Method for simultaneously determining migration volumes of three acrylamide compounds in food contact material and food contact product

Abstract

The invention relates to the field of detection of harmful substances in food contact materials and products, in particular to a method for simultaneously determining migration volumes of three acrylamide compounds in food contact materials and products, which comprises the following steps: S1, preparing a standard working solution, S2, preparing a food simulant, and S3, performing instrumental analysis. According to the method, the liquid chromatography-tandem mass spectrometry method is adopted for detection, the sensitivity is high, MRM ion mode collection is achieved, the anti-interference capacity is high, and the three acrylamide compounds can be measured at the same time. According to the method, the detection limits of three acrylamide compounds in water-based, acidic, ethanol-containing food simulants, grease-containing food simulants and chemical substitute solvent ethanol with the volume fraction of 95% are all 0.005 mg / kg, the quantitation limits are all 0.01 mg / kg, the recovery rate is 86.4%-98.8%, the repeatability is 2.1%-9.5%, the precision is high, and the requirements of laws and regulations are met.

Description

TECHNICAL FIELD

[0001] The present application relates to the field of food contact materials and articles harmful substance detection, and particularly relates to a method for simultaneously determining migration amounts of three kinds of acrylamide compounds in food contact materials and articles. BACKGROUND

[0002] Acrylamide is one of the main raw materials of polyacrylamide. Polyacrylamide is widely used in various food contact materials due to its excellent physical and chemical properties, such as water purification treatment, paper processing, and pipeline inner coating. However, this substance is a toxic chemical, and acrylamide is classified as a 2A carcinogen. Short-term high-concentration exposure (such as occupational exposure) may cause central and peripheral nerve damage and other problems.

[0003] Methacrylamide, also known as 2-methacrylamide, is an intermediate for the production of methyl methacrylate. Poly(methyl methacrylate) (PMMA) can be used to produce tableware due to its light weight, low cost, easy molding, and good chemical stability and weather resistance. However, this substance is a toxic chemical, has irritating effects on the eyes, skin, and mucous membranes, and has the risk of causing central nervous system disorders, which may pose a certain risk to human health.

[0004] N-(Hydroxymethyl)acrylamide (NMA) is mainly used in plastics, paper, rubber, coatings, and adhesives in food contact applications. For example, in plastics, NMA can enhance the heat resistance and mechanical strength of plastics; in paper, it can improve the water resistance and printing adaptability of paper; in rubber and coatings, NMA is used to improve the adhesion and durability. N-(Hydroxymethyl)acrylamide itself has certain toxicity, and animal experiments have shown that it may have adverse effects on the nervous system and reproductive system, such as abnormal neurological behavior and decreased reproductive ability. In addition, NMA may decompose to produce acrylamide during high-temperature processing.

[0005] The current domestic standard for the control and restriction requirements of these three substances are as follows in Table 1:

[0006]

[0007] At present, there is no domestic and foreign detection standard for simultaneously detecting the migration amount of three kinds of acrylamide compounds in food contact materials and products. The methods for detecting the three kinds of acrylamide compounds are gas chromatography mass spectrometry, liquid chromatography and liquid chromatography mass spectrometry. Since the limit requirement of migration amount in the national standard is ND (detection limit = 0.01 mg / kg), the detection limit of gas chromatography mass spectrometry cannot reach 0.01 mg / kg, and in GB 31604.18, only acrylamide has a detection method, and the method uses high performance liquid chromatography-ultraviolet detector for detection, which has low sensitivity and weak anti-interference ability. Therefore, how to develop a detection method for simultaneously determining the migration amount of three kinds of acrylamide compounds in food contact materials is an urgent problem to be solved by those skilled in the art. SUMMARY

[0008] In order to overcome the shortcomings and deficiencies in the prior art, the purpose of the present application is to provide a method for simultaneously determining the migration amount of three kinds of acrylamide compounds in food contact materials and products, which adopts liquid chromatography-tandem mass spectrometry detection, has high sensitivity, MRM ion mode collection, strong anti-interference ability, and can simultaneously determine the three kinds of acrylamide compounds.

