CN111624282A - Method for detecting phthalate substances in self-heating hot pot packaging inner box - Google Patents
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- G01N30/02—Column chromatography
- G01N30/04—Preparation or injection of sample to be analysed
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- G01N30/26—Conditioning of the fluid carrier; Flow patterns
- G01N30/28—Control of physical parameters of the fluid carrier
- G01N30/30—Control of physical parameters of the fluid carrier of temperature
- G01N2030/3076—Control of physical parameters of the fluid carrier of temperature using specially adapted T(t) profile
Abstract
The invention discloses a preparation method of a sample solution for detecting phthalate substances in an inner box of a self-heating hot pot package, and also provides a content detection method of the phthalate substances in the inner box of the self-heating hot pot package. The preparation method of the sample solution reduces the viscosity of the packaged sample, enables the phthalate substances in the sample to be easily dispersed, effectively improves the extraction efficiency, avoids the loss of the phthalate substances in the sample solution to be detected, and improves the detection accuracy. The method for detecting the content of the phthalate substances has the advantages of better universality and specificity, high sensitivity, convenient operation and moderate analysis time, provides effective guarantee for the quality control of the phthalate substances in the self-heating hot pot packaging inner box, and ensures the food safety.
Description
Technical Field
The invention relates to a method for detecting phthalate substances in food packaging, in particular to a method for detecting 18 phthalate substances in an internal self-heating type hot pot packaging box.
Background
Phthalate (PAEs) is a high-molecular plasticizer, is commonly used in food packaging materials, can greatly improve the plasticity and the ductility of the materials, however, the PAEs are also a persistent environmental hormone pollutant, can disturb the metabolism in vivo and poison internal organs and reproductive organs when being taken into a human body at an ultra-safe level, and even can cause three-cause effects on the human body. Because stable covalent bonds cannot be formed between the PAEs and the plastic monomers, when the environmental temperature, the PH and the like change or under the conditions of polar groups of food and the like, the PAEs are easy to separate out from the packaging material and permeate and migrate into the food, and further have adverse effects on the health of human bodies. Relevant standards and regulations aiming at the residual or migration limit of PAEs in food packaging materials are provided in various countries, and the content of phthalate in food is strictly monitored.
With the acceleration of the pace of life, the demand of people for fast food products for fast food is gradually increasing. The self-heating hot pot is concerned by light consumers since 2015 appears due to the consideration of rapidness of convenient foods and deliciousness of the hot pot, and the sales volume of the self-heating hot pot is increased in geometric multiples under the promotion of sugar wine and an e-commerce platform, so that the self-heating hot pot is moved to the national market from ChuanYu areas and becomes popular food which is well loved by consumers. The self-heating convenient hot pot food contains a large amount of grease, the inner packaging box in direct contact with the self-heating convenient hot pot food is mostly a plastic product, and the self-heating hot pot food is easily polluted by the plasticizer due to the good fat solubility of the plasticizer, and Phthalic Acid Ester (PAEs) migration residues may exist in the self-heating convenient hot pot food. The research on the migration of the plasticizer in the self-heating convenient hot pot packaging material is only rarely reported at present. Therefore, the method for detecting 18 PAEs in the self-heating type hot pot packaging inner box has important significance for quality control and PAEs safety risk assessment in the self-heating type hot pot food packaging production process.
Disclosure of Invention
In order to solve the problems, the invention provides a preparation method of a sample solution for detecting phthalate substances in an inner box of a self-heating hot pot package, which comprises the following steps:
1) adding a food simulant with the capacity of 2/3-3/4 into a self-heating hot pot packaging box, and heating for 15-30 min according to the heating process of the self-heating hot pot to obtain a food simulant solution;
2) and (2) adding n-hexane into the food simulation solution obtained in the step 1), uniformly mixing, performing ultrasonic extraction, centrifuging, and filtering supernatant to obtain the food simulation solution.
Further, the adding amount of the food simulant in the step 1) is 2/3 of the capacity of the self-heating hot pot packaging box; the heating is carried out for 15 min.
