CN112782298A - Method for rapidly detecting residual quantity of 32 compounds in food contact material - Google Patents
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Abstract
The invention provides a rapid detection method for residual quantities of 32 compounds in a food contact material, which adopts headspace-gas chromatography to carry out qualitative analysis and/or external standard quantitative analysis on the food contact material; the 32 compounds are ethanol, acetone, isopropanol, tert-butanol, butanone, ethyl acetate, benzene, isopropyl acetate, propylene glycol methyl ether, pentanal, n-butanol, sec-butyl acetate, toluene, hexanal, butyl acetate, ethylbenzene, styrene, p-xylene, m-xylene, propylene glycol methyl ether acetate, o-xylene, styrene, phenylpropene, 1,2, 3-trimethylbenzene, n-propylbenzene, alpha-methylstyrene, benzaldehyde, 1,2, 4-trimethylbenzene, sec-butylbenzene, n-butylbenzene, 1,3, 5-trimethylbenzene and divinylbenzene. The method is simple and convenient, is easy to operate, adopts a temperature programming mode for separation and an external standard method for quantification, and is 0.01-0.10 mg/m2The linear correlation coefficient was 0.995.
Description
Technical Field
The invention relates to a method for rapidly detecting the residual quantity of 32 compounds in a food contact material, in particular to a headspace gas chromatography detection method for the residual quantity of 32 compounds (ethanol, acetone, isopropanol, tert-butanol, butanone, ethyl acetate, benzene, isopropyl acetate, propylene glycol methyl ether, pentanal, n-butanol, sec-butyl acetate, toluene, hexanal, butyl acetate, ethylbenzene, styrene, p-xylene, m-xylene, propylene glycol methyl ether acetate, o-xylene, styrene, phenylpropene, 1,2, 3-trimethylbenzene, n-propylbenzene, alpha-methylstyrene, benzaldehyde, 1,2, 4-trimethylbenzene, sec-butylbenzene, n-butylbenzene, 1,3, 5-trimethylbenzene and divinylbenzene) in the food contact material.
Background
Food contact materials are products that come into direct contact with food, and their hygienic safety is closely related to the physical health of people. The novelty, the aesthetic appeal and the branding are new characteristics of food contact materials, so that the printing ink is more and more widely used on the food contact materials, however, the organic matters possibly contained in the printing ink are divided into: benzenes, alcohols, esters, aldehydes, ketones, and the like. After entering the human body, mild poisoning may cause dizziness, headache, nausea, vomiting, teetering gait, mild disturbance of consciousness and eye and upper respiratory tract irritation, and coma, convulsion, blood pressure drop and respiratory circulation failure in the serious patients.
The national standards GB 9685-2016 and GB 4806.1-2016 have no authorization for carcinogenic, mutagenic and reproductive toxic substances to be used for producing food contact materials, and stipulate that: propylene glycol methyl ether acetate (SML): 0.05 mg/kg; α -methylstyrene (SML): 0.05 mg/kg. GB 4806.10-2016 national food safety Standard food contact coatings and coatings reflects the migration and content of some harmful substances in food contact materials which may contact food, only with respect to the materials expected or already in contact with food. At present, the national standard of China (food safety national standard) composite material and product for food contact (quotation of comments) is in the process of making, and the residual quantity of solvent is regulated to be less than or equal to 5mg/m2. GB/T10004-2008 'plastic composite film for packaging, dry bag compounding and extrusion compounding' aims at that the total amount of solvent residues in the composite film and the bag is less than or equal to 5.0mg/m2The residual benzene solvent was not detected. However, harmful substances such as partial benzene, ester, alcohol, aldehyde and other compounds in the food contact composite material are not detected, and the residual quantity of the compounds is not clearly specified, so that the research on the residual solvent in the food contact material is urgent, and a method for measuring the residual solvent in the food contact material is needed.