[0009] The purpose of the present application is achieved by the following technical solutions:

[0010] A method for simultaneously determining the migration amount of three kinds of acrylamide compounds in food contact materials and products, comprising the following steps:

[0011] Step S1, configuration of standard working solution (S1.1) Configuration of standard stock solution (1000 mg / L): accurately weigh 10 mg (accurate to 0.1 mg) of three kinds of acrylamide compound standards, respectively, dissolve with methanol, transfer to a 10 mL volumetric flask, dilute to the mark, shake well, and store in a 0℃ to -4℃ refrigerator in a sealed state, with a validity period of 6 months.

[0012] (S1.2) Configuration of standard intermediate solution (10 mg / L): accurately transfer 0.10 mL of standard stock solution into a 10 mL volumetric flask, dilute to the mark with methanol, shake well, and obtain a 10 mg / L standard intermediate solution, which is prepared and used immediately.

[0013] (S1.3) Preparation of standard working solutions of water, alcoholic food simulants and chemical substitute solvents (95% ethanol): Transfer 0.005 mL, 0.01 mL, 0.02 mL, 0.04 mL, 0.06 mL, 0.08 mL and 0.10 mL of the above standard intermediate solution into seven 10 mL volumetric flasks, respectively, and dilute to volume with the corresponding food simulant or chemical substitute solvent (95% ethanol), shake well, and prepare standard working solutions with concentrations of 0.005 mg / L, 0.01 mg / L, 0.02 mg / L, 0.04 mg / L, 0.06 mg / L, 0.08 mg / L and 0.10 mg / L. (S1.4) Preparation of working standard solutions for acidic food simulants: Accurately transfer 0.005 mL, 0.01 mL, 0.02 mL, 0.04 mL, 0.06 mL, 0.08 mL, and 0.10 mL of the intermediate standard solution into seven 10 mL volumetric flasks, respectively. Dilute to the mark with acidic food simulant solution to obtain working standard solutions with mass concentrations of 0.005 mg / L, 0.01 mg / L, 0.02 mg / L, 0.04 mg / L, 0.06 mg / L, 0.08 mg / L, and 0.10 mg / L, respectively. Then, transfer approximately 5.0 mL of each working solution, add 0.5 mL of ammonia solution, mix well, and filter through a 0.45 μm filter membrane before analysis. Prepare and use immediately.

[0014] Step S2, Preparation of Food Simulators (S2.1) Migration Test: The selection of conditions and operating procedures for the migration test shall comply with GB 5009.156 and

[0015] The migration test shall be conducted in accordance with the provisions of GB31604.1. If the immersion solution obtained cannot be tested immediately, it shall be stored in a sealed container in a refrigerator at 0℃~4℃. Before testing, the immersion solution shall be brought to room temperature before proceeding to the next test.

[0016] (S2.2) Water, alcohol food simulants and chemical alternative solvents (95% ethanol) test solutions: Take about 1 mL of the water, alcohol food simulants or chemical alternative solvents (95% ethanol) soaking solution obtained from the migration test, filter it through a 0.45 μm filter membrane, and then test it.

[0017] (S2.3) Acidic food simulant test solution: Take about 5.0 mL of the acidic food simulant soaking solution obtained from the migration test, add 0.5 mL of ammonia water and mix well. Filter through a 0.45 mm filter membrane and then test.

[0018] (S2.4) Oil-containing food simulant test solution: Weigh 2.0g (accurate to 1mg) olive oil infusion into a stoppered centrifuge tube, add 2mL of water and vortex for 1min, sonicate for 20min, centrifuge at 4000r / min for 5min, collect the lower aqueous solution, filter through a 0.45um filter membrane and test.

