CN108680674B - Method for detecting special migration amount of 5-ethylidene-2-norbornene in food contact material - Google Patents
Method for detecting special migration amount of 5-ethylidene-2-norbornene in food contact material Download PDFInfo
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- CN108680674B CN108680674B CN201810488654.1A CN201810488654A CN108680674B CN 108680674 B CN108680674 B CN 108680674B CN 201810488654 A CN201810488654 A CN 201810488654A CN 108680674 B CN108680674 B CN 108680674B
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Abstract
The invention discloses a method for detecting the special migration amount of 5-ethylidene-2-norbornene in a food contact material, which comprises the following steps: sampling; pretreating and detecting the special migration amount of the 5-ethylidene-2-norbornene in the pretreated target object; wherein the pretreatment step comprises: mixing a sample with a simulation solution preheated to a first specified temperature to form a mixed solution and sealing; and standing the sealed mixed solution at a first specified temperature for a specified time. The method for detecting the special migration amount of the 5-ethylidene-2-norbornene in the food contact material has the advantages of low detection limit which is far lower than the national standard requirement (0.05mg/kg), accurate detection, simple operation, easy acquisition of used equipment, low cost and high popularization.
Description
Technical Field
The invention relates to the field of detection, in particular to a method for detecting the special migration amount of 5-ethylidene-2-norbornene in a food contact material.
Background
In recent years, as people have been concerned about food safety, food packaging materials have been paid much attention to their safety. Food contact materials and products may affect the flavor, taste and color of food during contact with food, and may release certain amounts of toxic chemicals such as heavy metals, toxic additives, which may migrate into food and be ingested by the human body and be harmful to human health. The safety of the food packaging material is also quite important in our country, a complete set of relevant laws and regulations and test standards are updated and released in 2016, and the safety quality requirements and test guidance of the food packaging material are standardized. Plastic products are one of the most common materials widely used for food packaging since the 60 th of the 20 th century, but due to monomer residues in the synthesis process of high molecular materials and relatively low molecular additives added in the forming process, unsatisfactory plastic materials can leave toxic and harmful monomers or migrate out so as to change certain characteristics of food or cause harm to human bodies. The technology fills the blank of a national standard method, and in GB 4806.6-2016 national food safety standard, the requirement of PP polymer materials in plastic resins for food contact for food packaging materials indicates that the limit value of the migration quantity of the 5-ethylidene-2-norbornene of the materials is 0.05mg/kg, and no official method for detecting the substances is established in the country and related industries.
At present, only related methods for detecting the content of the 5-ethylidene-2-norbornene monomer in the plastic product by adopting infrared and nuclear magnetic resonance methods exist, but the methods are not mature enough and detection instruments are expensive, and a method for detecting the content in the plastic by using a gas chromatography method exists, but the method cannot test the migration volume.
Disclosure of Invention
The invention mainly aims to provide a method for detecting the special migration quantity of 5-ethylidene-2-norbornene in a food contact material, so as to solve at least one problem in the background technology.
The invention provides a method for detecting the special migration amount of 5-ethylidene-2-norbornene in a food contact material, which comprises the following steps: sampling; pretreating and detecting the special migration amount of the 5-ethylidene-2-norbornene in the pretreated target object;
wherein the pretreatment step comprises:
mixing a sample with a simulation solution preheated to a first specified temperature to form a mixed solution and sealing;
and standing the sealed mixed solution at a first specified temperature for a specified time.
Further, the method for detecting the specific migration amount of 5-ethylidene-2-norbornene in the food contact material, after the step of standing the sealed mixed solution at the first specified temperature for the specified time, further comprises:
cooling the mixture to a second designated temperature.
Further, the method for detecting the specific migration amount of 5-ethylidene-2-norbornene in the food contact material comprises the following sampling steps:
the sample was cut to a specified size and then sampled.
