CN110596292B - Method for detecting organic matters in packaging material - Google Patents
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- CN110596292B CN110596292B CN201810603163.7A CN201810603163A CN110596292B CN 110596292 B CN110596292 B CN 110596292B CN 201810603163 A CN201810603163 A CN 201810603163A CN 110596292 B CN110596292 B CN 110596292B
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- G—PHYSICS
- G01—MEASURING; TESTING
- G01N—INVESTIGATING OR ANALYSING MATERIALS BY DETERMINING THEIR CHEMICAL OR PHYSICAL PROPERTIES
- G01N30/00—Investigating or analysing materials by separation into components using adsorption, absorption or similar phenomena or using ion-exchange, e.g. chromatography or field flow fractionation
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- G—PHYSICS
- G01—MEASURING; TESTING
- G01N—INVESTIGATING OR ANALYSING MATERIALS BY DETERMINING THEIR CHEMICAL OR PHYSICAL PROPERTIES
- G01N30/00—Investigating or analysing materials by separation into components using adsorption, absorption or similar phenomena or using ion-exchange, e.g. chromatography or field flow fractionation
- G01N30/02—Column chromatography
- G01N30/88—Integrated analysis systems specially adapted therefor, not covered by a single one of the groups G01N30/04 - G01N30/86
- G01N2030/8809—Integrated analysis systems specially adapted therefor, not covered by a single one of the groups G01N30/04 - G01N30/86 analysis specially adapted for the sample
- G01N2030/884—Integrated analysis systems specially adapted therefor, not covered by a single one of the groups G01N30/04 - G01N30/86 analysis specially adapted for the sample organic compounds
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- G—PHYSICS
- G01—MEASURING; TESTING
- G01N—INVESTIGATING OR ANALYSING MATERIALS BY DETERMINING THEIR CHEMICAL OR PHYSICAL PROPERTIES
- G01N30/00—Investigating or analysing materials by separation into components using adsorption, absorption or similar phenomena or using ion-exchange, e.g. chromatography or field flow fractionation
- G01N30/02—Column chromatography
- G01N30/88—Integrated analysis systems specially adapted therefor, not covered by a single one of the groups G01N30/04 - G01N30/86
- G01N2030/8809—Integrated analysis systems specially adapted therefor, not covered by a single one of the groups G01N30/04 - G01N30/86 analysis specially adapted for the sample
- G01N2030/884—Integrated analysis systems specially adapted therefor, not covered by a single one of the groups G01N30/04 - G01N30/86 analysis specially adapted for the sample organic compounds
- G01N2030/8854—Integrated analysis systems specially adapted therefor, not covered by a single one of the groups G01N30/04 - G01N30/86 analysis specially adapted for the sample organic compounds involving hydrocarbons
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Abstract
The invention belongs to the technical field of analysis and detection, and particularly relates to a method for detecting organic matters in a packaging material. The invention provides a method for detecting organic matters in a packaging material, which comprises the following steps: detecting a packaging material sample by adopting static headspace balance and gas chromatography-mass spectrometry to obtain gas chromatography data and mass spectrometry data, and obtaining the content of organic matters in the packaging material according to a standard curve of the gas chromatography data of an organic matter standard solution and the mass spectrometry data; the organic matter comprises one or more of pentamethylheptane, n-pentadecane, n-hexadecane and n-heptadecane. The method can simultaneously detect the content of pentamethyl heptane, n-pentadecane, n-hexadecane and n-heptadecane in the packaging material sample, and is simple, convenient, quick, accurate, good in repeatability and high in accuracy.
Description
Technical Field
The invention belongs to the technical field of analysis and detection, and particularly relates to a method for detecting organic matters in a packaging material.
Background
The packaging is a visual introduction of the product and plays a very important role in marketing, and the packaging box of food, cosmetics, cigarettes and the like can influence the first emotion of the consumer. With the continuous improvement of consumer demands and the rapid development of market competition, the appearance of the packaging box is more and more exquisite, and the quality requirement on the appearance is higher and higher.
