A pretreatment device for detecting OPO functional oils in dairy products
By designing a fully automated dairy product pretreatment device, the problems of complex, time-consuming, and low-precision pretreatment processes for detecting functional oils such as OPO in dairy products have been solved. This device achieves efficient and safe sample processing and is suitable for large-volume sample processing.
Patent Information
- Authority / Receiving Office
- CN · China
- Patent Type
- Utility models(China)
- Current Assignee / Owner
- ZHEJIANG GONGZHENG INSPECTION CENT CO LTD
- Filing Date
- 2025-05-26
- Publication Date
- 2026-06-30
AI Technical Summary
The existing technology for detecting functional oils such as OPO in dairy products involves a complex, time-consuming, and inefficient pretreatment process. Manual operation leads to insufficient accuracy and poses safety risks.
Design a pretreatment device for detecting functional oils such as OPO in dairy products, including an oil extraction module and a reagent loading module, to realize a fully automated process of total lipid extraction, separation of functional oils such as OPO, and removal of interfering substances, using an autosampler and a solid-phase extraction device for automated operation.
It achieves high efficiency, precision and safety in the pretreatment process of dairy products, is suitable for large-scale sample processing, reduces the contact between laboratory personnel and organic reagents, and improves safety and processing efficiency.
Smart Images
Figure CN224435899U_ABST
Abstract
Description
Technical Field
[0001] This utility model belongs to the field of experimental instruments, and specifically relates to a pretreatment device for detecting functional oils such as OPO in dairy products. Background Technology
[0002] 1,3-Diunsaturated fatty acid-2-palmitoylglycerols (UPUs) are a class of functional lipids with a natural breast milk structure and are important nutrients in breast milk and infant formula. UPUs have an unsaturated fatty acid (U) linked to the sn-1 and sn-3 positions of their glycerol backbone, and palmitic acid (P) linked to the sn-2 position. The main types include: 1,3-dioleoyl-2-palmitoylglycerol (OPO), 1-oleic-2-palmitoyl-3-linoleic acid triglyceride (OPL), and 1,3-dilinoleic-2-palmitoylglycerol (LPL).
[0003] The main methods for detecting functional oils such as OPO in dairy products include gas chromatography, liquid chromatography, and liquid chromatography-mass spectrometry. Before these methods, dairy products require pretreatment, which generally includes total lipid extraction, separation of functional oils such as OPO, and removal of interfering substances. In the laboratory, manual extraction of total lipids and separation of functional oils such as OPO require multiple extraction and separation steps, each requiring manual control. Removing interfering substances requires manual loading, washing, and elution of the forward SPE column. These manual steps result in long processing times and low efficiency, making them unsuitable for processing large batches of samples. Manual reagent addition and time control also lead to insufficient accuracy. Furthermore, most manually added reagents are organic, posing safety and health risks to laboratory personnel.
[0004] Therefore, there is an urgent need for an automated pre-processing device to solve the problems faced in the above-mentioned dairy product pre-processing process. Utility Model Content
[0005] To address the challenges of existing technologies, this invention provides a pretreatment device for detecting functional oils such as OPO in dairy products. The pretreatment device includes an oil extraction module and a reagent loading module. The oil extraction module comprises a total lipid extraction device, a functional oil separation device, an intermediate sample storage device, and a solid-phase extraction device, all connected by piping assemblies equipped with valves. The reagent loading module includes an autosampler and a reagent storage device; the autosampler draws reagents and adds them to the functional oil separation device or the solid-phase extraction device. This invention enables fully automated extraction of total lipids, separation of functional oils such as OPO, and removal of interfering substances from dairy products, solving the problems of complex, time-consuming, inaccurate, and unsafe manual pretreatment of samples for detecting functional oils such as OPO in dairy products.
[0006] This utility model provides a pretreatment device for detecting functional oils such as OPO in dairy products, including an oil extraction module and a reagent loading module; the oil extraction module includes a total lipid extraction device, a functional oil separation device, an intermediate sample storage device, and a solid-phase extraction device; the reagent loading module includes an autosampler and a reagent storage device.
[0007] Typically, sample pretreatment is required before using chromatographic analysis methods (such as gas chromatography and liquid chromatography) to detect functional oils like OPO in dairy products. The purpose of pretreatment is to separate OPO and other functional oils from the sample. This pretreatment process includes total lipid extraction, separation of OPO and other functional oils, and removal of interfering substances. These operations usually require manual intervention, which leads to long processing times, low efficiency, and is unsuitable for processing large batches of samples. Manual addition of reagents and manual time control also result in insufficient accuracy. Furthermore, most manually added reagents are organic, posing safety and health risks to laboratory personnel. The pretreatment device provided by this invention solves the above problems. This device integrates total lipid extraction, separation of OPO and other functional oils, and removal of interfering substances into a single, fully automated process, offering high efficiency, high accuracy, and high safety.