Further, the method for detecting the specific migration amount of 5-ethylidene-2-norbornene in the food contact material, wherein the step of detecting the specific migration amount of 5-ethylidene-2-norbornene in the pretreated target substance, comprises:
and detecting the special migration amount of the 5-ethylidene-2-norbornene in the pretreated target substance by using a GC-MS analyzer.
Further, in the method for detecting the specific migration amount of 5-ethylidene-2-norbornene in the food contact material, the headspace conditions of the GC-MS analyzer are as follows: the balance time is 20-45 min; the furnace temperature is 50-100 ℃; pressurizing for 1-5 min; the temperature of the sample injection needle is 90-130 ℃; the temperature of the transmission line is 90-140 ℃.
Further, in the method for detecting the specific migration amount of 5-ethylidene-2-norbornene in the food contact material, the temperature rise curve of the GC-MS analyzer is set as follows:
maintaining the column temperature at 60 deg.C for 2 min;
raising the temperature of the chromatographic column to 150 ℃ at a temperature rise speed of 10 ℃/min;
the column temperature was raised to 220 ℃ at a ramp rate of 30 ℃/min.
Further, in the method for detecting the special migration amount of the 5-ethylidene-2-norbornene in the food contact material, the sample inlet temperature of the GC-MS analyzer is 180 ℃.
Further, in the method for detecting the special migration amount of the 5-ethylidene-2-norbornene in the food contact material, the simulation liquid comprises any one of 10% -98% of ethanol, acetic acid and isooctane.
Further, in the method for detecting a specific migration amount of 5-ethylidene-2-norbornene in the food contact material, the ratio of the area of the sample to the volume of the simulant is 3cm2:4-6 mL.
Further, in the method for detecting the specific migration amount of 5-ethylidene-2-norbornene in the food contact material, the first specified temperature includes 30 ℃ to 90 ℃.
The method for detecting the special migration amount of the 5-ethylidene-2-norbornene in the food contact material has the advantages of low detection limit which is far lower than the national standard requirement (0.05mg/kg), accurate detection, simple operation, easy acquisition of used equipment, low cost and high popularization.
Drawings
FIG. 1 is a schematic flow chart showing a method for detecting a specific migration amount of 5-ethylidene-2-norbornene in a food contact material according to an embodiment of the present invention;
FIG. 2 is a schematic flow chart showing a method for detecting a specific migration amount of 5-ethylidene-2-norbornene in a food contact material according to an embodiment of the present invention;
FIG. 3 is a schematic diagram showing the linear correlation coefficient of the method for detecting the specific migration amount of 5-ethylidene-2-norbornene in the food contact material according to one embodiment of the present invention;
FIG. 4 is a schematic diagram showing the detection limit of a target substance in the method for detecting a specific migration amount of 5-ethylidene-2-norbornene in a food contact material according to an embodiment of the present invention;
FIG. 5 is a schematic gas chromatography diagram of a target substance in the method for detecting a specific migration amount of 5-ethylidene-2-norbornene in a food contact material according to an embodiment of the present invention.
The implementation, functional features and advantages of the objects of the present invention will be further explained with reference to the accompanying drawings.
Detailed Description
The technical solutions in the embodiments of the present invention will be clearly and completely described below with reference to the drawings in the embodiments of the present invention, and it is obvious that the described embodiments are only a part of the embodiments of the present invention, and not all of the embodiments. All other embodiments, which can be derived by a person skilled in the art from the embodiments given herein without making any creative effort, shall fall within the protection scope of the present invention.
In addition, the descriptions related to "first", "second", etc. in the present invention are for descriptive purposes only and are not to be construed as indicating or implying relative importance or implicitly indicating the number of technical features indicated. Thus, a feature defined as "first" or "second" may explicitly or implicitly include at least one such feature. In addition, the technical solutions of the respective embodiments may be combined with each other, but must be realized by those skilled in the art, and when the technical solutions are contradictory or cannot be realized, such a combination should not be considered to exist, and is not within the protection scope of the present invention.