The packaging box is mainly formed by packaging a BOPP (Biaxially Oriented Polypropylene) film by a packaging material through a packaging machine. The packing boxes are designed by adopting dark packing paper in the market, and the packing boxes are easy to have appearance defects of water mist, namely, substances similar to water mist are generated between the packing materials and the films, so that the haze of the films is increased, the appearance of the packing boxes is not smooth, bright and clean, and the clear feeling is lost, and the quality of the packing boxes and the product sale are influenced.
This "water mist" phenomenon is most likely to occur in offset printed packaging materials, and pentamethylheptane, n-pentadecane, n-hexadecane and n-heptadecane are the main substances of the "water mist" of the packaging box, and are mainly generated by solvent inks on the packaging paper. Whether the packaging material generates the phenomenon of water mist can be judged by detecting the content of pentamethyl heptane, n-pentadecane, n-hexadecane and n-heptadecane in the packaging material, so that the use of ink in the packaging material is improved, and the appearance quality of the packaging box is improved and stabilized. However, at present, no detection method is available for detecting pentamethylheptane, n-pentadecane, n-hexadecane and n-heptadecane in the packaging material.
Disclosure of Invention
In view of the above, the present invention provides a method for detecting organic matters in a packaging material, which is used to solve the problem that no detection method is available to detect pentamethylheptane, n-pentadecane, n-hexadecane and n-heptadecane in the packaging material at present.
The specific technical scheme of the invention is as follows:
a method of detecting organics in a packaging material comprising:
detecting a packaging material sample by adopting static headspace balance and gas chromatography-mass spectrometry to obtain gas chromatography data and mass spectrometry data, and obtaining the content of organic matters in the packaging material according to a standard curve of the gas chromatography data of an organic matter standard solution and the mass spectrometry data;
the organic matter comprises one or more of pentamethylheptane, n-pentadecane, n-hexadecane and n-heptadecane.
Preferably, the equilibrium temperature of the packaging material sample in the static headspace equilibrium is 60 ℃ to 140 ℃;
the static headspace balancing time is 5 min-60 min.
Preferably, the matrix correction agent for static headspace equilibrium is glyceryl triacetate.
The content of each component in the headspace gas is related to the volatility of the headspace gas and the sample matrix, particularly the component with high solubility (large distribution coefficient) in the sample matrix, and the matrix effect is more obvious, namely the composition of the headspace gas is different from that in the original sample, and the adverse effect on quantitative analysis is particularly serious. Therefore, in order to accurately perform quantitative analysis, the matrix of the quantitative analysis sample is selected to be the same as that of the standard solution, and the matrix effect of the sample can be effectively eliminated. In the invention, the matrix correction agent is glyceryl triacetate, so that the matrix effect of the packaging material sample can be effectively eliminated.
Preferably, the gas chromatography-mass spectrometry conditions are as follows:
the chromatographic column of the gas chromatography is an HP-5 chromatographic column or a chromatographic column equivalent to the HP-5 chromatographic column;
the mobile phase of the gas chromatographic column is helium;
the flow rate of the mobile phase is 0.6 mL/min-1.2 mL/min.
Preferably, the gas chromatography-mass spectrometry further comprises the following conditions:
the temperature of a sample inlet of the gas chromatograph is 140-200 ℃;
the gas chromatography is in a constant-current mode;
the gas chromatography has a split ratio of (5-50): 1.
preferably, the gas chromatography-mass spectrometry gas chromatography detection adopts temperature programming;
the temperature programming is as follows:
keeping the initial temperature at 30-60 ℃ for a first time, wherein the first time is 0-10 min;
heating to a second temperature at a first heating rate, wherein the first heating rate is 0-10 ℃/min, the second temperature is 70-180 ℃, and the second time is 0-10 min, and keeping the temperature for a second time;
and heating to a third temperature at a second heating rate of 10-30 ℃/min, keeping the temperature for a third time, wherein the third temperature is 190-250 ℃, and the third time is 0-10 min.