Further, the food simulant is 10-20% ethanol or 90-100% isooctane, preferably 10% ethanol or 100% isooctane.
Further, the mass-to-volume ratio of the food simulation solution in the step 2) to n-hexane is 0.5-1.5 g: 2ml, preferably 1 g: 2 ml.
Further, the ultrasonic extraction time of the step 2) is 10min, and the temperature is 40 ℃.
Further, the centrifugation time in the step 2) is 10min, and the speed is 4000 r/min; the filtration was performed with a 0.22 μm filter.
The invention also provides a method for detecting the content of the phthalate substances in the self-heating hot pot packaging inner box, which comprises the following steps:
a. test solution: taking the obtained sample solution to be detected as a test sample solution;
b. standard working solutions of series concentration: taking diallyl phthalate standard substance and 17 phthalate mixed standard substances, adding n-hexane for dissolving, and diluting into a series of concentration standard working solutions;
c. respectively absorbing a test solution and a series of concentration standard working solutions, injecting the solutions into a gas chromatography-mass spectrometer, measuring peak areas, and calculating the content of phthalate substances according to the peak areas by an external standard method;
the chromatographic conditions are as follows:
a chromatographic column: taking (5% -phenyl) -methyl polysiloxane as a filling agent, keeping the initial column temperature at 60 ℃ at the injection inlet temperature of 280 ℃, keeping the initial column temperature for 1min, heating to 220 ℃ at the speed of 20 ℃/min, keeping the initial column temperature for 1min, heating to 260 ℃ at the speed of 5 ℃/min, and keeping the initial column temperature for 0 min; finally, the temperature is increased to 300 ℃ at the speed of 10 ℃/min, and the temperature is kept for 3 min;
the mass spectrum conditions are as follows: the ion source is an electron bombardment source; the mass spectrometry monitoring mode is a selective ion monitoring mode.
Furthermore, the concentration of the diallyl phthalate in the series of concentration standard working solutions is 0.05138-5.138 mug/mL, and the concentration of the 17 phthalate mixed standard solution is 0.05-5.0 mug/mL.
Furthermore, the chromatographic column in the chromatographic condition is Agilent HP-5MS with the specification of 30m × 250 μm × 0.25 μm, the carrier gas is helium, the flow rate is 1mL/min, the sample injection mode is non-split flow sample injection, the sample injection amount is 1 μ L, and the solvent cutting time is 7 min.
Further, the ionization energy in the mass spectrometry conditions is: 70eV, the ion source temperature and the interface temperature are both 280 ℃ and the quadrupole rod temperature is 150 ℃.
The preparation method of the sample solution for detecting the phthalate substances in the self-heating hot pot packaging inner box reduces the viscosity of the packaged sample, enables the phthalate substances in the sample to be easily dispersed, effectively improves the extraction efficiency, avoids the loss of the phthalate substances in the sample solution to be detected, improves the detection accuracy, reduces the preparation steps of the sample solution to be detected, and saves the analysis time.
The test proves that: the method for detecting the content of the phthalate in the self-heating hot pot packaging inner box has the advantages of better universality and specificity, high sensitivity, convenience in operation and moderate analysis time, provides effective guarantee for quality control of the phthalate in the self-heating hot pot packaging inner box, ensures food safety and has good application prospect.
Obviously, many modifications, substitutions, and variations are possible in light of the above teachings of the invention, without departing from the basic technical spirit of the invention, as defined by the following claims.
The present invention will be described in further detail with reference to the following examples. This should not be understood as limiting the scope of the above-described subject matter of the present invention to the following examples. All the technologies realized based on the above contents of the present invention belong to the scope of the present invention.
