CN101625342A - Method for detecting polycyclic aromatic hydrocarbon in food contact material by gas chromatogram-mass spectrometry coupling technique - Google Patents
Method for detecting polycyclic aromatic hydrocarbon in food contact material by gas chromatogram-mass spectrometry coupling technique Download PDFInfo
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- CN101625342A CN101625342A CN200910043464A CN200910043464A CN101625342A CN 101625342 A CN101625342 A CN 101625342A CN 200910043464 A CN200910043464 A CN 200910043464A CN 200910043464 A CN200910043464 A CN 200910043464A CN 101625342 A CN101625342 A CN 101625342A
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Abstract
The invention provides a method for detecting polycyclic aromatic hydrocarbon in food contact material by gas chromatogram-mass spectrometry coupling technique, comprising: Soxhlet extraction method or ultrasonic extraction method is used for extracting the detected food contact material; the extract sample is detected by a gas chromatogram-mass spectrometry coupling instrument; the temperature of a sample inlet of the instrument is set to be 240-320 DEG C, and the flow rate of carrier gas is set to be 0.5-2.0ml/min; a weakly polar chromatographic column is adopted, and the interface temperature is set to be 180-300 DEG C; the pretreated sample enters into the chromatographic column through the sample inlet of the instrument for temperature programming, and the temperature is raised to be 270-330 DEG C from 70-100 DEG C; after being separated by the chromatographic column, all the components in the sample are detected by mass spectrum. The method has the characteristics of low price of the detection instrument, safety, accurate and rapid analysis method and little interference as well as being suitable for standard analysis and detection which can lead all the components of the polycyclic aromatic hydrocarbon in the sample to be cracked in a mass spectrum ion source and optimize all the components of the cracked product, etc.
Description
Technical field
The present invention relates to a kind of detection method of palycyclic aromatic, particularly relate to method by palycyclic aromatic in the gas chromatography-mass spectrography technology for detection food contact material.
Background technology
Palycyclic aromatic (polycyclic aromatic hydrocarbons, PAHs) be meant the compound of arranging with wire, horn shape or bunch shape by two or more phenyl ring, comprising kind of compound surplus naphthalene, anthracene, phenanthrene, the pyrene etc. 150, is a ubiquitous class chemical carcinogen and environmental contaminants in the present environment.Palycyclic aromatic has bio-refractory and cumulative bad, and its most outstanding characteristics are carcinogenic, teratogenesis and mutagenicity, and carcinogenicity increases along with the increase of phenyl ring number.Confirmed naphthalene, acenaphthylene, acenaphthene, fluorenes, phenanthrene, anthracene, fluoranthene, pyrene, benzo (a) anthracene at present, bent, benzo (b) fluoranthene, benzo (k) fluoranthene, benzo (a) pyrene, indeno (1,2,3-cd) pyrene, dibenzo (a, h) anthracene and benzo (g, h, i) these 16 kinds of palycyclic aromatics of perylene are high carcinogenic, aberration inducing, mutagenic material, so U.S. environment administration classifies these 16 kinds of materials as pollutant that emphasis detects.94 kinds of listing of IARC (IARC) (1976) in the carcinogenic compound of animal used as test 15 kinds belong to palycyclic aromatic, because benzo (a) pyrene is first found environmental chemical carcinogen, and carcinogenicity is very strong, so often with the representative of benzo (a) pyrene (BaP) as palycyclic aromatic, it accounts for 1%～20% of whole carcinogenicity palycyclic aromatics.
Food contact material, for example the wrappage of some other and Food Contact of preservative film, crisper and mainly are some plastic products, plastic products be palycyclic aromatic important have a carrier, the main cause that comprises polycyclic aromatic hydrocarbon pollutant in these materials has been to use: be subjected to polycyclic aromatic hydrocarbons contaminated rubber softening oil and nonrigid plastic, be subjected to polycyclic aromatic hydrocarbons contaminated rubber and the black toner in the plastics or be subjected to polycyclic aromatic hydrocarbons contaminated paint etc.; In addition, the naphthalene as transportation or storage anti-corrosion material also is the one of the main reasons that comprises polycyclic aromatic hydrocarbon pollutant in these materials.U.S. environment administration and experience exchangement office of German safety technique authentication center research back regulation: should detect with benzo (a) pyrene in the material that food contacts (＜0.2mg/kg), other 15 palycyclic aromatics of being paid close attention to of while also should detect (＜0.2mg/kg).