Preferably, the conditions of mass spectrometry in gas chromatography-mass spectrometry comprise:
the temperature of the transmission line of the mass spectrum is 200-260 ℃;
the ion source temperature of the mass spectrum is 220-280 ℃;
the solvent delay of the mass spectrum is 2 min-10 min.
Preferably, the conditions of the mass spectrum further include:
the ionization mode of the mass spectrum is EI;
the ionization energy of the mass spectrum is 70 eV;
the monitoring mode of the mass spectrum is full scanning and selective ion monitoring.
Preferably, the monitoring ions for the selective ion monitoring are 57 and 71.
Preferably, the standard curve is established according to the following steps:
detecting the organic matter standard solution through gas chromatography-mass spectrometry, recording the peak area of the organic matter, and establishing a standard curve according to the response value of the organic matter and the concentration of the organic matter standard solution.
Preferably, the solvent of the organic standard solution is triacetin.
Preferably, the detection limit of the pentamethyl heptane is 0.005 mu g/mL;
the detection limit of the n-pentadecane is 0.018 mu g/mL;
the detection limit of the n-hexadecane is 0.102 mu g/mL;
the detection limit of n-heptadecane was 0.262. mu.g/mL.
In summary, the present invention provides a method for detecting organic substances in a packaging material, including: detecting a packaging material sample by adopting static headspace balance and gas chromatography-mass spectrometry to obtain gas chromatography data and mass spectrometry data, and obtaining the content of organic matters in the packaging material according to a standard curve of the gas chromatography data of an organic matter standard solution and the mass spectrometry data; the organic matter comprises one or more of pentamethylheptane, n-pentadecane, n-hexadecane and n-heptadecane. The method can simultaneously detect the content of pentamethyl heptane, n-pentadecane, n-hexadecane and n-heptadecane in the packaging material sample, and is simple, convenient, quick, accurate, good in repeatability and high in accuracy.
Drawings
In order to more clearly illustrate the embodiments of the present invention or the technical solutions in the prior art, the drawings used in the description of the embodiments or the prior art will be briefly described below.
FIG. 1 is the peak areas of the response chromatogram of the organic substance at different equilibrium times in static headspace equilibrium according to the present invention;
FIG. 2 is the peak area of the response chromatogram of the organic material at different equilibrium temperatures in the static headspace equilibrium of the present invention;
FIG. 3 is a selection chromatogram of pentamethylheptane, n-pentadecane, n-hexadecane and n-heptadecane in the standard sample (A) and the wrapping paper (B).
Detailed Description
The invention provides a method for detecting organic matters in a packaging material, which is used for solving the problem that no detection method is available for detecting pentamethyl heptane, n-pentadecane, n-hexadecane and n-heptadecane in the packaging material at present.
The technical solutions in the embodiments of the present invention will be clearly and completely described below, and it is obvious that the described embodiments are only a part of the embodiments of the present invention, and not all 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.
Example 1
In this example, the static headspace equilibrium was followed by gas chromatography-mass spectrometry using different equilibration times.
Wherein the static headspace balance conditions are as follows:
sample equilibrium temperature: 110 ℃; sample ring temperature: 120 ℃; transmission line temperature: l40 deg.C; sample bottle pressurization pressure: 35 psi; carrier gas pressure: 40 psi; pressurizing time: 2.0 min; and (3) inflation time: 0.20 min; sample loop equilibration time: 0.05 min; sample introduction time: 0.1 min.
The conditions of the gas chromatography were as follows:
and (3) chromatographic column: HP-5 capillary column (30 m.times.0.32 mm.times.0.25 μm); furnace temperature: initially 50 deg.C (2min), 5 deg.C/min to 150 deg.C (1min), then 10 deg.C/min to 240 deg.C (3 min); sample inlet temperature: 150 ℃, split ratio: 10: 1; carrier gas: high-purity helium with the purity more than or equal to 99.999 percent; constant flow mode, column flow: 1.0 mL/min.