[0019] (S2.5) Blank solution: food simulants or chemical surrogate solvents (95% ethanol) which are not in contact with food contact materials and articles, are treated according to the above steps, respectively, to obtain the blank solution;

[0020] Step S3, instrument analysis (S3.1) Instrument parameter setting:

[0021]

[0022]

[0023] (S3.2) Draw the standard working curve: according to the reference chromatographic conditions listed above, the standard working solution is injected in turn for determination, and the concentration of methacrylamide in the standard working solution is taken as the abscissa, and the corresponding quantitative ion peak area is taken as the ordinate, to draw the standard working curve;

[0024] (S3.3) Determination of test solution: according to the reference chromatographic conditions listed above, the blank solution and sample test solution are determined in turn, and the qualitative retention time is determined, and the external standard method is used for quantitative determination;

[0025] (S3.4) Qualitative: the selected ions of the sample to be tested and the standard product appear at the same retention time (±1%), and the mass-to-charge ratio of the corresponding mass spectrum fragment ion is consistent with the standard product, and the abundance ratio compared with the standard product should meet the requirements of maximum ion abundance and allowable deviation, which can be qualitatively confirmed the target analyte.

[0026] The requirements of maximum ion abundance and allowable deviation are as follows:

[0027]

[0028]

[0029] The recovery of the method under the condition of repeatability is between 86.4% and 98.8%, and the repeatability is between 2.1% and 9.5%.

[0030] The detection limit and the quantitative limit of the method: the detection limit is calculated by S / N=3, and the quantitative limit is calculated by S / N=10. The detection limit of the method for the migration amount of three acrylamide compounds in water, acidic, alcoholic, and oil-containing food simulants and chemical surrogate solvents (95% ethanol) is 0.005 mg / kg, and the quantitative limit is 0.01 mg / kg.

[0031] The method designs different pretreatment schemes for different food simulants (aqueous, acidic, containing ethanol, containing oil): the acidic food simulants need to be adjusted with ammonia water, the oil-containing food simulants are extracted by water vortex ultrasonic, and the preparation method of seven concentration gradient standard working solutions is described, which ensures the applicability of the method in various food contact scenarios.

[0032] Regarding the selection of the mobile phase type: the chromatographic conditions of UPLC-MS / MS are optimized, three target components and 7 food simulants are involved in the method, the three compounds are all in positive ion mode, so after comparing water-acetonitrile, water-methanol, 0.1% formic acid aqueous solution-acetonitrile, 0.1% formic acid aqueous solution-methanol, 5mmol / L ammonium acetate aqueous solution-methanol as the mobile phase, 0.1% formic acid aqueous solution-methanol is used as the mobile phase to elute the target, which can get good peak shape, the separation degree can be the best for 7 food simulants, finally 0.1% formic acid aqueous solution-methanol is used as the mobile phase.

[0033] Regarding the selection of the chromatographic column: the three target components in the method are all easily soluble in water, so the sample is out of peak in high water phase. Therefore, three columns with different stationary phases in the Waters series are compared, which are UPLC BEHC 8 / UPLC BEH C18 / UPLC HSS T3. It is found that C18 and T3 can meet the requirements, but when doing precision test, it is found that when using C18 stationary phase as test column, the column efficiency becomes worse with time, the sensitivity becomes lower, and the peak shape becomes worse, which leads to that the recovery rate and repeatability cannot meet the requirements. It is because the C18 group modified in the C18 stationary phase will curl in high water phase for a long time, which leads to the above results. Therefore, the T3 column resistant to high water phase is used for testing in the follow-up, and no problem is found. Therefore, UPLC HSST3 is finally used as the test chromatographic column.

[0034] The method is developed through systematic column and mobile phase optimization experiments, and is specially adapted to the characteristics of acrylamide compounds, solving the technical problem of column efficiency decline in high water phase for a long time in the prior art. According to the conventional practice in the field of food contact material detection: for the analysis of polar compounds, the conventional first choice is traditional C18 column and traditional C8 column, and the inventors of the present application foresee the stability problem of C18 column stationary phase under high water phase condition, and the technical superiority of T3 column is verified through many experiments: the detection limit of the method reaches 0.005mg / kg, the recovery rate is 86.4%~98.8%, the repeatability is 2.1%~9.5%, and the long-term use stability is good. It can be seen that the selection of the T3 column of the present application is based on the specific technical problem found through experiments, and overcomes the technical bias.

[0035] The beneficial effects of the present application are:

[0036] 1、This method fills the gap of the detection standard. The method uses liquid chromatography-tandem mass spectrometry for detection, has high sensitivity, and can simultaneously determine the three acrylamide compounds by using multiple reaction monitoring (MRM) ion mode acquisition and strong anti-interference ability.