Drawings
FIG. 1 shows total ion current chromatogram of chromatographic column HP-5MS for separating 18 PAEs (the PAEs represented by the numbers of each peak in the figure are shown in tables 1 and 2)
Detailed Description
Example 1 detection of the content of phthalate in the inner packaging case of self-heating chafing dish
1. Preparation of test solution
1) Adding 2/3% of 10% ethanol into a self-heating hot pot packaging box, and heating for 20min according to the heating process of the self-heating hot pot to obtain 10% ethanol food simulation solution;
2) taking 1g (accurate to 0.1mg) of the 10% ethanol food simulation solution obtained in the step 1), accurately adding 2mL of n-hexane into a 10mL colorimetric tube, carrying out vortex oscillation for 10min to fully and uniformly mix the solution, carrying out ultrasonic treatment for 10min at 40 ℃ in a water bath, centrifuging for 5min at 4000r/min, collecting supernatant, and filtering through a 0.22 mu m Nylon filter membrane to obtain a test solution;
2. preparation of Standard solutions
Accurately weighing 0.03491g of diallyl phthalate standard substance into a 10mL volumetric flask, dissolving with n-hexane for constant volume to obtain 3.425mg/mL diallyl phthalate standard stock solution, accurately transferring 150 mu L of diallyl phthalate standard stock solution, keeping the n-hexane constant volume to 50mL, and uniformly oscillating to obtain 10.275 mu g/mL diallyl phthalate standard intermediate solution;
accurately transferring 1.0mL of 17 phthalate mixed standard substances, diluting the normal hexane to 100mL, and uniformly oscillating to obtain 17 phthalate mixed standard intermediate solution of 10 mu g/mL;
accurately transferring 5, 20, 100, 200, 400 and 500 mu L of 17 phthalate mixed standard intermediate liquid with the concentration of 10 mu g/mL and 10.275 mu g/mL diallyl phthalate standard intermediate liquid respectively, and using normal hexane to fix the volume to 1.0mL to prepare the phthalate mixed standard with the concentrations of 17 phthalate: 0.05, 0.2, 1.0, 2.0, 4.0 and 5.0 μ g/mL, and diallyl phthalate concentrations were: 0.05138, 0.2055, 1.028, 2.055, 4.11 and 5.138 μ g/mL of mixed-series concentration standard working solutions;
3. respectively absorbing a test solution and a series of concentration standard working solutions, injecting the solutions into a gas chromatography-mass spectrometer, measuring the peak area of a quantitative ion, and calculating the content of phthalate substances according to the peak area of the quantitative ion by an external standard method;
the chromatographic conditions are as follows:
a chromatographic column: agilent HP-5MS (30m is multiplied by 250 mu m is multiplied by 0.25 mu m), helium is taken as carrier gas in the instrument, the linear flow rate is 1mL/min, the temperature of a sample inlet is 280 ℃, split-flow sample injection is not carried out, the sample injection amount is 1 mu L, the solvent cutting time is 7min, the temperature raising program is set to be 60 ℃ at the initial temperature, the temperature is maintained for 1min, the temperature is raised to 220 ℃ at the rate of 20 ℃/min, the temperature is maintained for 1min, the temperature is raised to 260 ℃ at the rate of 5 ℃/min, and the temperature is maintained. Finally, the temperature is increased to 300 ℃ at the speed of 10 ℃/min, and the temperature is kept for 3 min;
mass spectrum conditions:
the ion source type is electron impact source (EI), and the ionization energy is: 70 eV; the ion source temperature and the interface temperature are both 280 ℃, and the quadrupole rod temperature is 150 ℃; the scanning mode is SIM; data acquisition was performed using a Selective Ion Monitoring (SIM) mode, with SIM parameters as shown in table 1.