Temperature rising procedure: the initial temperature is 50 ℃, the temperature is kept for 2min, the temperature is increased to 150 ℃ at the temperature rising speed of 5 ℃/min, the temperature is kept for 1min, the temperature is increased to 240 ℃ at the temperature rising speed of 10 ℃/min, and the temperature is kept for 3 min;
the conditions of the mass spectrum were as follows:
EI ionization energy: 70 eV; ion source temperature: 230 ℃; transmission line: 250 ℃; solvent retardation: 5.0 min; the scanning mode is as follows: full scan, scan range 29-500 aeu; ion Monitoring (SIM) was selected, with the monitored ions 57 and 71.
Adding 100 mu L of pentamethylheptane, n-pentadecane, n-hexadecane and n-heptadecane standard solutions with the concentrations of 0.94mg/mL, 0.81mg/mL, 0.80mg/mL and 1.75mg/mL into base paper, adding 1mL of glyceryl triacetate, carrying out gas chromatography-mass spectrometry on static headspace equilibrium by adopting different equilibrium times (5min, 10min, 15min, 30min, 40min and 60min), and obtaining a result, referring to a graph 1, which is a peak area of a response chromatogram of an organic matter in the static headspace equilibrium of the invention under different equilibrium times. FIG. 1 shows that peak areas of response chromatograms of target compounds of pentamethylheptane, n-pentadecane, n-hexadecane and n-heptadecane tend to rise in the equilibrium time of 5min to 30 min; the peak area of a response chromatogram of pentamethyl heptane is reduced between 30min and 60min, n-pentadecane and n-heptadecane slightly fluctuate, and n-hexadecane hardly changes. In the embodiment of the invention, the temperature programming time of the chromatogram is 35min, and the balance time is optimally 30 min.
Example 2
In this example, the static headspace equilibrium was determined by gas chromatography-mass spectrometry using different equilibrium temperatures.
Wherein the static headspace balance conditions are as follows:
sample equilibration time: 30 min; sample ring temperature: 120 ℃; transmission line temperature: l40 deg.C; sample bottle pressurization pressure: 35 psi; carrier gas pressure: 40 psi; pressurizing time: 2.0 min; and (3) inflation time: 0.20 min; sample loop equilibration time: 0.05 min; sample introduction time: 0.1 min.
The conditions of the gas chromatography were as follows:
a chromatographic column: HP-5 capillary column (30 m.times.0.32 mm.times.0.25 μm); furnace temperature: initially 50 deg.C (2min), 5 deg.C/min to 150 deg.C (1min), then 10 deg.C/min to 240 deg.C (3 min); sample inlet temperature: 150 ℃, split ratio: 10: 1; carrier gas: high-purity helium with the purity more than or equal to 99.999 percent; constant flow mode, column flow: 1.0 mL/min.
Temperature rising procedure: the initial temperature is 50 ℃, the temperature is kept for 2min, the temperature is increased to 150 ℃ at the temperature rising speed of 5 ℃/min, the temperature is kept for 1min, the temperature is increased to 240 ℃ at the temperature rising speed of 10 ℃/min, and the temperature is kept for 3 min;
the conditions of the mass spectrum were as follows:
EI ionization energy: 70 eV; ion source temperature: 230 ℃; transmission line: 250 ℃; solvent retardation: 5.0 min; the scanning mode is as follows: full scan, scan range 29-500 aeu; ion Monitoring (SIM) was selected, with the monitored ions 57 and 71.