Therefore, a test method for rapidly determining the content of 32 compounds (ethanol, acetone, isopropanol, tert-butanol, butanone, ethyl acetate, benzene, isopropyl acetate, propylene glycol methyl ether, valeraldehyde, n-butanol, sec-butyl acetate, toluene, hexanal, butyl acetate, ethylbenzene, styrene, p-xylene, m-xylene, propylene glycol methyl ether acetate, o-xylene, styrene, phenylpropene, 1,2, 3-trimethylbenzene, n-propylbenzene, alpha-methylstyrene, benzaldehyde, 1,2, 4-trimethylbenzene, sec-butylbenzene, n-butylbenzene, 1,3, 5-trimethylbenzene and divinylbenzene) in a food contact material product is established, and has important significance for researching and improving the quality of the food contact material.
A headspace-gas chromatography method is published for simultaneously measuring 17 solvent residues in a composite membrane bag, wherein the 17 solvent residues comprise 2-methylpentane, ethanol, acetone, isopropanol, butanone, ethyl acetate, benzene, isopropyl acetate, n-butanol, 1, 2-dichloroethane, n-butanol, toluene, butyl acetate, propylene glycol monomethyl ether acetate, p-xylene, m-xylene, o-xylene and the like, and compounds such as easily-detected ethylbenzene and the like are not measured; separating with DB-WAX capillary chromatographic column (30m × 0.25mm, 0.25 μm), and measuring by external standard method. The method can only measure 17 solvent residues in the composite membrane bag, and other parts of alpha-methyl styrene, benzaldehyde and divinylbenzene are not described in documents. The document is difficult to carry out accurate qualitative confirmation on the 32 compounds, and has certain limitation in the practical application process. At present, no research report on a headspace gas chromatography detection method of 32 compounds in food contact material products exists in China.
Disclosure of Invention
The invention aims to provide a method for rapidly detecting the residual quantity of 32 compounds in food contact materials, so as to solve the problems in the prior art.
The technical scheme of the invention is as follows:
a rapid detection method for 32 compound residual quantities in food contact materials is characterized in that qualitative analysis and/or external standard quantitative analysis are carried out on the food contact materials by adopting headspace-gas chromatography;
the 32 compounds are ethanol, acetone, isopropanol, tert-butanol, butanone, ethyl acetate, benzene, isopropyl acetate, propylene glycol methyl ether, pentanal, n-butanol, sec-butyl acetate, toluene, hexanal, butyl acetate, ethylbenzene, styrene, p-xylene, m-xylene, propylene glycol methyl ether acetate, o-xylene, styrene, phenylpropene, 1,2, 3-trimethylbenzene, n-propylbenzene, alpha-methylstyrene, benzaldehyde, 1,2, 4-trimethylbenzene, sec-butylbenzene, n-butylbenzene, 1,3, 5-trimethylbenzene and divinylbenzene.
More specifically, the invention provides a method for rapidly detecting the residual quantity of 32 compounds in a food contact material, which is characterized by comprising the following steps:
(1) cutting a food contact material sample into fragments not larger than (1-10) mmx (1-30) mm to serve as a sample; putting the sample into a headspace bottle, adding olive oil serving as a solvent matrix, filling nitrogen, sealing and shaking uniformly, and performing headspace extraction at 20-150 ℃ for 10-180 min;
(2) carrying out gas chromatography analysis on the gas in the headspace bottle, determining the peak emergence time and the peak area of the 32 compounds, and calculating according to a standard working curve to obtain the residual quantity of the 32 compounds in the sample;
the feed-liquid ratio of the sample to the extraction solvent is as follows: (0.001 to 0.010) m2Sample/(0.01-1) mL solvent matrix.
Further, in the step (1), accurately taking (0.001-0.010) m2The sample is sent into a 20mL headspace bottle, 10-100 mu L of olive oil is added to serve as a solvent matrix, nitrogen is filled, and the mixture is vortexed, shaken and uniformly mixed.
Further, in the step (2), the test conditions of the gas chromatograph are as follows: a column of 6% cyanopropylphenyl 94% dimethylpolysiloxane, for example a 60 m.times.1.8 um.times.0.32 mm DB-624 column or a functionally equivalent column; the sample injection volume is as follows: 1-10 mL; the carrier gas is nitrogen, and the flow rate of the carrier gas is as follows: 0.1-5 mL/min; hydrogen Flame Ionization Detector (FID) detection;
the column temperature heating program of the gas chromatography is as follows: keeping the initial temperature at 30-70 ℃ for 0-10 min; then raising the temperature to 70 ℃ at the speed of 2-30 ℃/min, and keeping the temperature for 0-10 min; raising the temperature to 180 ℃ at the speed of 2-40 ℃/min, and keeping the temperature for 0-10 min; then raising the temperature to 240 ℃ at the speed of 1-30 ℃/min, and keeping the temperature for 0-10 min.