At present, the conventional sense method of palycyclic aromatic is a high performance liquid chromatography, and its separation method mostly is the gradient elution method greatly.The national standard of China is the gradient elution of first alcohol and water, and external method is the gradient elution of acetonitrile and water, although above-mentioned two kinds of methods can realize the separation of palycyclic aromatic, its shortcoming is analysis time long (national standard of China is 60min), and has the problem of baseline wander.Also can analyse fluorophotometric method, fluorescence spectrophotometry or capillary column gas chromatography method in addition and wait and detect palycyclic aromatic, but have characteristics such as detection sensitivity is low, qualitative, quantitative weak effect by thin-layer chromatography fluorophotometric method, ply of paper.
Summary of the invention
The technical problem to be solved in the present invention is to avoid the weak point of above-mentioned technology and proposes the detection method of the palycyclic aromatic of a kind of gas chromatography-mass spectrography technology by routine in can qualitative exactly, quantitative food contact material.This method is the effective means of Analysis of Complex potpourri, the high score that can utilize chromatogram simultaneously is from ability and mass spectral high sensitivity identification capacity, has inexpensive, the safety of detecting instrument, analytical approach is accurate, quick, interference is little, be suitable for standardization, can make palycyclic aromatic in the sample in mass ion source generation cracking and make each component of pyrolysis product carry out characteristics such as optimized analyzing and testing.
The method of palycyclic aromatic comprises the steps in the gas chromatography-mass spectrography technical measurement food contact material that the present invention proposes,
1. utilize soxhlet extraction or ultrasonic extraction method that the food contact material that is detected is extracted, obtain detection solution to be analyzed;
2. gas chromatograph-mass spectrometer (GCMS) is set: injector temperature is 240 ℃～320 ℃, and flow rate of carrier gas is made as 0.5 ml/min～2.0 ml/min, and chromatographic column is selected low-pole column, and interface temperature is 180 ℃～300 ℃;
3. the injection port of test sample by described gas chromatograph-mass spectrometer (GCMS) entered in the chromatographic column, carry out temperature programme,, be warming up to 270 ℃～330 ℃ since 70 ℃～100 ℃, each component in the solution to be detected is separated by chromatographic column, and determines each component concentration;
4. separated sample each component enters Mass Spectrometer Method and partly carries out Mass Spectrometer Method, determines each component structure; The ion gun of described Mass Spectrometer Method adopts electron bombardment ionization source.
Use alkanes, alkyl chloride hydro carbons, alcohols, ketone or benzene kind solvent during the 1. described extraction of step; Preferred normal hexane or toluene.
When 1. step used soxhlet extraction, extraction time was 8 hours～24 hours, preferred 12-24 hour.
When 1. step used the ultrasonic extraction method, extraction time was 1 hour～5 hours, preferred 1-3 hour.
Step 3. in, the mode of described temperature programme is, since 70 ℃～100 ℃, is warming up to 120 ℃～180 ℃ with 10 ℃～30 ℃/minute speed, keeps 0～10 minute; And then be warming up to 270 ℃～330 ℃ with 5 ℃～20 ℃/minute speed, kept 10～20 minutes.
The step 4. ion gun bombarding energy of described Mass Spectrometer Method is 70eV, and ion source temperature is set at 230 ℃～300 ℃.
Palycyclic aromatic in the above-mentioned food contact material comprises naphthalene, acenaphthylene, acenaphthene, fluorenes, phenanthrene, anthracene, fluoranthene, pyrene, benzo (a) anthracene, bends, benzo (b) fluoranthene, benzo (k) fluoranthene, benzo (a) pyrene, indeno (1,2,3-cd) pyrene, dibenzo (a, h) anthracene and benzo (g, h, i) perylene.
The method of utilizing this gas chromatograph-mass spectrometer (GCMS) to detect detects and is limited to 0.03mg/kg, and quantitative limit reaches 0.10mg/kg.