Adding 100 mu L of pentamethylheptane, n-pentadecane, n-hexadecane and n-heptadecane standard solutions with the concentrations of 0.94mg/mL, 0.81mg/mL, 0.80mg/mL and 1.75mg/mL into base paper, adding 1mL of glyceryl triacetate, balancing for 30min, and performing gas chromatography-mass spectrometry on static headspace equilibrium at different balancing temperatures (60 ℃, 80 ℃, 100 ℃, 110 ℃, 120 ℃ and 140 ℃), wherein the result is shown in figure 1, which is the peak area of a response chromatogram of an organic substance at different balancing temperatures in the static headspace equilibrium of the invention. FIG. 2 shows that at an equilibrium temperature of 60 ℃ and 80 ℃, n-pentadecane, n-hexadecane and n-heptadecane have almost no response; with the increase of the equilibrium temperature, the peak areas of pentamethylheptane, n-pentadecane, n-hexadecane and n-heptadecane gradually increase, when the equilibrium temperature is between 80 and 120 ℃, the peak area acceleration of the target compound is slightly small, and the acceleration is obvious at 120 to 140 ℃. The physical temperature which can be borne by the packaging paper and the working temperature of the packaging machine during packaging are about 110 ℃, and the balance temperature is 110 ℃ optimally.
Example 3
In this example, pentamethylheptane, n-pentadecane, n-hexadecane and n-heptadecane were detected by static headspace equilibrium gas chromatography-mass spectrometry.
Wherein the static headspace balance conditions are as follows:
sample equilibrium temperature: 110 ℃; sample equilibration time: 30 min; sample ring temperature: 120 ℃; transmission line temperature: l40 deg.C; sample bottle pressurization pressure: 35 psi; carrier gas pressure: 40 psi; pressurizing time: 2.0 min; and (3) inflating time: 0.20 min; sample loop equilibration time: 0.05 min; sample introduction time: 0.1 min.
The conditions of the gas chromatography were as follows:
a chromatographic column: HP-5 capillary column (30 m.times.0.32 mm.times.0.25 μm); furnace temperature: initially 50 deg.C (2min), 5 deg.C/min to 150 deg.C (1min), then 10 deg.C/min to 240 deg.C (3 min); sample inlet temperature: 150 ℃, split ratio: 10: 1; carrier gas: high-purity helium with the purity more than or equal to 99.999 percent; constant flow mode, column flow: 1.0 mL/min.
Temperature rising procedure: the initial temperature is 50 ℃, the temperature is kept for 2min, the temperature is raised to 150 ℃ at the temperature rising speed of 5 ℃/min, the temperature is kept for 1min, the temperature is raised to 240 ℃ at the temperature rising speed of 10 ℃/min, and the temperature is kept for 3 min;
the conditions of the mass spectrum were as follows:
EI ionization energy: 70 eV; ion source temperature: 230 ℃; transmission line: 250 ℃; solvent retardation: 5.0 min; the scanning mode is as follows: full scan, scan range 29-500 aeu; ion Monitoring (SIM) was selected, with the monitored ions 57 and 71.
FIG. 3-A shows a chromatogram for the selection of the standard samples pentamethylheptane, n-pentadecane, n-hexadecane and n-heptadecane. Please refer to fig. 3-B, which is a selection chromatogram of pentamethylheptane, n-pentadecane, n-hexadecane and n-heptadecane in the wrapping paper. In FIG. 3, 1 represents pentamethylheptane, 2 represents n-pentadecane, 3 represents n-hexadecane, and 4 represents n-heptadecane. FIGS. 3-A and 3-B show that the HP-5 capillary (30 m.times.0.32 mm.times.0.25 μm) as a chromatographic column can achieve a better baseline separation of the target compounds pentamethylheptane, n-pentadecane, n-hexadecane and n-heptadecane. And the whole separation process was completed in 35 min. The mass spectrum is scanned by selecting ions, and identification information of target compounds such as pentamethylheptane, n-pentadecane, n-hexadecane and n-heptadecane is shown in table 1, and the result shows that when the target compound selects the target ion 57, the target compounds such as pentamethylheptane, n-pentadecane, n-hexadecane and n-heptadecane can obtain better chromatograms.
TABLE 1 identification of target Compounds
Example 4
In this example, the pentamethylheptane, the n-pentadecane, the n-hexadecane and the n-heptadecane were subjected to detection by static headspace equilibrium and gas chromatography-mass spectrometry under the same conditions as in example 3, and a standard curve was established.