Further, the method for rapidly detecting the residual quantity of the 32 compounds in the food contact material further comprises the following manufacturing process of the standard working curve:
(1) respectively weighing 32 compounds of 0.1000g, placing the compounds in volumetric flasks, respectively dissolving the compounds with N, N-dimethylacetamide and fixing the volume to prepare a standard stock solution with the concentration of 1000 mg/L;
(2) diluting the standard stock solution step by adopting N, N-dimethylacetamide to obtain a series of gradient standard working solutions of 10-100 mg/L;
(3) and injecting the gradient standard working solution into a headspace bottle, balancing for a period of time, determining peak positions of the 32 compounds in a gas chromatograph, recording peak areas of the 32 compounds, and making a standard working curve by taking the concentrations of the 32 compounds as abscissa and the peak areas as ordinate.
Compared with the prior art, the invention has the following advantages:
the headspace-gas chromatography is adopted, the method is simple and convenient, the operation is easy, the waste of a large amount of time is avoided, and meanwhile, the pollution to the environment is avoided by adopting a small amount of solvent matrix; the 32 compound target substances are effectively separated from other components by adopting a temperature programming mode, direct qualitative and external standard method quantitative determination are accurate, the accuracy of detection results is ensured, and the detection sensitivity is improved; the invention has the most complete extraction effect, can meet the requirements of effective separation and quantitative analysis, and is 0.01-0.10 mg/m2The linear correlation coefficient is 0.995, and the quantitative limit of the method is 0.01mg/m2The recovery rate of the mixed standard solution is 81.9-116.7%, and the RSD value is 4.9-18.0%.
Drawings
FIG. 1 is a gas chromatogram of 32 compounds;
the chromatographic peaks in the figure are sequentially: ethanol, acetone, isopropanol, tert-butanol, butanone, ethyl acetate, benzene, isopropyl acetate, propylene glycol methyl ether, pentanal, n-butanol, sec-butyl acetate, toluene, hexanal, butyl acetate, ethylbenzene, styrene, p-xylene, m-xylene, propylene glycol methyl ether acetate, o-xylene, styrene, cumene, phenylpropylene, 1,2, 3-trimethylbenzene, n-propylbenzene, alpha-methylstyrene, benzaldehyde, 1,2, 4-trimethylbenzene, sec-butylbenzene, n-butylbenzene, 1,3, 5-trimethylbenzene, divinylbenzene.
Detailed Description
The invention will be further illustrated with reference to the following specific examples. It should be understood that this example is for illustrative purposes only and is not intended to limit the scope of the present invention. Further, it should be understood that various changes or modifications of the present invention may be made by those skilled in the art after reading the teaching of the present invention, and such equivalents may fall within the scope of the present invention as defined in the appended claims.
All reagents should be chromatographically pure unless otherwise specified.
Gas chromatograph: equipped with a hydrogen Flame Ionization Detector (FID) and a headspace instrument.
Analytical balance: the index values were 0.0001g and 0.00001 g.
Example 1
(1) Preparing a sample to be tested:
taking a representative food contact sample, and cutting the food contact sample into fragments of not more than 10mm multiplied by 30mm to be used as a sample; accurately weighing 0.004m2Placing in a headspace bottle, adding 40 μ L oleum Olivarum as extraction solvent, introducing nitrogen gas, shaking, and performing headspace extraction at 80 deg.C for 30 min;
(2) preparation of standard solutions:
(1)0.1000g of 32 compounds are weighed out and placed in volumetric flasks, 0.1000g of the compounds are dissolved by N, N-dimethylacetamide and the volume is constant, and standard stock solutions with the concentration of 1000mg/L are prepared.
(2) Diluting the standard stock solution with N, N-dimethylacetamide to obtain 0.01mg/m2、0.02mg/m2、0.04mg/m2、0.08mg/m2And 0.10mg/m2Series of gradients standard working solutions.