Table 118 PAEs basic information and monitoring parameters
Example 2 detection of the content of phthalate in the inner packaging case of self-heating chafing dish
1. Preparation of test solution
1) Adding 100% isooctane into a self-heating hot pot packaging box, wherein the volume of the food simulant is 2/3, and heating for 20min according to the heating process of the self-heating hot pot to obtain a food simulant solution;
2) taking 1g (accurate to 0.1mg) of the 100% isooctane food simulation solution obtained in the step 1), accurately adding 2mL of n-hexane into a 10mL colorimetric tube, carrying out vortex oscillation for 10min to fully and uniformly mix the solution, carrying out ultrasonic treatment for 10min at 40 ℃ in a water bath, centrifuging for 5min at 4000r/min, collecting supernate, and filtering the supernate through a 0.22 mu m Nylon filter membrane to obtain a test solution;
2. preparation of Standard solutions
Accurately weighing 0.03491g of diallyl phthalate standard substance into a 10mL volumetric flask, dissolving with n-hexane for constant volume to obtain 3.425mg/mL diallyl phthalate standard stock solution, accurately transferring 150 mu L of diallyl phthalate standard stock solution, keeping the n-hexane constant volume to 50mL, and uniformly oscillating to obtain 10.275 mu g/mL diallyl phthalate standard intermediate solution;
accurately transferring 1.0mL of 17 phthalate mixed standard substances, diluting the normal hexane to 100mL, and uniformly oscillating to obtain 17 phthalate mixed standard intermediate solution of 10 mu g/mL;
accurately transferring 5, 20, 100, 200, 400 and 500 mu L of 17 phthalate mixed standard intermediate liquid with the concentration of 10 mu g/mL and 10.275 mu g/mL diallyl phthalate standard intermediate liquid respectively, and using normal hexane to fix the volume to 1.0mL to prepare the phthalate mixed standard with the concentrations of 17 phthalate: 0.05, 0.2, 1.0, 2.0, 4.0 and 5.0 μ g/mL, and diallyl phthalate concentrations were: 0.05138, 0.2055, 1.028, 2.055, 4.11 and 5.138 μ g/mL of mixed-series concentration standard working solutions;
3. respectively absorbing a test solution and a series of concentration standard working solutions, injecting the solutions into a gas chromatography-mass spectrometer, measuring the peak area of a quantitative ion, and calculating the content of phthalate substances according to the peak area of the quantitative ion by an external standard method;
the chromatographic conditions are as follows:
a chromatographic column: agilent HP-5MS (30m is multiplied by 250 mu m is multiplied by 0.25 mu m), helium is taken as carrier gas in the instrument, the linear flow rate is 1mL/min, the temperature of a sample inlet is 280 ℃, split-flow sample injection is not carried out, the sample injection amount is 1 mu L, the solvent cutting time is 7min, the temperature raising program is set to be 60 ℃ at the initial temperature, the temperature is maintained for 1min, the temperature is raised to 220 ℃ at the rate of 20 ℃/min, the temperature is maintained for 1min, the temperature is raised to 260 ℃ at the rate of 5 ℃/min, and the temperature is maintained. Finally, the temperature is increased to 300 ℃ at the speed of 10 ℃/min, and the temperature is kept for 3 min;
mass spectrum conditions:
the ion source type is electron impact source (EI), and the ionization energy is: 70 eV; the ion source temperature and the interface temperature are both 280 ℃, and the quadrupole rod temperature is 150 ℃; the scanning mode is SIM; data acquisition was performed using a Selective Ion Monitoring (SIM) mode, with SIM parameters as shown in table 1.
The advantageous effects of the present invention are described below by way of test examples.
Test example 1 methodology verification of detection of 18 phthalates in self-heating chafing dish packaging inner box
Gas chromatography/mass spectrometer (Agilent 7890B/5977A, Agilent, USA); electronic balance (ME204E, METTLER TOLEDO, switzerland), column: agilent HP-5MS (30 m.times.250. mu.m.times.0.25 μm), vortex stirrer (IKA, Germany), high speed refrigerated centrifuge (Sigma, USA).
17 phthalate compound standards from DIKMA; diallyl phthalate standard, available from MANHAGE corporation; n-hexane, chromatographically pure, from Merck, germany; ultra pure water machines (Milli-Q, Millipore, USA); the total number of commercial self-heating convenient chafing dish products is 182, and the material of the inner box is Polypropylene (PP): PP white, PP transparent color, PP orange and aluminum foil.