Referring to fig. 1, in an embodiment of the present invention, the present invention provides a method for detecting a specific migration amount of 5-ethylidene-2-norbornene in a food contact material, including: s1, sampling; s2, preprocessing and S3, detecting the special migration amount of the 5-ethylidene-2-norbornene in the preprocessed target object,
wherein the pretreatment step comprises: s21, mixing the sample with a simulation solution preheated to a first specified temperature to form a mixed solution and sealing; and S22, standing the sealed mixed solution at the first specified temperature for a specified time at a constant temperature.
As mentioned in step S1, sampling is generally one of the important steps for extracting a small amount of target substance from a target object for detection, and has one of the effective ways to obtain various data from the target object under the condition of not affecting the main properties of the target object, the extraction amount of the target object is sufficient for 3-5 times of tests, the sampling requires randomness in the selection process of the sampling region of the target object, and subjective selection cannot be mixed in the selection process, in the embodiment of the present invention, the sampling area is generally 40-80cm2Preferably 40cm2、60cm2Or 80cm2。
As the step S2, the pretreatment is generally a step for the purpose of impurity removal and purification before performing an effective process on the target object, and in some special experiments, the pretreatment step also includes the purpose of changing the material property, and in the embodiment of the present invention, the pretreatment step is preferably the steps S21-S23.
As the step S3, detecting the specific migration amount of 5-ethylidene-2-norbornene in the pretreated target object, generally performing a specified experiment or detection step on the target object after the steps S1-S2, and generally obtaining direct data or indirect data, wherein the direct data is data of the target object value or result; the indirect data is data of a target value or result obtained only after corresponding calculation, replacement or comparison, the detection result generally has a deviation value according to the deviation of detection equipment, environment, preprocessing steps and auxiliary products, and after the difference between the preprocessing step and the auxiliary products is used for formulating a detection standard, the error amplitude caused by the preprocessing step and the auxiliary products can be correspondingly and effectively avoided.
In the step S21, the sample is mixed with the simulant preheated to the first predetermined temperature to form a mixture and sealed, and in the process of performing the step S21, the first predetermined temperature is generally 30 ℃ to 90 ℃, and in the embodiment of the present invention, preferably 30 ℃, 70 ℃ or 90 ℃, the sample and the simulant are mixed to such an extent that the sample and the simulant are in contact with each other in the same reactor, and after the sample and the extractant are mixed, the container is sealed, and since the container has a high temperature and the simulant is generally a volatile substance with a low boiling point, for example: ethanol, acetic acid, etc., and therefore, a material having elasticity or ductility is generally used for sealing to prevent bursting due to excessive pressure inside the container, and is generally a wrap film or an elastic plastic film.
And (3) allowing the sealed mixture to stand at the constant temperature for a predetermined time at the first predetermined temperature in the step S22, wherein the temperature in the reaction apparatus is maintained at the first predetermined temperature during the step S22, wherein the first predetermined temperature is generally 30 ℃ to 90 ℃, preferably 30 ℃, 70 ℃ or 90 ℃ in the embodiment of the present invention, and the standing time is generally 20 to 50min, preferably 20min, 30min or 50 min.
Referring to fig. 2, in this embodiment, the method for detecting the specific migration amount of 5-ethylidene-2-norbornene in the food contact material further comprises, after the step of allowing the sealed mixed solution to stand at a constant temperature for a predetermined time at a first predetermined temperature: s23, cooling the mixed liquid to a second designated temperature.
In the step S23, the mixed solution is cooled to a second predetermined temperature, and in the step S23, the mixed solution obtained in the step S21 is shaken for a predetermined time, wherein the predetermined time is generally 20 to 50min, preferably 20min, 30min or 50min, and the temperature in the reaction apparatus is maintained at the second predetermined temperature during the step S24, wherein the second predetermined temperature is generally 20 to 50 ℃, and in the present embodiment, preferably 20 ℃, 25 ℃, 27 ℃ or 50 ℃.
Referring to fig. 2, in this embodiment, the method for detecting the specific migration amount of 5-ethylidene-2-norbornene in the food contact material comprises the following steps: and S11, cutting the sample to a specified size and then sampling.