(3) Injecting the gradient standard working solution into a gas chromatograph by a headspace method, measuring by a hydrogen flame ionization detector, determining 32 compounds, namely ethanol, acetone, isopropanol, tert-butyl alcohol, butanone, ethyl acetate, benzene, isopropyl acetate, propylene glycol monomethyl ether, valeraldehyde, n-butyl alcohol, sec-butyl acetate, toluene, hexanal, butyl acetate and ethylbenzene, styrene, p-xylene, m-xylene, propylene glycol methyl ether acetate, o-xylene, styrene, phenylpropylene, 1,2, 3-trimethylbenzene, n-propylbenzene, alpha-methylstyrene, benzaldehyde, 1,2, 4-trimethylbenzene, sec-butylbenzene, n-butylbenzene, 1,3, 5-trimethylbenzene and divinylbenzene, recording peak areas of standard substances, and making a standard working curve equation by taking the concentration ratio as a horizontal coordinate and the peak areas as a vertical coordinate.
The gas chromatography conditions were: a chromatographic column: DB-62460m × 1.8um × 0.32mm capillary column; carrier gas: n is a radical of2(ii) a Flow rate of carrier gas: 1.0 ml/min; a sample inlet: the temperature is 200 ℃, the sample injection amount is 1mL, and the split ratio is 5: 1; column temperature: keeping the temperature at 40 ℃ for 3min, heating to 70 ℃ at 2 ℃/min, keeping the temperature for 0min, heating to 180 ℃ at 20 ℃/min, keeping the temperature for 3.5min, heating to 240 ℃ at 20 ℃/min, and keeping the temperature for 2.5 min;
the balance time is 30min, and the balance temperature is 80 ℃; the temperature of the transmission line is 100 ℃; the pressure balance time is 1min, and the sample injection time is 1 min.
(4) According to the method in the step (3), gas in the headspace bottle in the step (1) is subjected to gas chromatography, 31 compounds and peak areas thereof are measured, calculation is performed according to the standard working curve equation (linear equation) obtained in the step (3), linear fitting is performed by adopting a least square method, and linear equations, correlation coefficients of the 32 compounds and quantitative limits calculated by a 10S/N calculation method are shown in Table 1.
(5) Qualitative analysis
Corresponding to the step (4), under the same test conditions, the retention time (± 0.5%) of the analyte in the sample and the 31 substance standard substances detected simultaneously is the same, and then the presence of the corresponding analyte in the sample can be determined.
(6) Quantitative analysis
Corresponding to the step (4), the method adopts an external standard method for quantification, selects standard working solution with similar concentration according to the content of the substance to be detected in the sample, inserts the same volume of the standard working solution and the sample solution into the sample for measurement, and the response values of the 32 compounds in the standard working solution and the sample solution to be detected are within the linear range of the instrument.
If the detection response value of the sample liquid is beyond the linear range detected by the instrument, the sample liquid can be properly diluted and then measured. The chromatograms of the 32 compounds under the above chromatographic conditions are shown in FIG. 1.
Linear equation, retention time, linear range, correlation coefficient and quantitative limit for the method of table 1
(7) Detection lower bound
Headspace measurements were performed on 32 compounds at different concentrations in the blank food-contact samples according to the pretreatment and analysis methods described above, with the lowest detection limit concentration determined at 3-fold signal-to-noise ratio (S/N ═ 3) and the lowest detection limit concentration determined at 10-fold signal-to-noise ratio (S/N ═ 10), with a detection limit of 0.01mg/m2。
Experimental example: recovery rate experiment and precision experiment
Adding 0.050mg/m into blank food contact sample2The 32 compounds with the concentration are repeated for 3 times according to the pretreatment and analysis method, the average recovery rate is obtained by measuring and calculating, the precision is calculated by Relative Standard Deviation (RSD), the recovery rate is 81.9-116.7%, the RSD value is 4.9-18.0%, and the test requirement is met.
