward to separate from the insulation ring 42.

[0052] It should be explained that a single elution component can provide an independent insulation environment, and different chromatographic columns 43 can be set inside, providing a basis for multiple detection methods to be carried out simultaneously, and the mobile phase ratio and flow rate can be adjusted independently and conveniently. At the same time, it is suitable for multiple detection methods to achieve simultaneous detection of additives in the product, avoid additional detection of single additives, etc., and achieve the purpose of reducing detection time and improving detection efficiency.

[0053] In the specific implementation, according to the types of additives in the sample, the existing high performance liquid chromatography method for simultaneously determining multiple additives is screened, and a single or multiple methods are selected according to the requirement of covering all types of sample additives with the least number of methods. According to the fingerprint spectrum of the additive mixed standard solution, each method obtains the chromatographic conditions of the chromatographic column 43, mobile phase system, elution method, pH of the buffer solution, column temperature and flow rate, and completes the sample processing in advance. Under the optimal chromatographic conditions, multiple methods are operated simultaneously, and then the target additive content in the sample is determined. This is very suitable for the situation where the existing pre-prepared dishes have a wide variety of additives and confusion. At the same time, it provides an equipment foundation for improving the elution method according to the type of product additives and further reducing the detection time.

[0054] What has been described above is only a preferred specific implementation manner of the present application, but the protection scope of the present application is not limited thereto. Any technician familiar with the technical field can make equivalent substitutions or changes within the technical scope disclosed in the present application according to the technical solution and application concept of the present application, which should be covered by the protection scope of the present application.

Claims

1. A rapid detection device for food additives in pre-prepared dishes, characterized by: The invention comprises a modularly arranged high performance liquid chromatography device and a detection system, wherein the high performance liquid chromatography device is stacked and connected in sequence from top to bottom and is provided with a vacuum degassing system (1), a sample injection system (2), a mobile phase delivery system (3) and a separation system (4), wherein the vacuum degassing system (1) has a built-in vacuum degasser for performing vacuum degassing treatment on the inside of a container and a pipeline; the detection system comprises a detector (5) and a workstation connected to the high performance liquid chromatography device, wherein the detector (5) and the workstation are used for sample signal recognition, signal recording and data acquisition and output; The sample injection system (2) comprises a plurality of sample liquid processing components (22), wherein the sample liquid processing components (22) integrate mutually nested ultrasonic microwave extraction components (221) and centrifuges (222), wherein the centrifuge (222) is provided with a placement hole (223) for placing a sample liquid storage bottle (27), and a filter screen (28) is arranged in the sample liquid storage bottle (27); The sample injection system (2) further comprises: a module square shell (21) for accommodating the sample liquid processing assembly (22), and a delivery pipeline (23) and a distribution slide member (24) are also arranged in the module square shell (21), and a single distribution slide member (24) corresponds to two sample liquid processing assemblies (22); the delivery pipeline (23) integrates a sample injection valve, a sample injection loop, an initial sample liquid input pipe and a preparation liquid delivery pipe; The distribution slide plate (24) is provided with a mechanical arm, and the mechanical arm clamps a blender (25) and a liquid adding pipe (26) connected to the conveying pipeline (23); The mechanical arm also holds a sample liquid extraction connector, and the blender (25), the liquid adding tube (26) and the sample liquid extraction connector are adjusted to move above different sample liquid storage bottles (27) through the distribution slide member (24) and the mechanical arm, and the adjustment method also includes height adjustment; The sample liquid extraction joint passes through the filter screen (28) and controls the extraction of the processed sample liquid through the injection valve, and the sample liquid extraction joint has a replaceable filter membrane built in it, which is used to subsequently transport the sample liquid through the injection loop tube; the pulverizer (25) further pulverizes the original sample liquid transmitted through the initial sample liquid input tube, and then adds the sample liquid to the sample liquid storage bottle (27), and the liquid adding tube (26) is used to add a reagent for preparation or cleaning; The mobile phase delivery system (3) comprises an integrated processing unit (32) and a plurality of mobile phase storage tubes (34) which are interconnected; The integrated processing unit (32) contains a plurality of eluent raw material storage tanks, cleaning liquid storage tanks and matching delivery pumps, and a single mobile phase storage pipe (34) is connected to each storage tank; The mobile phase delivery system (3) further comprises: a stand (31) provided with a plurality of sockets (311), wherein the sockets (311) are used to place the mobile phase storage tube (34), the integrated processing unit (32) is also placed on the stand (31), and a metering pump (33) is also arranged on the stand (31); The lower end of the mobile phase storage tube (34) is connected to the integrated processing unit (32), and the upper end of the mobile phase storage tube (34) is connected to the metering pump (33) by means of a hose; The separation system (4) comprises a plurality of elution components, wherein the elution components are composed of an adjustment clamping plate (41), a heat preservation ring (42) and a chromatographic column (43); The separation system (4) also includes a plurality of constant flow plunger pumps (44), one end of a single constant flow plunger pump (44) is connected to a group of elution components, and the other end is correspondingly connected to a mobile phase storage tube (34) and an injection loop tube.

2. The rapid detection device for food additives in pre-prepared dishes according to claim 1, characterized in that: The insulation ring (42) is symmetrically arranged at both ends of the chromatographic column (43), and the chromatographic column (43) is externally sleeved with an insulation sleeve, both ends of the insulation sleeve contact the insulation ring (42), and the adjustment clamping plate (41) clamps the insulation sleeve for deflection.

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