By selecting suitable chromatographic column, control suitable injector temperature, chromatogram column temperature and interface temperature, set suitable flow rate of carrier gas, can make palycyclic aromatic in the different food products contact material in mass ion source generation cracking and make each component of pyrolysis product carry out optimized analyzing and testing.
Adopt the palycyclic aromatic of gas chromatography-mass spectrography technology GC-MS of the present invention (EI source) ionization in can qualitative exactly, quantitative different food products contact material, inexpensive, the safety of instrument; Compare conventional high performance liquid chromatography and other certain methods, a kind of detection method that is suitable for the palycyclic aromatic in the different food products contact material is provided, analytical approach is accurate, quick, interference is little, is suitable for standardization.
Description of drawings
Fig. 1 a is the chromatogram of the palycyclic aromatic standard solution that detected of the embodiment of the invention 1, and the ordinate in this chromatogram is represented the intensity at peak, and horizontal ordinate is represented retention time, and unit is minute;
Naphthalene in the palycyclic aromatic that the embodiment of the invention 1 that is respectively Fig. 1 b-1q is detected, acenaphthylene, acenaphthene, fluorenes, phenanthrene, anthracene, fluoranthene, pyrene, benzo (a) anthracene, bend, benzo (b) fluoranthene, benzo (k) fluoranthene, benzo (a) pyrene, indeno (1,2,3-cd) pyrene, dibenzo (a, h) anthracene and benzo (g, h, i) mass spectrogram of perylene pyrolysis product, the ordinate in the mass spectrogram is represented the relative abundance of ion, and horizontal ordinate is represented the numerical value of ion mass-to-charge ratio;
Fig. 2 is the uncertainty source analysis of the embodiment of the invention 2 testing processes.
Embodiment
Experiment condition: GC (7890)-MS (5975C) type gas chromatograph-mass spectrometer (GCMS) of using the production of Agilent company detects, and agents useful for same is chromatographically pure, the DB-5MS type chromatographic column that chromatographic column selects for use Agilent company to produce.The injector temperature of gas chromatograph-mass spectrometer (GCMS) is set at 240～320 ℃, and interface temperature is set at 180～300 ℃; Carrier gas is a helium, and flow velocity is 0.5～2.0 ml/min; The pattern of temperature programme is adopted in chromatogram column temperature control, since 70～100 ℃, is warming up to 120～180 ℃ with 10～30 ℃/minute speed, keeps 0～10 minute; And then be warming up to 270～330 ℃ with 5～20 ℃/minute speed, kept 10～20 minutes; The ion gun of Mass Spectrometer Method adopts electron bombardment ionization source (EI source), and the ion gun bombarding energy is 70eV, and ion source temperature is set at 230～300 ℃; Sample size 1～2 microlitre.Computer system record chromatogram and mass spectrum figure with the peak area of the 16 kinds of palycyclic aromatics response as object, carry out qualitative and quantitative analysis to this sample.It is as follows to use the specific embodiment that above-mentioned test condition does:
Embodiment 1
With toluene is solvent, and preparation palycyclic aromatic standard solution carries out gas chromatograph-mass spectrometer (GCMS) GC-MS analyzing and testing by above-mentioned experiment condition, and wherein the gas chromatograph-mass spectrometer (GCMS) injector temperature is set at 280 ℃, and interface temperature is set at 280 ℃; Carrier gas is a helium, flow velocity 1 ml/min; The pattern of temperature programme is adopted in chromatogram column temperature control, since 90 ℃, is warming up to 120 ℃ with 30 ℃/minute speed, keeps 1 minute; And then be warming up to 300 ℃ with 15 ℃/minute speed, kept 15 minutes; The ion gun of Mass Spectrometer Method adopts electron bombardment ionization source (EI source), and the ion gun bombarding energy is 70eV, and ion source temperature is set at 230 ℃; Sample size 1 microlitre.