Second, preparation of standard solution
Diallyl phthalate standard stock solution (3.425 mg/mL): 0.03491g of diallyl phthalate standard substance is accurately weighed in a 10mL volumetric flask, and dissolved by n-hexane to a constant volume.
Diallyl phthalate standard intermediate (10.275. mu.g/mL): accurately transferring 150 mu L of diallyl phthalate standard stock solution (3.425mg/mL), diluting normal hexane to 50mL, and shaking and mixing uniformly.
17 phthalate ester mixed standard intermediate solutions (10. mu.g/mL): accurately transferring 1.0mL of 17 phthalate mixed standard products, diluting normal hexane to 100mL, and shaking and uniformly mixing.
Standard curve for 18 phthalate blends: accurately transferring 5, 20, 100, 200, 400 and 500 mu L of 17 phthalate mixed standard intermediate solution (10 mu g/mL) and diallyl phthalate standard intermediate solution (10.275 mu g/mL) respectively, and diluting to 1.0mL by using normal hexane to prepare the phthalate mixed standard solutions with the concentration of 17 phthalate: 0.05, 0.2, 1.0, 2.0, 4.0 and 5.0 μ g/mL, and diallyl phthalate concentrations were: 0.05138, 0.2055, 1.028, 2.055, 4.11, and 5.138 μ g/mL of mixed series concentrations of standard working solutions.
Third, Experimental methods
1. Sample pretreatment
The method comprises the following steps of extracting phthalate ester substances from 182 batches of self-heating type hot pot packaging box samples:
respectively adding food simulants (acetonitrile, isooctane, petroleum ether and 10% ethanol) with the volume being 2/3 of the volume of the packaging box into the packaging box, gradually heating the sample from the initial temperature to 120 ℃ (the highest contact temperature actually used by the commercial self-heating chafing dish) according to the heating process of the self-heating chafing dish, and maintaining for 20min to respectively obtain food simulant solutions;
weighing 1g (accurate to 0.1mg) of food simulation solution in a 10mL colorimetric tube, accurately adding 2mL of n-hexane, carrying out vortex oscillation for 10min to fully disperse the sample, carrying out ultrasonic treatment for 10min at 40 ℃ in a water bath to fully extract the target compound, centrifuging for 5min at 4000r/min, collecting supernatant, and passing the supernatant through a 0.22 mu m Nylon filter membrane for GC-MS analysis;
2. conditions of instrumental analysis
Gas chromatography conditions: an Agilent HP-5MS chromatographic column (30m is multiplied by 250 mu m is multiplied by 0.25 mu m), helium is taken as a carrier gas in the instrument, the linear flow rate is 1mL/min, the temperature of a sample inlet is 280 ℃, split-flow sample injection is not carried out, the sample injection amount is 1 mu L, the solvent cutting time is 7min, the temperature raising program is set to be 60 ℃ at the initial temperature, the temperature is maintained for 1min, the temperature is raised to 220 ℃ at 20 ℃/min, the temperature is maintained for 1min, and then the temperature is raised to 260 ℃ at 5 ℃/min and the temperature is maintained for 0 min. Finally, the temperature is increased to 300 ℃ at the speed of 10 ℃/min and is kept for 3 min.
Mass spectrum conditions: the ion source type is electron impact source (EI), and the ionization energy is: 70 eV; the ion source temperature and the interface temperature are both 280 ℃, and the quadrupole rod temperature is 150 ℃; the scanning mode is SIM. Data acquisition is performed in a Selective Ion Monitoring (SIM) mode.
