CN210626153U - Pretreatment device for N-dimethyl nitrosamine in meat products - Google Patents
Pretreatment device for N-dimethyl nitrosamine in meat products Download PDFInfo
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- CN210626153U CN210626153U CN201921105590.9U CN201921105590U CN210626153U CN 210626153 U CN210626153 U CN 210626153U CN 201921105590 U CN201921105590 U CN 201921105590U CN 210626153 U CN210626153 U CN 210626153U
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Abstract
The utility model provides a pretreatment device of N-dimethyl nitrosamine in meat products, which comprises a body, a crushing device, an adsorption device, an extraction device, a drying device, a concentration device and a magnet, wherein the crushing device is connected with the adsorption device, the adsorption device is provided with a water inlet and a dichloromethane nozzle, and the adsorption device is connected with the extraction device through a first outlet pipe and a recovery pipe to form a loop; the adsorption device is connected with the drying device through a second outlet pipe; the extraction device is respectively connected with the ultrasonic device and the waste liquid bottle; the drying device is connected with the concentrating device, and the magnet is arranged on the outer side of the adsorption device. The device of the utility model has the advantages of strong adsorption capacity and easy separation; the maximum extraction of the N-dimethyl nitrosamine is realized through the quantitative arrangement of the spraying of a dichloromethane nozzle.
Description
Technical Field
The utility model relates to a detection area of N-dimethyl nitrosamine in meat products, in particular to preceding processing apparatus of N-dimethyl nitrosamine in meat products.
Background
N-dimethyl Nitrosamine (NDMA) is a semi-volatile organic chemical, widely exists in various pickled, smoked and roasted meat products and hot processed foods, is quickly absorbed by digestive tract and respiratory tract, is slowly absorbed by skin, mainly causes liver damage and has great harm to human bodies. The national standard GB2762-2017 'limit of pollutants in national food for food safety' has a clear limit regulation on NDMA, wherein the maximum limit value of NDMA in meat products (except meat cans) is 3 mug/Kg.
At present, the detection method of N-dimethyl nitrosamine mainly comprises a gas chromatography-thermal energy analyzer method, a gas chromatography-mass spectrometry method, a gas chromatography-tandem mass spectrometry method and the like, while the pretreatment method of N-dimethyl nitrosamine in food mainly comprises a steam distillation method, a solvent extraction method, a vacuum distillation method, a solid phase extraction method and the like, and the traditional extraction method has the defects of complex operation, large consumption of organic solvent, large sample amount, unstable recovery rate, inconvenience for batch treatment and the like; meanwhile, the meat product has high oil content, complex matrix and low content of target substances, and the improvement of the pretreatment of the sample is still the key for the research of the N-nitrosamine detection method.
Therefore, how to simplify the pretreatment device, avoid the loss of the sample amount caused by complicated treatment steps, achieve the purpose of stable recovery rate, and ensure that the content of the detection result is consistent with that of the actual sample becomes the important factor in the current research.
Disclosure of Invention
An object of the utility model is to overcome the technical problem that exists among the prior art, provide a preceding processing apparatus of N-dimethyl nitrosamine among meat products to realize simplifying the pretreatment step, realize the unanimous effect of the content of the stable, testing result of rate of recovery and actual sample.
In order to achieve the above object, the utility model provides a following technical scheme: a pretreatment device for N-dimethyl nitrosamine in meat products comprises a body, a crushing device, an adsorption device, an extraction device, a drying device and a concentration device, wherein the crushing device is connected with the adsorption device, the adsorption device is provided with a water inlet and a dichloromethane nozzle and is connected with the extraction device through a first outlet pipe and a recovery pipe to form a loop; the adsorption device is connected with the drying device through a second outlet pipe; the extraction device is respectively connected with the ultrasonic device and the waste liquid bottle; the drying device is connected with the concentration device, and the magnet is arranged on the outer side of the adsorption device.
Further, the concentration device is connected with a nitrogen pipe, and the aim of drying and concentration is fulfilled by blowing nitrogen;
furthermore, the adsorption device contains a porous magnetic adsorption material which can adsorb N-dimethyl nitrosamine in meat products; the porous magnetic adsorption material is preferably porous magnetic activated carbon, porous magnetic zeolite or porous magnetic hydroxyapatite;
further, the adsorption device is provided with a stirring device;
further, glass wool is arranged at the bottom of the drying device, and a drying substance is arranged above the glass wool, wherein the drying substance is preferably anhydrous sodium sulfate;
further, the first outlet tube and the second outlet tube are not open at the same time;
furthermore, the magnet is an electromagnet and can control the switch of the magnetic field.