[0037] 2、The method has a detection limit of 0.005 mg / kg for the three acrylamide compounds in aqueous, acidic, ethanol-containing food simulant, oil-containing food simulant and chemical alternative solvent 95% (volume fraction) ethanol, a quantitative limit of 0.01 mg / kg, a recovery rate of 86.4% to 98.8%, and a repeatability of 2.1% to 9.5%, high precision, and meets the regulatory requirements. BRIEF DESCRIPTION OF DRAWINGS

[0038] Figure 1 is the first ion chromatogram of extraction of the three acrylamide compounds of the present application in T3 chromatographic column and food simulant water, and the three curves from left to right represent acrylamide, methacrylamide and N-(hydroxymethyl) acrylamide.

[0039] Figure 2 is the ion chromatogram of extraction of the three acrylamide compounds in C18 chromatographic column and food simulant water, and the three curves from left to right represent acrylamide, methacrylamide and N-(hydroxymethyl) acrylamide.

[0040] Figure 3 is the ion chromatogram of extraction of the three acrylamide compounds in C8 chromatographic column and food simulant water, and the three curves from left to right represent acrylamide, methacrylamide and N-(hydroxymethyl) acrylamide.

[0041] Figure 4 is the second ion chromatogram of extraction of the three acrylamide compounds of the present application in T3 chromatographic column and food simulant water, and the three curves from left to right represent acrylamide, methacrylamide and N-(hydroxymethyl) acrylamide. DETAILED DESCRIPTION

[0042] The technical solutions in the embodiments of the present application will be described in detail below with reference to the drawings in the embodiments of the present application. Obviously, the described embodiments are only a part of the embodiments of the present application, not all the embodiments. Based on the embodiments of the present application, all other embodiments obtained by those skilled in the art without creative labor fall within the scope of the present application.

[0043] It should be noted that all the directionality indications in the embodiments of the present application (such as up, down, left, right, front, back, etc.) are only used to explain the relative position relationship, motion condition, etc. between components in a certain specific posture (as shown in the drawings), and if the specific posture changes, the directionality indications will also change accordingly.

[0044] In addition, the descriptions involving "first", "second" and the like in the present application are only for the purpose of description, and cannot be understood as indicating or implying the relative importance of the indicated technical features or implicitly indicating the number of the indicated technical features. Therefore, the features defined as "first" and "second" can explicitly or implicitly include at least one of the features. In addition, the technical solutions of various embodiments can be combined with each other, but it must be based on the fact that a person skilled in the art can realize it, and when the combination of technical solutions contradicts each other or cannot be realized, it should be considered that the combination of technical solutions does not exist and is not within the protection scope required by the present application.

[0045] Embodiments

[0046] In this embodiment, first, the type of mobile phase used in the present application is selected, and the specific experiment is as follows:

[0047] The chromatographic conditions of UPLC-MS / MS are optimized. In this method, three target components and seven food simulants are involved. The three compounds are all in positive ion mode, so after comparing water-acetonitrile, water-methanol, 0.1% formic acid aqueous solution-acetonitrile, 0.1% formic acid aqueous solution-methanol, 5mmol / L ammonium acetate aqueous solution-methanol as mobile phase, 0.1% formic acid aqueous solution-methanol is used as mobile phase to elute the target, which can get good peak shape, and the separation degree can best consider the seven food simulants. Finally, 0.1% formic acid aqueous solution-methanol is used as the mobile phase.

[0048] Secondly, the selection of the chromatographic column is as follows: In this method, the three target components are all easily soluble in water, so the sample is out of peak in high water phase. Therefore, three columns with different stationary phases in the Waters series are compared, which are UPLC BEH C 8 / UPLC BEH C18 / UPLC HSS T3. It is found that C18 and T3 can both meet the requirements, but when doing precision test, it is found that when using C18 stationary phase as test column, the column efficiency becomes worse with time, the sensitivity becomes lower, and the peak shape becomes worse, which leads to that the recovery rate and repeatability cannot meet the requirements. It is because the C18 group modified in the C18 stationary phase will curl up in high water phase for a long time, which leads to the above results. Therefore, in the follow-up test, the T3 column resistant to high water phase is used, and no problem is found. Therefore, UPLCHSS T3 is finally used as the test chromatographic column.