Firstly, preparing a standard solution: weighing pentamethylheptane, n-pentadecane, n-hexadecane and n-heptadecane with the mass of 0.0094g, 0.0081g, 0.0080g and 0.0175g respectively, dissolving with glyceryl triacetate, transferring into a 10mL brown volumetric flask respectively, and fixing the volume with the glyceryl triacetate, wherein the mass concentrations of the pentamethylheptane, the n-pentadecane, the n-hexadecane and the n-heptadecane are respectively 0.94mg/mL, 0.81mg/mL, 0.80mg/mL and 1.75 mg/mL.
Then, 5. mu.L, 10. mu.L, 20. mu.L, 50. mu.L, 100. mu.L, 200. mu.L, and 500. mu.L of the standard solutions were measured in a 10mL brown volumetric flask, and a series of standard solutions were prepared by diluting with triacetin to a constant volume. The 7 standard solutions with different concentrations were subjected to static headspace equilibrium and gas chromatography-mass spectrometry, and regression analysis was performed with pentamethylheptane, n-pentadecane, n-hexadecane, and n-heptadecane peak areas as ordinate and corresponding mass concentration X (μ g/mL) as abscissa, and the regression equations for pentamethylheptane, n-pentadecane, n-hexadecane, and n-heptadecane were Y1 ═ 5090.91X (r2 ═ 0.997), Y2 ═ 120.07X (r2 ═ 0.992), Y3 ═ 43.94X (r2 ═ 0.996), and Y4 ═ 9.77X (r2 ═ 0.995), respectively. The detection limits of pentamethylheptane, N-pentadecane, N-hexadecane and N-heptadecane were calculated to be 0.005. mu.g/mL, 0.018. mu.g/mL, 0.102. mu.g/mL and 0.262. mu.g/mL, respectively, with a 3-fold signal-to-noise ratio (S/N. gtoreq.3).
Example 5
In this example, the recovery rate and the repeatability of pentamethylheptane, n-pentadecane, n-hexadecane and n-heptadecane were determined by static headspace equilibrium and gas chromatography-mass spectrometry under the same conditions as in example 3.
Cutting a central area of a main packaging surface of a packaging box with an area of 22.0cm multiplied by 5.5cm, rolling the packaging box into a cylinder shape with a printing surface facing inwards, putting the cylinder into a 20mL headspace bottle, respectively adding 1mL three-gradient standard solutions, wherein the concentrations of pentamethyl heptane, n-pentadecane, n-hexadecane and n-heptadecane in the first gradient standard solution are respectively 0.47 mu g/mL, 0.405 mu g/mL, 0.40 mu g/mL and 0.875 mu g/mL, the concentrations of pentamethyl heptane, n-pentadecane, n-hexadecane and n-heptadecane in the second gradient standard solution are respectively 0.94 mu g/mL, 0.81 mu g/mL, 0.80 mu g/mL and 1.75 mu g/mL, the concentrations of pentamethyl heptane, n-pentadecane, n-hexadecane and n-heptadecane in the third gradient standard solution are respectively 4.70 mu g/mL, 4.05 mu g/mL, 4.00 mu g/mL, 8.75 mu g/mL, static headspace equilibrium and gas chromatography-mass spectrometry are adopted for detection, each concentration is tested for 6 times in parallel, and the recovery rate is calculated according to the measured amount, the additive amount and the original content, and the result is shown in table 2. The result shows that the recovery rate of the target compounds of pentamethylheptane, n-pentadecane, n-hexadecane and n-heptadecane is between 90% and 96.3%, which indicates that the detection method has higher accuracy; the relative standard deviation of the target compounds pentamethylheptane, n-pentadecane, n-hexadecane and n-heptadecane is less than 5%, which shows that the repeatability of the detection method is better.
Table 2 recovery of target compound (n ═ 6)
Example 6
In this example, the contents of pentamethylheptane, n-pentadecane, n-hexadecane and n-heptadecane in the packaging material were determined by static headspace equilibrium and gas chromatography-mass spectrometry, wherein the conditions of static headspace equilibrium and gas chromatography-mass spectrometry were the same as in example 3.