The utility model discloses following beneficial effect has:
(1) the N-dimethyl nitrosamine in the meat product is adsorbed by applying the porous magnetic adsorption material under the stirring condition, then the magnetic field is applied to gather the porous magnetic adsorption material at one side of the magnet, and the meat product enters the extraction device through the first outlet pipe, so that the extraction device has the advantages of strong adsorption capacity and easiness in separation;
(2) spraying quantitative dichloromethane through a dichloromethane nozzle to clean the adsorption device, flowing into the extraction device for further extraction relative to N-dimethyl nitrosamine in meat products, applying ultrasonic waves for a certain time in the process to promote extraction efficiency, and then returning an extract phase to the adsorption device through a recovery pipe to elute the porous magnetic adsorption material so as to resolve the adsorbed N-dimethyl nitrosamine; thereby realizing the extraction of the N-dimethyl nitrosamine to the maximum extent;
(3) the analytic solution enters a drying device through a second outlet pipe for drying, then is filtered to a concentration device through glass wool, and a nitrogen blowing drying and concentration method is used, so that the loss of N-dimethyl nitrosamine can be avoided, and the consistency of the detection result and the actual content is ensured;
(4) the utility model discloses a pretreatment step has been simplified greatly to the method, has avoided the loss of sample volume and the experimental error that leads to in loaded down with trivial details pretreatment step, simultaneously, through the detection to actual sample, discovery pretreatment technique has good specificity enrichment effect to N-dimethyl nitrosamine, has effectively kept apart the influence of impurity such as grease, moisture in the traditional meat article to the experimental result.
Drawings
FIG. 1 is a schematic structural view of a pretreatment device for N-dimethylnitrosamine in meat products of the present invention.
The device comprises a body 1, a smashing device 2, an adsorption device 3, an extraction device 4, a drying device 5, an ultrasonic device 6, a waste liquid bottle 7, a concentration device 8, a water inlet 9, a dichloromethane nozzle 10, a recovery pipe 11, a nitrogen pipe 12, glass wool 13, a magnet 14, a stirring device 15, a second outlet pipe 16 and a first outlet pipe 17.
Detailed Description
The drawings are for illustrative purposes only and are not to be construed as limiting the patent; for the purpose of better illustrating the embodiments, certain features of the drawings may be omitted, enlarged or reduced, and do not represent the size of an actual product;
it will be understood by those skilled in the art that certain well-known structures in the drawings and descriptions thereof may be omitted. The technical solution of the present invention will be further explained with reference to the accompanying drawings and examples.
Example 1
FIG. 1 is a schematic view showing the structure of a pretreatment apparatus for N-dimethylnitrosamine in meat products of the present invention, which comprises a main body 1, a pulverization apparatus 2, an adsorption apparatus 3, an extraction apparatus 4, a drying apparatus 5, and a concentration apparatus 8,
wherein, the adsorption device 3 is connected with the crushing device 2, is provided with a water inlet 9 and a dichloromethane nozzle 10 and is connected with the extraction device 4 through a first outlet pipe 17 and a recovery pipe 11 to form a loop; and the adsorption device 3 is connected with the drying device 5 through a second outlet pipe 16; meanwhile, the extraction device 4 is respectively connected with the ultrasonic device 6 and the waste liquid bottle 7; the concentration device 8 is respectively connected with the drying device 5 and the nitrogen pipe 12;
in addition, a magnet 14 is arranged on the outer side of the adsorption device 3, and a stirring device 15 and a plurality of porous magnetic adsorption materials are arranged in the adsorption device; the bottom of the drying device 5 is provided with glass wool 13, and the upper part of the glass wool 13 is provided with the anhydrous sodium sulfate of the drying substance.
In the working process, after a sample meat food to be detected is sent into the crushing device 2 to be crushed, the crushed meat food is added into the adsorption device 2, a proper amount of deionized water is added through the water inlet 9, the stirring device 15 is started, after 30min of adsorption, the magnet 14 is started to carry out adsorption separation on the porous magnetic adsorption material, and meanwhile, the first outlet pipe 17 is opened to flow the residual mixture into the extraction device 4;
spraying a proper amount of dichloromethane through a dichloromethane nozzle 10 to clean the adsorption device 3, taking the dichloromethane as an extraction medium to flow into an extraction device 4 to extract N-dimethyl nitrosamine in the residual mixture, starting an ultrasonic device 6 to apply ultrasonic waves in the extraction process, ending after 15min, and standing until layering; the lower layer water phase flows into a waste liquid bottle 7, and the extract phase returns to the adsorption device 3 through a recovery pipe 11 to analyze the porous magnetic adsorption material for 15-min;
after the analysis is finished, the magnet 14 is started to adsorb and separate the porous magnetic adsorbing material, the second outlet pipe 16 is opened to flow the liquid phase into the drying device 5, after the liquid phase is dried for 2 hours, the liquid phase is filtered through the glass wool 13 and enters the concentration device 8, and nitrogen is blown in through the nitrogen pipe 12 to be dried and concentrated, so that the liquid to be detected containing the N-dimethyl nitrosamine is obtained. The specific porous magnetic adsorption material is porous coconut shell activated carbon.