Fig. 1 a is the chromatogram of the palycyclic aromatic standard solution that detected of the embodiment of the invention 1, and the ordinate in this chromatogram is represented the intensity at peak, and horizontal ordinate is represented retention time, and unit is minute; Naphthalene in the palycyclic aromatic that the embodiment of the invention 1 that is respectively Fig. 1 b-1q is detected, acenaphthylene, acenaphthene, fluorenes, phenanthrene, anthracene, fluoranthene, pyrene, bend, benzo (a) anthracene, benzo (b) fluoranthene, benzo (k) fluoranthene, benzo (a) pyrene, indeno (1,2,3-cd) pyrene, dibenzo (a, h) anthracene and benzo (g, h, i) mass spectrogram of perylene pyrolysis product, the ordinate in the mass spectrogram is represented the relative abundance of ion, and horizontal ordinate is represented the numerical value of ion mass-to-charge ratio.The retention time of 16 kinds of palycyclic aromatics that obtain from above-mentioned figure and the characteristic ion of every kind of component see Table 1, two data of characteristic ion are used for the qualitative of palycyclic aromatic component, first data of getting every kind of component are used for quantitatively, the method of utilizing this gas chromatograph-mass spectrometer (GCMS) to detect detects and is limited to 0.03mg/kg, and quantitative limit reaches 0.10mg/kg.
The retention time of 16 kinds of palycyclic aromatic components of table 1 and the characteristic ion of every kind of component
Accurately take by weighing 0.5000 gram crisper sample in the head space bottle, add an amount of toluene, be positioned in the ultrasound bath extraction apparatus, 60 ℃ of ultrasonic extractions are got extract and are carried out the gas chromatography-mass spectrography test after 3 hours.This sample is made ten parallel samples, and experiment numbers is A, B, C, D, E, F, G, H, I and J, and analysis result sees Table 2, and to first parallel sample (test number A) replication 5 times, analysis result sees Table 3.Analysis result is found only to have naphthalene in this crisper sample, other 15 kinds of palycyclic aromatics all do not detect (＜0.10mg/kg).Because testing process may be subjected to factor affecting such as testing staff, equipment, environment, so done the truth that uncertainty evaluation comes the fiducial interval of response measurement, relevant uncertainty source as shown in Figure 2, analysis on Uncertainty the results are shown in Table 4, detection and analysis result show that this crisper contains naphthalene 1.10mg/kg, and uncertainty is 8.0%.
The test content of palycyclic aromatic in this crisper sample of table 2
This crisper sample test repeatability of table 3
| Number of times numbering (mg/kg) | ??1 | ??2 | ??3 | ??4 | ??5 | Mean value | ??RSD％ |
| ??A | ??1.10 | ??1.10 | ??1.20 | ??1.10 | ??1.20 | ??1.10 | ??4.00％ |
Table 4 test analysis on Uncertainty
Claims (10)
1, the method for palycyclic aromatic in a kind of gas chromatography-mass spectrography technical measurement food contact material is characterized in that, comprise the steps,
1. utilize soxhlet extraction or ultrasonic extraction method that the food contact material that is detected is extracted, obtain detection solution to be analyzed;
2. gas chromatograph-mass spectrometer (GCMS) is set: injector temperature is 240 ℃～320 ℃, and flow rate of carrier gas is made as 0.5 ml/min～2.0 ml/min, and chromatographic column is selected low-pole column, and interface temperature is 180 ℃～300 ℃;
3. the injection port of test sample by described gas chromatograph-mass spectrometer (GCMS) entered in the chromatographic column, carry out temperature programme,, be warming up to 270 ℃～330 ℃ since 70 ℃～100 ℃, each component in the solution to be detected is separated by chromatographic column, and determines each component concentration;
4. separated sample each component enters Mass Spectrometer Method and partly carries out Mass Spectrometer Method, determines each component structure; The ion gun of described Mass Spectrometer Method adopts electron bombardment ionization source.
2, the detection method of palycyclic aromatic in the food contact material according to claim 1 is characterized in that, alkanes, alkyl chloride hydro carbons, alcohols, ketone or benzene kind solvent are used in the 1. described extraction of step.
3, the detection method of palycyclic aromatic in the food contact material according to claim 2 is characterized in that, normal hexane or toluene are used in the 1. described extraction of step.
4, the detection method of palycyclic aromatic in the food contact material according to claim 1 is characterized in that, when 1. step used soxhlet extraction, extraction time was 8 hours～24 hours.