Claims (6)
1. A rapid detection method for 32 compound residual quantities in food contact materials is characterized in that qualitative analysis and/or external standard quantitative analysis are carried out on the food contact materials by adopting headspace-gas chromatography;
the 32 compounds are ethanol, acetone, isopropanol, tert-butanol, butanone, ethyl acetate, benzene, isopropyl acetate, propylene glycol methyl ether, pentanal, n-butanol, sec-butyl acetate, toluene, hexanal, butyl acetate, ethylbenzene, styrene, p-xylene, m-xylene, propylene glycol methyl ether acetate, o-xylene, styrene, phenylpropene, 1,2, 3-trimethylbenzene, n-propylbenzene, alpha-methylstyrene, benzaldehyde, 1,2, 4-trimethylbenzene, sec-butylbenzene, n-butylbenzene, 1,3, 5-trimethylbenzene and divinylbenzene.
2. The method of claim 1 for rapid detection of residual amounts of 32 compounds in food contact materials, comprising the steps of:
(1) cutting a food contact material sample into fragments not larger than (1-10) mmx (1-30) mm to serve as a sample; putting the sample into a headspace bottle, adding olive oil serving as an extraction solvent matrix, filling nitrogen, sealing and shaking uniformly, and performing headspace extraction at 20-150 ℃ for 10-180 min;
(2) and (3) carrying out gas chromatography analysis on the gas in the headspace bottle, measuring the peak emergence time and the peak area of the 32 compounds, and calculating the residual quantity of the 32 compounds in the sample according to a standard working curve.
3. The method for rapidly detecting the residual amount of 32 compounds in a food contact material according to claim 3, wherein the feed-to-liquid ratio of the sample to the extraction solvent is: (0.001 to 0.010) m2Sample/(0.01-1) mL solvent matrix.
4. The method for rapidly detecting the residual quantity of 32 compounds in food contact material according to claim 3, wherein in the step (1), (0.001-0.010) m is accurately selected2The method comprises the steps of conveying a sample into a 20mL headspace bottle, adding 10-100 mu L of olive oil serving as a solvent matrix, filling nitrogen, and carrying out vortex oscillation and uniform mixing.
5. The method for rapidly detecting the residual quantity of 32 compounds in a food contact material according to claim 3, wherein in the step (2), the test conditions of the gas chromatography are as follows: a column of 6% cyanopropylphenyl 94% dimethylpolysiloxane, for example a 60 m.times.1.8 um.times.0.32 mm DB-624 column or a functionally equivalent column; the sample injection volume is as follows: 1-10 mL; the carrier gas is nitrogen, and the flow rate of the carrier gas is as follows: 0.1-5 mL/min; hydrogen Flame Ionization Detector (FID) detection;
the column temperature heating program of the gas chromatography is as follows: keeping the initial temperature at 30-70 ℃ for 0-10 min; then raising the temperature to 70 ℃ at the speed of 2-30 ℃/min, and keeping the temperature for 0-10 min; raising the temperature to 180 ℃ at the speed of 2-40 ℃/min, and keeping the temperature for 0-10 min; then raising the temperature to 240 ℃ at the speed of 1-30 ℃/min, and keeping the temperature for 0-10 min.
6. The method for rapidly detecting the residual quantity of 32 compounds in a food contact material according to claim 3, further comprising the step of preparing the standard working curve:
(1) respectively weighing 32 compounds of 0.1000g, placing the compounds in volumetric flasks, respectively dissolving the compounds with N, N-dimethylacetamide and fixing the volume to prepare a standard stock solution with the concentration of 1000 mg/L;
(2) diluting the standard stock solution step by adopting N, N-dimethylacetamide to obtain a series of gradient standard working solutions of 10-100 mg/L;
(3) and injecting the gradient standard working solution into a headspace bottle, balancing for a period of time, determining peak positions of the 32 compounds in a gas chromatograph, recording peak areas of the 32 compounds, and making a standard working curve by taking the concentrations of the 32 compounds as abscissa and the peak areas as ordinate.
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| CN114544834A (en) * | 2022-03-07 | 2022-05-27 | 四川蓝城检测技术有限公司 | Method for measuring volatile flavor components in soy sauce by using static headspace-gas chromatography |
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| Publication number | Priority date | Publication date | Assignee | Title |
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| CN114544834A (en) * | 2022-03-07 | 2022-05-27 | 四川蓝城检测技术有限公司 | Method for measuring volatile flavor components in soy sauce by using static headspace-gas chromatography |
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