Example 2
FIG. 1 is a schematic view showing the structure of a pretreatment apparatus for N-dimethylnitrosamine in meat products of the present invention, which comprises a main body 1, a pulverization apparatus 2, an adsorption apparatus 3, an extraction apparatus 4, a drying apparatus 5, and a concentration apparatus 8,
wherein, the adsorption device 3 is connected with the crushing device 2, is provided with a water inlet 9 and a dichloromethane nozzle 10 and is connected with the extraction device 4 through a first outlet pipe 17 and a recovery pipe 11 to form a loop; and the adsorption device 3 is connected with the drying device 5 through a second outlet pipe 16; meanwhile, the extraction device 4 is respectively connected with the ultrasonic device 6 and the waste liquid bottle 7; the concentration device 8 is respectively connected with the drying device 5 and the nitrogen pipe 12;
in addition, a magnet 14 is arranged on the outer side of the adsorption device 3, and a stirring device 15 and a plurality of porous magnetic adsorption materials are arranged in the adsorption device; the bottom of the drying device 5 is provided with glass wool 13, and the upper part of the glass wool 13 is provided with the anhydrous sodium sulfate of the drying substance.
In the working process, after a sample meat food to be detected is sent into the crushing device 2 to be crushed, the crushed meat food is added into the adsorption device 2, a proper amount of deionized water is added through the water inlet 9, the stirring device 15 is started, after 60min of adsorption, the magnet 14 is started to carry out adsorption separation on the porous magnetic adsorption material, and meanwhile, the first outlet pipe 17 is opened to flow the residual mixture into the extraction device 4;
spraying a proper amount of dichloromethane through a dichloromethane nozzle 10 to clean the adsorption device 3, taking the dichloromethane as an extraction medium to flow into an extraction device 4 to extract N-dimethyl nitrosamine in the residual mixture, starting an ultrasonic device 6 to apply ultrasonic waves in the extraction process, ending after 20min, and standing until layering; the lower layer water phase flows into a waste liquid bottle 7, and the extract phase returns to the adsorption device 3 through a recovery pipe 11 to analyze the porous magnetic adsorption material for 30 min;
after the analysis is finished, the magnet 14 is started to adsorb and separate the porous magnetic adsorbing material, the second outlet pipe 16 is opened to flow the liquid phase into the drying device 5, after the liquid phase is dried for 4 hours, the liquid phase is filtered through the glass wool 13 and enters the concentration device 8, and nitrogen is blown in through the nitrogen pipe 12 to be dried and concentrated, so that the liquid to be detected containing the N-dimethyl nitrosamine is obtained. The specific porous magnetic adsorption material is porous magnetic hydroxyapatite.
It is obvious that the above embodiments of the present invention are only examples for clearly illustrating the present invention, and are not limitations to the embodiments of the present invention. Other variations and modifications will be apparent to persons skilled in the art in light of the above description. And are neither required nor exhaustive of all embodiments. Any modification, equivalent replacement, and improvement made within the spirit and principle of the present invention should be included in the protection scope of the claims of the present invention.
Claims (5)
1. A pretreatment device for N-dimethyl nitrosamine in meat products is characterized in that: the device comprises a body (1), a crushing device (2), an adsorption device (3), an extraction device (4), a drying device (5), a concentration device (8) and a magnet (14), wherein the crushing device (2) is connected with the adsorption device (3), the adsorption device (3) is provided with a water inlet (9) and a dichloromethane nozzle (10), and the adsorption device and the extraction device (4) are connected through a first outlet pipe (17) and a recovery pipe (11) to form a loop; the adsorption device (3) is connected with the drying device (5) through a second outlet pipe (16); the extraction device (4) is respectively connected with the ultrasonic device (6) and the waste liquid bottle (7); the drying device (5) is connected with the concentration device (8), and the magnet (14) is arranged on the outer side of the adsorption device (3).
2. The apparatus for pretreating N-dimethylnitrosamine in meat products as claimed in claim 1, wherein: the concentration device (8) is connected with a nitrogen pipe (12).
3. The apparatus for pretreating N-dimethylnitrosamine in meat products as claimed in claim 1, wherein: the adsorption device (3) contains a porous magnetic adsorption material and is provided with a stirring device (15).
4. The apparatus for pretreating N-dimethylnitrosamine in meat products as claimed in claim 1, wherein: and glass wool (13) is arranged at the bottom of the drying device (5).
5. The apparatus for pretreating N-dimethylnitrosamine in meat products as claimed in claim 1, wherein: the first outlet duct (17) and the second outlet duct (16) are not open at the same time.
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Address after: 524001 No. 48, Renmin South Road, Xiashan District, Guangdong, Zhanjiang Patentee after: AGRICULTURAL PRODUCT PROCESSING Research Institute CHINESE ACADEMY OF TROPICAL AGRICULTURAL SCIENCES Address before: 524001 No. 48, South Renmin Avenue, Xiashan District, Guangzhou, Guangdong Province Patentee before: AGRICULTURAL PRODUCT PROCESSING Research Institute CHINESE ACADEMY OF TROPICAL AGRICULTURAL SCIENCES |