[0049] The specific experimental content is as follows:

[0050] Step S1, configuration of standard working solution

[0051] (S1.1) Configuration of standard stock solution (1000 mg / L): Accurately weigh 10 mg (accurate to 0.1 mg) of each of the three acrylamide compound standard samples, dissolve in methanol, transfer to a 10 mL volumetric flask, dilute to the mark, shake well, and store in a 0-4°C refrigerator in a sealed state. The effective period is 6 months.

[0052] (S1.2) Configuration of standard intermediate solution (10 mg / L): Accurately transfer 0.10 mL of the standard stock solution to a 10 mL volumetric flask, dilute to the mark with methanol, shake well, and obtain a 10 mg / L standard intermediate solution. The solution is prepared immediately before use.

[0053] (S1.3) Configuration of standard working solution of water, alcohol food simulant, and chemical surrogate solvent (95% ethanol): Transfer 0.005 mL, 0.01 mL, 0.02 mL, 0.04 mL, 0.06 mL, 0.08 mL, and 0.10 mL of the above standard intermediate solution to seven 10 mL volumetric flasks, respectively, dilute to the mark with the corresponding food simulant or chemical surrogate solvent (95% ethanol), shake well, and prepare standard working solutions with concentrations of 0.005 mg / L, 0.01 mg / L, 0.02 mg / L, 0.04 mg / L, 0.06 mg / L, 0.08 mg / L, and 0.10 mg / L, respectively.

[0054] Step S2, preparation of food simulant

[0055] (S2.1) Migration test: The conditions and operation steps of the migration test are carried out in accordance with the provisions of GB 5009.156 and GB 31604.1. If the immersion solution obtained from the migration test cannot be tested immediately, it should be stored in a 0-4°C refrigerator in a sealed state. Before testing, the immersion solution should be restored to room temperature and then subjected to the next step of the test.

[0056] (S2.2) Water, alcohol food simulant and chemical surrogate solvent (95% ethanol) test solution: Take about 1 mL of water, alcohol food simulant or chemical surrogate solvent (95% ethanol) soaking solution obtained from the migration test, filter through a 0.45 um filter membrane, and then test.

[0057] (S2.3) Acidic food simulant test solution: Take about 5.0 mL of acidic food simulant soaking solution obtained from the migration test, add 0.5 mL of ammonia water, mix well, filter through a 0.45 mm filter membrane, and then test.

[0058] (S2.4) Oil-containing food simulant test solution: Weigh 2.0 g (accurate to 1 mg) of olive oil soaking solution into a centrifuge tube with a stopper, add 2 mL of water, vortex for 1 min, ultrasonic extract for 20 min, centrifuge at 4000 r / min for 5 min, collect the lower aqueous solution, and filter through a 0.45 um filter membrane for testing.

[0059] (S2.5) Blank test solution: Food simulant or chemical surrogate solvent (95% ethanol) not in contact with materials and products in contact with food, respectively, according to the above steps, to obtain the blank test solution.

[0060] Step S3, instrument analysis

[0061] (S3.1) Instrument parameter setting:

[0062]

[0063]

[0064] (S3.2) Draw the standard working curve: according to the reference chromatographic conditions listed above, the standard working solution is injected in turn to determine the concentration of methacrylamide in the standard working solution as the abscissa, and the corresponding quantitative ion peak area as the ordinate, and the standard working curve is drawn;

[0065] (S3.3) Test solution determination: according to the reference chromatographic conditions listed above, the blank test solution and sample test solution are determined in turn, and the retention time is qualitatively determined by the external standard method;

[0066] (S3.4) Qualitative: The selected ions of the sample to be tested and the standard product appear at the same retention time (± 1%), and the mass-to-charge ratio of the corresponding mass spectrum fragment ion is consistent with the standard product, and the abundance ratio compared with the standard product should meet the requirements of maximum ion abundance and allowable deviation, which can be qualitatively confirmed the target analyte.