As in step S11, the sample is cut to a predetermined size and sampled, typically 40-80cm2Preferably 40cm2、60cm2Or 80cm2。
In this embodiment, in the method for detecting a specific migration amount of 5-ethylidene-2-norbornene in a food contact material, and in the step for detecting a specific migration amount of 5-ethylidene-2-norbornene in a pretreated target, a GC-MS (gas chromatography-mass spectrometry) analyzer is used for detection, in this embodiment, GC135 is preferably used, wherein in the detection process, the conditions of the GC-MS analyzer are preferably as follows:
headspace conditions equilibration time: 30 min;
furnace temperature: 80 ℃;
pressurizing time: 2 min;
temperature of the sample injection needle: 110 ℃;
transmission line temperature: 120 ℃;
column: DB-VRX;
sample inlet temperature: 180 ℃;
shunting mode: no split flow;
temperature program: initially: maintaining at 60 deg.C for 2 min;
temperature rise stage 1: temperature rise rate: heating to 150 ℃ at a speed of 10 ℃/min;
a temperature rise stage 2: temperature rise rate: heating to 220 ℃ at a temperature of 30 ℃/min.
In this example, in the method for detecting the specific migration amount of 5-ethylidene-2-norbornene in the food contact material, the simulant is any one of 10% to 98% ethanol, acetic acid and isooctane, and in the inventive example, 10% ethanol, 50% ethanol, 95% ethanol, 4% acetic acid or isooctane is preferably used.
In this example, in the method for detecting the specific migration amount of 5-ethylidene-2-norbornene in the food contact material, the ratio of the area of the sample to the volume of the simulant was 3cm24-6mL, wherein, in the invention embodiment, the volume ratio of the sample area to the simulated liquid is preferably 3cm2:4mL、3cm25mL or 3cm2:6mL。
In this embodiment, the first prescribed temperature includes 30 ℃ to 90 ℃ and in the embodiment of the present invention, it is preferable to be 30 ℃, 70 ℃ or 90 ℃ in the method for detecting the specific migration amount of 5-ethylidene-2-norbornene in the food contact material.
Referring to fig. 3-5, in an embodiment, 100uL of 1000mg/L standard solution is transferred to 5 10mL volumetric flasks and the volume is determined by using the simulation solution, in this embodiment, the simulation solution is 5 in total, and is 10% ethanol, 50% ethanol, 95% ethanol, 4% acetic acid or isooctane, each volumetric flask is determined by using different simulation solutions, and the volume is determined and then filtered, and the theoretical value of the concentration of the target in the solution after the scaling is 10 mg/L. And finally, calculating the standard recovery rate and the lowest detection limit of the 5-ethylidene-2-norbornene in each sample according to the test result, wherein the test result is as follows:
table 1 recovery of 5-ethylidene-2-norbornene measured using the method of the present invention, instrumental test conditions:
headspace conditions equilibration time: 30 min;
furnace temperature: 80 ℃;
pressurizing time: 2 min;
temperature of the sample injection needle: 110 ℃;
transmission line temperature: 120 ℃;
column: DB-VRX;
sample inlet temperature: 180 ℃;
shunting mode: no split flow;
temperature program: initially: maintaining at 60 deg.C for 2 min;
temperature rise stage 1: temperature rise rate: heating to 150 ℃ at a speed of 10 ℃/min;
the main technical parameters are as follows: linear range: the linear range was 0mg/L, 1mg/L, 2mg/L, 5mg/L, 10mg/L, 20 mg/L. The linear correlation coefficient is shown in fig. 3.
Wherein the test recovery is shown in table 1:
| simulated liquid | 10 |
50% ethanol | 95% ethanol | 4% acetic acid | Isooctane |
| Recovery (%) | 92 | 90 | 90 | 91 | 91 |
TABLE 1
The lowest detection limit of 5-ethylidene-2-norbornene measured using the method of the present invention: 0.01 mg/L.