5, the detection method of palycyclic aromatic in the food contact material according to claim 4 is characterized in that, when 1. step used soxhlet extraction, extraction time was 12 hours～24 hours.
6, the detection method of palycyclic aromatic in the food contact material according to claim 1 is characterized in that, when 1. step used the ultrasonic extraction method, extraction time was 1 hour～5 hours.
7, the detection method of palycyclic aromatic in the food contact material according to claim 6 is characterized in that, when 1. step used the ultrasonic extraction method, extraction time was 1 hour～3 hours.
8, the detection method of palycyclic aromatic in the food contact material according to claim 1 is characterized in that, step 3. in, the mode of described temperature programme is, since 70 ℃～100 ℃, be warming up to 120 ℃～180 ℃ with 10 ℃～30 ℃/minute speed, kept 0～10 minute; And then be warming up to 270 ℃～330 ℃ with 5 ℃～20 ℃/minute speed, kept 10～20 minutes.
9, the detection method of palycyclic aromatic in the food contact material according to claim 1 is characterized in that, the step 4. ion gun bombarding energy of described Mass Spectrometer Method is 70eV, and ion source temperature is set at 230 ℃～300 ℃.
10, according to the detection method of palycyclic aromatic in each described food contact material of claim 1～9, it is characterized in that, palycyclic aromatic in the described food contact material comprises naphthalene, acenaphthylene, acenaphthene, fluorenes, phenanthrene, anthracene, fluoranthene, pyrene, benzo (a) anthracene, bends, benzo (b) fluoranthene, benzo (k) fluoranthene, benzo (a) pyrene, indeno (1,2,3-cd) pyrene, dibenzo (a, h) anthracene and benzo (g, h, i) perylene.
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| CN102578701A (en) * | 2012-02-21 | 2012-07-18 | 河南省科学院同位素研究所有限责任公司 | Method for reducing polyaromatic hydrocarbon content in tar of cigarette smoke |
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| CN107561183A (en) * | 2017-08-31 | 2018-01-09 | 中国检验检疫科学研究院 | The assay method of polycyclic aromatic hydrocarbon migration amount in a kind of soy bean milk making machine |
| CN108169388A (en) * | 2017-12-25 | 2018-06-15 | 中国第汽车股份有限公司 | The assay method of 18 kinds of polycyclic aromatic hydrocarbon PAHs in filling tires oil |
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| CN102578701A (en) * | 2012-02-21 | 2012-07-18 | 河南省科学院同位素研究所有限责任公司 | Method for reducing polyaromatic hydrocarbon content in tar of cigarette smoke |
| CN102578701B (en) * | 2012-02-21 | 2013-07-10 | 河南省科学院同位素研究所有限责任公司 | Method for reducing polyaromatic hydrocarbon content in tar of cigarette smoke |
| CN103063791A (en) * | 2012-12-06 | 2013-04-24 | 国家烟草质量监督检验中心 | Method of simultaneously determining contents of 1-OHP ,3-OHB[a]P and 3-OHB[a]A in urine |
| CN108627591A (en) * | 2017-03-24 | 2018-10-09 | 上海安谱实验科技股份有限公司 | The extracting method of polycyclic aromatic hydrocarbon in PA6 products |
| CN107561183A (en) * | 2017-08-31 | 2018-01-09 | 中国检验检疫科学研究院 | The assay method of polycyclic aromatic hydrocarbon migration amount in a kind of soy bean milk making machine |
| CN108169388A (en) * | 2017-12-25 | 2018-06-15 | 中国第汽车股份有限公司 | The assay method of 18 kinds of polycyclic aromatic hydrocarbon PAHs in filling tires oil |
| CN108680681A (en) * | 2018-07-09 | 2018-10-19 | 江苏理工学院 | Method that is a kind of while measuring polycyclic aromatic hydrocarbons on atmospheric particles and n-alkane |
| CN109164176A (en) * | 2018-07-09 | 2019-01-08 | 江苏理工学院 | A kind of method of n-alkane in detection Atmospheric particulates |
| CN110927335A (en) * | 2019-11-20 | 2020-03-27 | 珠海格力绿色再生资源有限公司 | Method for detecting peculiar smell gas of plastic package motor composite material |
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Application publication date: 20100113 |