[0008] Furthermore, the bottom of the total fat extraction device is connected to the functional oil separation device via a first pipeline assembly, and the first pipeline assembly is equipped with a first valve.
[0009] Furthermore, the total lipid extraction device is equipped with a first stirrer.
[0010] The total lipid extraction device is used to extract total lipids from dairy products. Dairy products and an extractant (such as a chloroform-methanol mixed solvent) are added to the total lipid extraction device. After stirring by the first stirrer and standing, the solvent separates into layers. The lower chloroform solution contains the extracted total lipids. At this time, the first valve is opened, and the lower chloroform solution enters the functional oil separation device.
[0011] Furthermore, the bottom of the functional oil separation device is connected to the intermediate sample storage device via a second pipeline assembly. The second pipeline assembly includes a sample input pipe and a waste liquid pipe. The sample input pipe is equipped with a second valve, and the waste liquid pipe is equipped with a third valve.
[0012] Furthermore, the functional oil separation device is also equipped with a first sample inlet tube and a second stirrer.
[0013] Furthermore, the functional grease separator is also equipped with a temperature control system and a filtration device.
[0014] After the chloroform solution enters the functional oil separation device, the autosampler draws the separation reagent (such as urea-methanol solution) and adds it to the first injection tube. Once the separation reagent enters the functional oil separation device, the second stirrer starts low-temperature, low-speed stirring. After standing, the liquid separates into layers. The second valve opens, and the filtrate from the lower layer enters the intermediate sample storage device through the sample input tube. The second valve closes, and the third valve opens, allowing the upper layer liquid to drain through the waste liquid tube. Urea can form inclusion complexes with unsaturated fatty acids. The difference in the ability of different fatty acids to form inclusion complexes with urea is used to separate lipids. The lower layer is chloroform, and the upper layer is urea-methanol solution. Functional oils such as OPO are in the lower layer.
[0015] Furthermore, the bottom of the intermediate sample storage device is connected to the solid phase extraction device via a third pipeline assembly, and the third pipeline assembly is equipped with a fourth valve.
[0016] Intermediate samples before solid-phase extraction are temporarily stored in an intermediate sample storage device.
[0017] Furthermore, the third pipeline assembly is also connected to the second injection tube.
[0018] The solid-phase extraction device is a normal-phase SPE column filled with silica gel to remove interfering substances such as proteins, sugars, and phospholipids from the sample, thereby improving detection sensitivity.
[0019] Furthermore, the solid-phase extraction device is provided with a sample outlet at the bottom, and the liquid discharged from the sample outlet is collected through a sample collection bottle.
[0020] First, the autosampler draws an activation solution (such as n-hexane) and adds it to the second injection tube to activate the normal-phase SPE column. Then, the fourth valve opens, and the intermediate sample enters the solid-phase extraction device. Functional oils such as OPO are adsorbed onto the silica gel column. After loading, the autosampler draws a washing solution (such as n-hexane) and adds it to the second injection tube to wash the normal-phase SPE column. Finally, the autosampler draws different eluents (such as a hexane-dichloromethane mixture or a dichloromethane-methanol mixture) and adds them to the second injection tube to perform gradient elution of the OPO and other functional oils adsorbed on the normal-phase SPE column. The eluent is collected from the sample outlet. The eluent can be further concentrated using nitrogen blowing.
[0021] Furthermore, the autosampler includes an injection device, a robotic arm, and a base; the reagent storage device includes multiple reagent storage bottles; the injection device draws reagent from the reagent storage bottles and adds it to a first injection tube or a second injection tube.
[0022] Compared to manual reagent addition, the automated sampler offers higher precision and less error. Furthermore, the automated sampler prevents the lab technician from directly contacting organic reagents, increasing the technician's safety.
[0023] The reagent storage bottle is pre-filled with the separation reagent, activation solution, washing solution and elution solution used in the operation of the pretreatment device.
[0024] Furthermore, the total lipid extraction device is equipped with a top cover.
[0025] Open the top cover of the total fat extraction device and add the dairy products and extraction agent.
[0026] This utility model has the following beneficial effects:
[0027] 1. The pretreatment device provided by this utility model is specifically used for the extraction of functional oils such as OPO from dairy products, integrating total lipid extraction, separation of functional oils such as OPO and removal of interfering substances;
[0028] 2. The pretreatment device solves the problems of long processing time, low efficiency and unsuitability for large-scale sample processing in manual dairy product pretreatment. The whole process is fully automated, with high efficiency and high precision.
[0029] 3. The pretreatment device reduces the contact between the experimenter and the reagents, improving safety and reducing the risk factor. Attached Figure Description
[0030] Figure 1 This is a schematic diagram of the overall structure of the pretreatment device;
[0031] Figure 2 This is a schematic diagram of the total lipid extraction device and the functional oil separation device;
[0032] Figure 3 This is a schematic diagram of the internal structure of the total lipid extraction device;
[0033] Figure 4 This is a schematic diagram of the functional oil separation device and intermediate sample storage device.