[0067] The requirements of maximum ion abundance and allowable deviation are as follows:

[0068]

[0069] The determination results are as follows:

[0070] 1. The standard curve of the present application is as follows:

[0071]

[0072] 2. Precision and recovery rate experiment of the detection method

[0073]

[0074] Through the above test process, it can be known that the linear range, detection limit, quantification limit and precision of the test method of the present application all meet the requirements.

[0075] The recovery rate of the present method under repetitive conditions is between 86.4% and 98.8%, and the repeatability is between 2.1% and 9.5%.

[0076] It can be seen from Figure 1 that acrylamide, methacrylamide and N-(hydroxymethyl) acrylamide can be effectively separated and have symmetrical peak shapes, which can meet the daily testing needs of the present method.

[0077] Figures 2-4 The chromatograms of the present application are obtained using three different chromatographic columns under the same concentration / same instrument conditions. It can be seen from Figures 2-4 that when C8 chromatographic column is used for analysis, the response of acrylamide and methacrylamide is low and the peak shape is poor, which cannot meet the requirements of detection limit and accurate quantification; when C18 and T3 are used for analysis, the responses of the two are equivalent, but when the precision test is performed, the peak shape will become worse and the response will decrease with the passage of time when C18 chromatographic column is used. As Figure 3 Because the C18 stationary phase is exposed to a high aqueous mobile phase, the C18 surface will dehydrate due to the high surface tension, which is called stationary phase collapse, chain folding or stationary phase knotting, and the compound cannot normally interact with the stationary phase for retention, so this phenomenon occurs. The present inventors have verified through many experiments that the T3 column is finally selected for testing, which uses T3 bonded phase and high-strength silica gel, and can be compatible with 100% water phase, and no above phenomenon occurs during subsequent precision test. The present method has undergone systematic chromatographic column and mobile phase optimization experiments, and has been specially adapted for the characteristics of acrylamide compounds, solving the technical problem of long-term column efficiency decline in high aqueous phase conditions in the prior art. The selection of the T3 column of the present application is based on the specific technical problem found through experiments, which overcomes the technical bias.

[0078] The detection limit and the quantitative limit of the method: the detection limit is calculated by S / N=3, and the quantitative limit is calculated by S / N=10. The detection limit of the method for the migration amount of the three acrylamide compounds in water, acid, alcohol, oil-containing food simulation materials and chemical alternative solvents (95% ethanol) is 0.005 mg / kg, and the quantitative limit is 0.01 mg / kg. There is no detection method for the three acrylamide compounds before, and there is no detection standard for the migration amount of the three acrylamide compounds in food contact materials and products at home and abroad at present, which leads to the fact that the project cannot be judged in compliance, and is not conducive to the product quality control and improvement of the production enterprises. The method fills the gap in the market.

[0079] While embodiments of the present application have been shown and described, it is to be understood that the embodiments described are merely divergences, modifications, replacements and variations of the embodiments, and the scope of the present application is defined by the appended claims and their equivalent ranges.