Fourth, result and discussion
1. Sample pretreatment and optimization of instrument conditions
The box in the self-heating chafing dish packing of market is mostly PP material, and few high-end brand is the aluminium foil material, and target object PAEs is lipophilic low volatility compound, utilizes the similar principle of dissolving mutually to extract, refers to the current report and directly uses n-hexane to extract, finds that PP material cutlery box sample caking in the extraction process, so the experiment compares 10% ethanol, acetonitrile, isooctane, the extraction effect of 4 kinds of extraction solvents of petroleum ether. Experiments show that the background value of DBP in petroleum ether is higher than the quantitative limit of the method, the impurity peak of an acetonitrile extraction sample influences the accuracy of subsequent experiments, the solubility of isooctane to water-soluble impurities is poor, and the interference of a sample matrix is less, so that isooctane and 10% ethanol are finally selected as extraction solvents.
In the further extraction process of adding n-hexane, the vortex oscillation can not completely disperse the food simulation solution isooctane or 10% ethanol, the water bath heating function is opened from 5min to 10min to 40 ℃ after the ultrasonic extraction is prolonged, the extraction effect can be better through ultrasonic waves in the ultrasonic process, meanwhile, the temperature of the extraction liquid is improved through proper water bath heating assistance, the viscosity of the solution is reduced, the solution is easy to disperse, the extraction efficiency is effectively enhanced, but the extraction liquid is turbid and not easy to filter after ultrasonic treatment, so that the centrifugal treatment is selected to replace automatic sedimentation clarification.
PAEs have isomeric structures and high boiling points and are volatile, aiming at the separation by using a weak polarity chromatographic column HP-5MS, the baseline separation of 18 target objects can be perfectly realized, the sensitivity is improved by an SIM scanning mode, most of matrix interference can be well eliminated, the qualitative and quantitative analysis of the target objects is realized, and the specific separation condition is shown in figure 1.
2. Linear range and quantitative limit
Under the optimized experimental conditions in the early period, 18 PAEs standard solutions analyzed by GC-MS are used for quantification by an external standard method. And (3) taking the mass concentration of each compound as an abscissa and the corresponding quantitative ion peak area as an ordinate to prepare a standard curve, thereby obtaining a linear equation of 18 PAEs.
The results show that: all 18 PAEs showed good linear relationship and correlation coefficient (R)2) Are all greater than 0.999. The linear range is 0.05-5.14. mu.g/mL. The corresponding substance content when the response signal is more than 3 times of the noise is taken as the detection limit, the corresponding substance content when the response signal is more than 10 times of the noise is taken as the quantitative limit, the detection limit of each substance method is between 0.005 and 0.02 mu g/L, and the quantitative limit is between 0.02 and 0.04 mu g/L, which shows that the method has higher sensitivity. See table 2 for details.
Linear relationship and method detection limits for the 218 PAEs
3. Recovery and precision
18 PAEs were added to each of the 10% ethanol and 100% isooctane simulant solutions at 3 different concentration levels, 0.05. mu.g, 0.5. mu.g and 1. mu.g, and the process recovery and precision were obtained by repeating 6 experiments at each spiked level (see Table 3). The results show that the recovery rate of the method for 18 substances in 10% ethanol solution is 92.0-99.5%, and the Relative Standard Deviation (RSD) is 0.32-0.99%; the recovery rate of 18 substances in 100 percent isooctane solution is 95.9 to 99.6 percent, and the Relative Standard Deviation (RSD) is 0.77 to 2.23 percent. The method is proved to meet the trace analysis requirement.
Table 318 PAEs with standard recovery and precision (n ═ 6)
In conclusion, the method for detecting the content of the phthalate in the self-heating hot pot packaging inner box has the advantages of better universality and specificity, high sensitivity, convenience in operation and moderate analysis time, provides effective guarantee for the quality control of the phthalate in the self-heating hot pot packaging inner box, ensures the food safety and has good application prospect.
Claims (10)
1. A preparation method of a sample solution for detecting phthalate substances in an inner box of a self-heating hot pot package is characterized by comprising the following steps: it comprises the following steps:
1) adding a food simulant with the capacity of 2/3-3/4 into a self-heating hot pot packaging box, and heating for 15-30 min according to the heating process of the self-heating hot pot to obtain a food simulant solution;
2) and (2) adding n-hexane into the food simulation solution obtained in the step 1), uniformly mixing, performing ultrasonic extraction, centrifuging, and filtering supernatant to obtain the food simulation solution.