[0034] Figure 5 This is a schematic diagram of the internal structure of a functional grease separator;
[0035] Figure 6 This is a schematic diagram of the intermediate sample storage device and the solid-phase extraction device.
[0036] Figure 7 This is a schematic diagram of the automatic sampler and reagent storage device. Detailed Implementation
[0037] The present invention will be further described in detail below with reference to the accompanying drawings and embodiments. It should be noted that the embodiments described below are intended to facilitate the understanding of the present invention and do not constitute any limitation thereof.
[0038] like Figure 1The image shows a pretreatment device for detecting functional oils such as OPO in dairy products. It includes an oil extraction module and a reagent loading module. The oil extraction module is used to extract functional oils such as OPO from dairy products. Before using chromatographic analysis methods (such as gas chromatography, liquid chromatography, etc.) to detect functional oils such as OPO in dairy products, sample pretreatment is required. The purpose of pretreatment is to separate functional oils such as OPO from the sample. The oil extraction module includes a total lipid extraction device 1, a functional oil separation device 2, an intermediate sample storage device 3, and a solid-phase extraction device 4; the reagent loading module includes an autosampler 5 and a reagent storage device 6.
[0039] like Figure 2-3 As shown, the bottom of the total lipid extraction device 1 is connected to the functional lipid separation device 2 via a first pipeline assembly 7, and the first pipeline assembly 7 is equipped with a first valve 8. The total lipid extraction device 1 is also equipped with a top cover 9, and a first stirrer 10 is installed inside it. The total lipid extraction device 1 is used to extract total lipids from dairy products. The top cover 9 is opened, and dairy products and an extractant (such as a chloroform-methanol mixed solvent) are added to the total lipid extraction device 1. The first stirrer 10 starts stirring. After standing, the solvent separates into layers. The lower chloroform solution contains the extracted total lipids. At this time, the first valve 8 is opened, and the lower chloroform solution enters the functional lipid separation device 2.
[0040] like Figure 4-5 As shown, the bottom of the functional oil separation device 2 is connected to the intermediate sample storage device 3 via a second pipeline assembly 11. The second pipeline assembly 11 includes a sample input pipe 12 and a waste liquid pipe 13. The sample input pipe 12 is equipped with a second valve 14, and the waste liquid pipe 13 is equipped with a third valve 15. The functional oil separation device 2 is also equipped with a first sample inlet pipe 16, which contains a second stirrer 17, a filter device, and a temperature control system. After the chloroform solution containing total lipids enters the functional oil separation device 2, the autosampler 5 draws the separation reagent (such as urea-methanol solution) and adds it to the first sample inlet pipe 16. After the urea-methanol solution enters the functional oil separation device 2, the second stirrer 17 starts stirring at a low temperature and low speed. After standing, the liquid separates into layers. The second valve 14 opens, and the filtrate of the lower layer liquid, after being filtered by the filter device, enters the intermediate sample storage device 3 through the sample input pipe 12. The second valve 14 closes, the third valve 15 opens, and the upper layer liquid is discharged through the waste liquid pipe 13. Urea can form inclusion complexes with unsaturated fatty acids. Lipids are separated by utilizing the difference in the ability of different fatty acids to form inclusion complexes with urea. The lower liquid is chloroform, and the upper liquid is a urea-methanol solution. Functional oils such as OPO are in the lower liquid.
[0041] like Figure 6As shown, the intermediate sample is temporarily stored in the intermediate sample storage device 3 before solid-phase extraction (SPE). The bottom of the intermediate sample storage device 3 is connected to the solid-phase extraction device 4 via a third pipeline assembly 18. The third pipeline assembly 18 is equipped with a fourth valve 19 and is also connected to a second sample inlet tube 20. The solid-phase extraction device 4 has a sample outlet 21 at its bottom, and the liquid discharged from the sample outlet 21 is collected through a sample collection bottle 22. The solid-phase extraction device 4 is a normal-phase SPE column, and its packing material is silica gel, which is used to remove interfering substances such as proteins, sugars, and phospholipids from the sample to improve detection sensitivity. During solid-phase extraction (SPE), firstly, the autosampler 5 draws an activation solution (such as n-hexane) and adds it to the second injection tube 20 to activate the normal-phase SPE column. Then, the fourth valve 19 is opened, and the intermediate sample enters the SPE device 4. Functional oils such as OPO are adsorbed onto the silica gel column. After loading, the autosampler 5 draws a washing solution (such as n-hexane) and adds it to the second injection tube 20 to wash the normal-phase SPE column. Finally, the autosampler 5 draws different eluents (such as a hexane-dichloromethane mixture or a dichloromethane-methanol mixture) and adds them to the second injection tube 20 to perform gradient elution of the OPO and other functional oils adsorbed on the normal-phase SPE column. A new sample vial 22 is then replaced, and the different eluents are collected from the sample outlet 21. After subsequent nitrogen blowing concentration and other steps, the eluents can be used for chromatographic analysis.