Claims

1. A method for simultaneously determining the migration of three acrylamide compounds from food contact materials and articles, characterized in that, Comprising the following steps: Step S1, configuration of standard working solution (S1.1) Configuration of standard stock solution: accurately weigh three acrylamide compound standard samples respectively, dissolve them with methanol, transfer them to a volumetric flask, and dilute to the mark, shake well, and store them in a 0℃ to -4°C refrigerator; (S1.2) Configuration of standard intermediate solution: accurately pipette the standard stock solution into a volumetric flask, dilute to the mark with methanol, shake well, and obtain the standard intermediate solution; (S1.3) Configuration of standard working solution of water, alcohol food simulant, and chemical alternative solvent: pipette the above standard intermediate solution into a volumetric flask, dilute to the mark with the corresponding food simulant or chemical alternative solvent, shake well, and prepare the standard working solution; (S1.4) Configuration of standard working solution of acidic food simulant: pipette the standard intermediate solution into a volumetric flask, dilute to the mark with the acidic food simulant solution, obtain the standard working solution, then pipette the working solution, add ammonia water, mix well, filter through a filter membrane, and test; Step S2, preparation of food simulant (S2.1) Migration test: the conditions and operation steps of the migration test are performed according to the provisions of GB 5009.156 and GB 31604.1, and the immersion liquid obtained by the migration test should be stored in a 0℃ to 4°C refrigerator if it cannot be tested immediately; (S2.2) Test solution of water, alcohol food simulant, and chemical alternative solvent: take the water, alcohol food simulant, or chemical alternative solvent immersion liquid obtained by the migration test, filter through a filter membrane, and test; (S2.3) Test solution of acidic food simulant: take the acidic food simulant immersion liquid obtained by the migration test, add ammonia water, mix well, filter through a filter membrane, and test; (S2.4) Test solution of oil-containing food simulant: weigh the olive oil immersion liquid into a centrifugal tube with a stopper, add water, vortex, ultrasonic extract, centrifuge, collect the lower aqueous solution, filter through a filter membrane, and test; (S2.5) Blank test solution: the food simulant or chemical alternative solvent (95% ethanol) not in contact with the food contact material and product is treated according to the above steps to obtain the blank test solution; Step S3, instrument analysis (S3.2) Draw the standard working curve: according to the reference chromatographic conditions listed above, the standard working solution is sequentially injected and measured to draw the standard working curve; (S3.3) Determination of test solution: according to the reference chromatographic conditions listed above, the blank test solution and sample test solution are sequentially determined, qualitatively determined according to the retention time, and quantitatively determined by the external standard method; (S3.4) Qualitative analysis: the selected ion of the sample to be tested and the standard sample appears at the same retention time, and the mass-to-charge ratio of the corresponding mass spectrum fragment ion is consistent with that of the standard sample, and the abundance ratio compared with the standard sample should meet the requirements of maximum ion abundance and allowable deviation, which can be qualitatively confirmed.

2. The method for simultaneously determining the migration amounts of three acrylamide compounds in food contact materials and articles according to claim 1, characterized in that, The precision of the method is that the recovery rate is between 86.4% and 98.8% under repetitive conditions, and the repeatability is between 2.1% and 9.5%.

3. The method for simultaneously determining the migration amounts of three acrylamide compounds in food contact materials and articles according to claim 2, characterized in that, The method has a detection limit and a quantitative limit: the detection limit is calculated by S / N=3, and the quantitative limit is calculated by S / N=10; the detection limit of the method for the migration amount of the three acrylamide compounds in water, acid, alcohol, oil-containing food simulant and chemical alternative solvent is 0.005 mg / kg, and the quantitative limit is 0.01 mg / kg.

4. The method of simultaneously determining the migration of three acrylamide compounds from food contact materials and articles of claim 1, wherein, The chemical alternative solvent is 95% ethanol by volume.

5. The method of simultaneously determining the migration of three acrylamide compounds from food contact materials and articles of claim 1, wherein, In the step S3.1, the A solution is 0.1% formic acid water, and the B solution is methanol; 0.1% formic acid water-methanol is used as the mobile phase.

6. The method of simultaneously determining the migration of three acrylamide compounds from food contact materials and articles of claim 1, wherein, In the step S3.2, a standard working curve is drawn: the concentration of methacrylamide in the standard working solution is used as the horizontal coordinate, and the corresponding quantitative ion peak area is used as the vertical coordinate.

7. The method of simultaneously determining the migration of three acrylamide compounds from food contact materials and articles of claim 1, wherein, In the step S3.4, the maximum ion abundance and the allowable deviation are as follows:

8. The method of simultaneously determining the migration of three acrylamide compounds from food contact materials and articles of claim 1, wherein, In the step S1.3, the water, alcohol food simulant and chemical alternative solvent standard working solution are configured in seven concentrations, which are 0.005 mg / L, 0.01 mg / L, 0.02 mg / L, 0.04 mg / L, 0.06 mg / L, 0.08 mg / L and 0.10 mg / L.

9. The method of simultaneously determining the migration of three acrylamide compounds from food contact materials and articles of claim 1, wherein, In the step S1.4, the acid food simulant standard working solution is configured in seven mass concentrations, which are 0.005 mg / L, 0.01 mg / L, 0.02 mg / L, 0.04 mg / L, 0.06 mg / L, 0.08 mg / L and 0.10 mg / L.

Images