2. The configuration method according to claim 1, wherein: step 1), the adding amount of the food simulant is 2/3 of the volume of the self-heating hot pot packaging box; the heating is carried out for 15 min.
3. The configuration method according to claim 1 or 2, characterized in that: the food simulant in the step 1) is 10-20% of ethanol or 90-100% of isooctane, preferably 10% of ethanol or 100% of isooctane.
4. The configuration method according to claim 1, wherein: and 2) the mass volume ratio of the food simulation solution to n-hexane is 0.5-1.5 g: 2ml, preferably 1 g: 2 ml.
5. The configuration method according to claim 1, wherein: the ultrasonic extraction time is 10min, and the temperature is 40 ℃.
6. The configuration method according to claim 1, wherein: the centrifugation time is 10min, and the speed is 4000 r/min; the filtration was performed with a 0.22 μm filter.
7. A method for detecting the content of phthalate substances in an inner packaging box of a self-heating hot pot is characterized by comprising the following steps: it comprises the following steps:
a. test solution: taking the test sample solution obtained in claim 1 as a test solution;
b. standard working solutions of series concentration: taking diallyl phthalate standard substance and 17 phthalate mixed standard substances, adding n-hexane for dissolving, and diluting into a series of concentration standard working solutions;
c. respectively absorbing a test solution and a series of concentration standard working solutions, injecting the solutions into a gas chromatography-mass spectrometer, measuring peak areas, and calculating the content of phthalate substances according to the peak areas by an external standard method;
the chromatographic conditions are as follows:
a chromatographic column: taking (5% -phenyl) -methyl polysiloxane as a filling agent, keeping the initial column temperature at 60 ℃ at the injection inlet temperature of 280 ℃, keeping the initial column temperature for 1min, heating to 220 ℃ at the speed of 20 ℃/min, keeping the initial column temperature for 1min, heating to 260 ℃ at the speed of 5 ℃/min, and keeping the initial column temperature for 0 min; finally, the temperature is increased to 300 ℃ at the speed of 10 ℃/min, and the temperature is kept for 3 min;
the mass spectrum conditions are as follows: the ion source is an electron bombardment source; the mass spectrometry monitoring mode is a selective ion monitoring mode.
8. The detection method according to claim 7, characterized in that: the diallyl phthalate concentration of the series of concentration standard working solutions is 0.05138-5.138 mug/mL, and the concentration of the 17 phthalate mixed standard solution is 0.05-5.0 mug/mL.
9. The detection method according to claim 7, characterized in that: in the chromatographic condition, a chromatographic column is Agilent HP-5MS, the specification of the chromatographic column is 30m multiplied by 250 m multiplied by 0.25 m, carrier gas is helium, the flow rate is 1mL/min, the sample injection mode is non-flow splitting sample injection, the sample injection amount is 1 mu L, and the solvent cutting time is 7 min.
10. The detection method according to claim 7, characterized in that: the ionization energy in the mass spectrometry conditions is: 70eV, the ion source temperature and the interface temperature are both 280 ℃ and the quadrupole rod temperature is 150 ℃.
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| CN110646547A (en) * | 2019-10-16 | 2020-01-03 | 台州科技职业学院 | Method for simultaneously measuring di (2-ethyl) hexyl ortho-, meta-and terephthalate in food simulant |
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| CN104535666A (en) * | 2015-02-11 | 2015-04-22 | 浙江中烟工业有限责任公司 | A method of measuring migration amounts of eighteen phthalic acid esters in a conveyor belt by adopting a gas chromatography-mass spectrometry instrument |
| CN110646547A (en) * | 2019-10-16 | 2020-01-03 | 台州科技职业学院 | Method for simultaneously measuring di (2-ethyl) hexyl ortho-, meta-and terephthalate in food simulant |
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