The method for detecting the special migration amount of the 5-ethylidene-2-norbornene in the food contact material has the advantages of low detection limit which is far lower than the national standard requirement (0.05mg/kg), accurate detection, simple operation, easy acquisition of used equipment, low cost and high popularization.
The above description is only a preferred embodiment of the present invention, and not intended to limit the scope of the present invention, and all modifications of equivalent structures and equivalent processes, which are made by using the contents of the present specification and the accompanying drawings, or directly or indirectly applied to other related technical fields, are included in the scope of the present invention.
Claims (3)
1. A method for detecting the special migration amount of 5-ethylidene-2-norbornene in a food contact material is characterized by comprising the following steps: sampling; pretreating and detecting the special migration amount of the 5-ethylidene-2-norbornene in the pretreated target object;
wherein the pretreatment step comprises:
mixing a sample with a simulated liquid preheated to 30-90 ℃ to form a mixed liquid and sealing; wherein the ratio of the area of the sample to the volume of the simulant comprises 3cm2:4-6mL；
Standing the sealed mixed solution at constant temperature of 30-90 ℃ for 20-50 min;
cooling the mixed solution to 20-27 ℃;
wherein the step of detecting the special migration amount of the 5-ethylidene-2-norbornene in the pretreated target object comprises the following steps: detecting the special migration amount of the 5-ethylidene-2-norbornene in the pretreated target object by using a GC-MS analyzer;
specifically, the detection conditions of the GC-MS analyzer comprise:
the balance time is as follows: 30 min; furnace temperature: 80 ℃; pressurizing time: 2 min; temperature of the sample injection needle: 110 ℃; transmission line temperature: 120 ℃; column: DB-VRX; sample inlet temperature: 180 ℃; shunting mode: no split flow;
temperature program: initially: maintaining at 60 deg.C for 2 min;
temperature rise stage 1: temperature rise rate: heating to 150 ℃ at a speed of 10 ℃/min;
a temperature rise stage 2: temperature rise rate: heating to 220 ℃ at a speed of 30 ℃/min;
the main technical parameters are as follows: linear range: the linear range was 0mg/L, 1mg/L, 2mg/L, 5mg/L, 10mg/L, 20 mg/L.
2. The method of claim 1, wherein the sampling step comprises:
the sample was cut to a specified size and then sampled.
3. The method for detecting the specific migration amount of 5-ethylidene-2-norbornene in the food contact material according to claim 1, wherein the simulated liquid comprises any one of acetic acid, isooctane and ethanol with a volume ratio of 10% -98%.
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| DE69706287T2 (en) * | 1996-03-07 | 2002-05-16 | Cryovac Inc | ZEOLITE IN A PACKAGING FILM |
| JP2007518863A (en) * | 2004-01-19 | 2007-07-12 | ディーエスエム アイピー アセッツ ビー．ブイ． | Thermoplastic elastomer composition |
| JP4694474B2 (en) * | 2004-03-03 | 2011-06-08 | 三菱化学メディエンス株式会社 | Method for testing fat-soluble vitamins and / or fat-soluble food factors by saliva analysis |
| CN102879510B (en) * | 2012-09-21 | 2014-09-10 | 福建出入境检验检疫局检验检疫技术中心 | Method for detecting migration quantity of nipagin ester substances in plastic food package bag |
| CN104215732A (en) * | 2014-09-26 | 2014-12-17 | 云南中烟工业有限责任公司 | Method of taking Tenax as simulant to measure migration amount from paper and volatile and semi-volatile organic matter in paperboard by TD-GC/MS |
| CN106770805A (en) * | 2017-03-02 | 2017-05-31 | 深圳天祥质量技术服务有限公司 | The assay method of hexene migration amount in a kind of food contact plastic products |
| CN107037151B (en) * | 2017-04-13 | 2019-10-15 | 宁波出入境检验检疫局检验检疫技术中心 | A kind of measuring method of transfer volume of epoxy chloropropane in food contact material |
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