[0042] like Figure 7 As shown, the autosampler 5 includes an injection device 23, a robotic arm 24, and a base 25. The reagent storage device 6 includes multiple reagent storage bottles 26 for storing reagents used during the operation of the pretreatment device. The injection device 23 draws reagents from the reagent storage bottles 26 and adds them to the first injection tube 16 or the second injection tube 20.
[0043] Taking milk powder as an example, the pretreatment process of milk powder using this invention is as follows:
[0044] 1. Add reagents, including separation reagent, activation solution, washing solution, and elution solution, to reagent storage bottle 26 in advance;
[0045] 2. Open the top cover 9, add the milk powder and extractant that have been dissolved in water to the total lipid extraction device 1, stir with the first stirrer 10, let stand, the liquid separates into layers, open the first valve 8, and the lower layer solution enters the functional oil separation device 2.
[0046] 3. The autosampler 5 draws the separation reagent into the first injection tube 16, and the second stirrer 17 starts stirring at low temperature and low speed. After standing, the liquid separates into layers. The second valve 14 is opened, and the filtrate after the lower layer of liquid is filtered by the filter device enters the intermediate sample storage device 3 through the sample input tube 12. The second valve 14 is closed, the third valve 15 is opened, and the upper layer of liquid is discharged through the waste liquid tube 13.
[0047] 4. The autosampler 5 draws the activation solution and adds it to the second injection tube 20 to activate the normal phase SPE column. The fourth valve 19 is opened, and the intermediate sample enters the solid phase extraction device 4. Functional oils such as OPO are adsorbed on the silica gel column. After the sample loading is completed, the autosampler 5 draws the washing solution and adds it to the second injection tube 20 to wash the normal phase SPE column. Finally, the autosampler 5 draws different eluents and adds them to the second injection tube 20 to perform gradient elution of the functional oils such as OPO adsorbed on the normal phase SPE column. A new sample bottle 22 is replaced, and the eluent is collected from the sample outlet 21.
[0048] The pretreatment device provided by this utility model integrates total lipid extraction, OPO and other functions for oil separation and removal of interfering substances. The whole process is fully automated, with high efficiency, high precision and high safety.
[0049] While the present invention has been disclosed above, it is not limited thereto. Any person skilled in the art can make various modifications and alterations without departing from the spirit and scope of the present invention; therefore, the scope of protection of the present invention should be determined by the scope defined in the claims.
Claims
1. A pretreatment device for detecting OPO functional oil in a dairy product, characterized by, It includes an oil extraction module and a reagent addition module; the oil extraction module includes a total lipid extraction device (1), a functional oil separation device (2), an intermediate sample storage device (3), and a solid phase extraction device (4); the reagent addition module includes an autosampler (5) and a reagent storage device (6). The bottom of the total lipid extraction device (1) is connected to the functional oil separation device (2) via a first pipeline assembly (7); the total lipid extraction device (1) is equipped with a first stirrer (10); the bottom of the functional oil separation device (2) is connected to the intermediate sample storage device (3) via a second pipeline assembly (11); the functional oil separation device (2) is also equipped with a first injection tube (16) and a second stirrer (17); the bottom of the intermediate sample storage device (3) is connected to the solid phase extraction device (4) via a third pipeline assembly (18); the third pipeline assembly (18) is also connected to a second injection tube (20). The autosampler (5) includes an injection device (23), a robotic arm (24), and a base (25); the reagent storage device (6) includes multiple reagent storage bottles (26); the injection device (23) draws reagents from the reagent storage bottles (26) and adds them to the first injection tube (16) or the second injection tube (20).
2. The pre-treatment device of claim 1, wherein The first pipeline assembly (7) is equipped with a first valve (8).
3. The pre-treatment device of claim 2, wherein The second pipeline assembly (11) includes a sample input pipe (12) and a waste liquid pipe (13), wherein the sample input pipe (12) is provided with a second valve (14) and the waste liquid pipe (13) is provided with a third valve (15).
4. The pretreatment apparatus as described in claim 3, characterized in that, The third piping assembly (18) is equipped with a fourth valve (19).
5. The pretreatment apparatus as described in claim 4, characterized in that, The solid phase extraction device (4) is provided with a sample outlet (21) at the bottom, and the liquid discharged from the sample outlet (21) is collected through a sample collection bottle (22).
6. The pretreatment apparatus as described in claim 5, characterized in that, The total lipid extraction device (1) is equipped with a top cover (9).