Cutting the central area of the main packaging surface of the packaging box with the area of 22.0cm multiplied by 5.5cm, rolling the printed surface inwards to form a cylinder, putting the cylinder into a 20mL headspace bottle, adding 1mL glyceryl triacetate, sealing and then analyzing on a machine. The contents of pentamethylheptane, n-pentadecane, n-hexadecane and n-heptadecane in the packaging box were determined by detection using static headspace equilibrium and gas chromatography-mass spectrometry, and the results were shown in table 3 by quantitative analysis using an external standard method.
TABLE 3 determination of the target content in 6 pack samples by the method
The foregoing is only a preferred embodiment of the present invention, and it should be noted that, for those skilled in the art, various modifications and amendments can be made without departing from the principle of the present invention, and these modifications and amendments should also be considered as the protection scope of the present invention.
Claims (3)
1. A method of detecting organics in a packaging material, comprising:
detecting a packaging material sample by adopting static headspace balance and gas chromatography-mass spectrometry to obtain gas chromatography data and mass spectrometry data, and obtaining the content of organic matters in the packaging material according to a standard curve of the gas chromatography data of an organic matter standard solution and the mass spectrometry data;
the gas chromatography conditions in the gas chromatography-mass spectrometry are as follows:
the chromatographic column of the gas chromatography is an HP-5 chromatographic column; the mobile phase of the gas chromatograph is helium; the flow rate of the mobile phase is 1.0 mL/min; the sample inlet temperature of the gas chromatography is 150 ℃; the gas chromatography is in a constant-current mode; the gas chromatography split ratio is 10: 1;
the gas chromatography in the gas chromatography-mass spectrum adopts temperature programming;
the temperature programming is as follows: the initial temperature is 50 ℃, the temperature is kept for 2min, the temperature is increased to 150 ℃ at the temperature rising speed of 5 ℃/min, the temperature is kept for 1min, the temperature is increased to 240 ℃ at the temperature rising speed of 10 ℃/min, and the temperature is kept for 3 min;
the temperature rise time of the temperature programming is 35 min;
the conditions of mass spectrum in the gas chromatography-mass spectrum comprise:
the transmission line temperature of the mass spectrum is 250 ℃; the ion source temperature of the mass spectrum is 230 ℃; the solvent delay of the mass spectrum is 5.0 min; the ionization mode of the mass spectrum is EI; the ionization energy of the mass spectrum is 70 eV; the monitoring mode of the mass spectrum is full scanning; selecting the monitoring ions for ion monitoring as 57 and 71;
the organic matter comprises pentamethyl heptane, n-pentadecane, n-hexadecane and n-heptadecane;
the balance temperature of the packaging material sample in the static headspace balance is 110 ℃, the balance time of the packaging material sample in the static headspace balance is 30min, the temperature of a sample ring is 120 ℃, the temperature of a transmission line is l40 ℃, the pressurizing pressure of a sample bottle is 35psi, the pressure of carrier gas is 40psi, the pressurizing time is 2.0min, the inflating time is 0.20min, the balance time of the sample ring is 0.05min, and the sample injection time is 0.1 min.
2. The method of claim 1, wherein the static headspace equilibrium matrix correction agent is glyceryl triacetate.
3. The method of claim 1, wherein the standard curve is established according to the following steps:
detecting the organic matter standard solution through gas chromatography-mass spectrometry, recording the peak area of the organic matter, and establishing a standard curve according to the response value of the organic matter and the concentration of the organic matter standard solution.
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| US3969196A (en) * | 1963-04-16 | 1976-07-13 | Studiengesellschaft Kohle M.B.H. | Process for the separation of mixtures of substances |
| CN106168611A (en) * | 2016-10-10 | 2016-11-30 | 国家烟草质量监督检验中心 | The assay method of VOC in a kind of quick-fried pearl |
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