CN106501432A - A kind of detection method of fatty acid irradiated products in food - Google Patents
A kind of detection method of fatty acid irradiated products in food Download PDFInfo
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- CN106501432A CN106501432A CN201610943972.3A CN201610943972A CN106501432A CN 106501432 A CN106501432 A CN 106501432A CN 201610943972 A CN201610943972 A CN 201610943972A CN 106501432 A CN106501432 A CN 106501432A
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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
- G01N30/62—Detectors specially adapted therefor
- G01N30/64—Electrical detectors
- G01N30/68—Flame ionisation detectors
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Abstract
The invention discloses a kind of detection method of fatty acid irradiated products in food, the food samples that will be enriched in fat carry out radiation treatment, mixed solvent is added to be extracted, upper oil phase is dried concentration, and further processes, prepare the fat-extraction liquid of different concentration, using chromatography post separation standard working solution, from nonpolar capillary column HP 5, separated with GC, using " not shunting " sample introduction, detected with FID；Testing result is sorted out by concentration proportioning, and is counted.The inventive method realizes the detection of the radiation-processed food of fatty acids by simple step, effective detection raw meat and rich in the composition in food after fatty fruit radiation treatment and content, accurately, versatility is good for testing result, can be used as the means of detection irradiated foods.
Description
Technical field
The present invention relates to field of food detection, specifically a kind of detection method of fatty acid irradiated products in food.
Background technology
Radiation-processed food, i.e., the food for being processed with radioactive source.Sterilized by radiation-processed food or parasite killing, it
It is another the food fresh keeping New Machining Technology after the technology such as the canned heating of food, freezing, after processing via radiation
Food have can keep the spies such as original local flavor, energy-conservation, the pathogenic bacteria that product centre position can be killed, drug residue free
Point, can preserve under room temperature or refrigerated condition, reduce shelter cost.
Due to the plurality of advantages of radiation-processed food, radiation-processed food is commercially increasing, current 40 Duo Ge states
Family allows to produce more than 60 kinds of radiation treatment food, about produces the food of 500,000 radiation treatment every year.But according to investigation, very
The food of many radiation treatment does not make specific identifier in relevant position, and some commodity also have illegal process, excessive
The phenomenons such as radiation treatment, seem particularly significant hence with correlation technique to whether food carries out detection through radiation treatment.
However, the energy due to radiating is below each component in food may induce radioactive threshold energy, Bu Hui
Radioactivity is induced in food, so whether there cannot be radioactivity to judge food whether through radiation treatment by food.Heat is released
Light, photo stimulated luminescence are which can be deposited according to the silicate impurity mixed in food at present using relatively broad detection method
Storage emittance, and being detected being heated, the characteristics of release energy in the case of photostimulation, but at present these methods due to receiving
The limitation of food institute silicate quantity, current and inapplicable raw meat based food.
Content of the invention
It is an object of the invention to provide a kind of detection method of fatty acid irradiated products in food, above-mentioned to solve
The problem proposed in background technology.
For achieving the above object, the present invention provides following technical scheme：
A kind of detection method of fatty acid irradiated products in food, comprises the following steps：
（1）Weigh rich fatty food samples, be processed rubbing process, after allowing, carry out radiation treatment, add pentane and
The mixed solvent of propanol, stirs, and is transferred in glass tubing, is then centrifuged for 20～30min, separates upper oil phase and lower floor's thing
Matter, adds above-mentioned mixed solvent to be extracted twice again, merges three upper oil phases, and less than 42 DEG C are carried out with Rotary Evaporators
Concentration, is subsequently adding pentane, and adds anhydrous sodium sulfate to be dried, and constantly vibrate, be filtered to remove anhydrous sodium sulfate, and 42
Concentrated in vacuo, removing solvent is carried out below DEG C；
（2）Fat-extraction liquid concentrated in vacuo is transferred in weighed sealing test tube, N2Stream drying sample to constant weight, i.e.,
Be obtained in food samples or fat-extraction liquid in fat content；
（3）Measure fat-extraction liquid to be placed in volumetric flask, add methanol ultrasonic dissolution, be cooled to room temperature, with methanol constant volume, prepare
Into standard reserving solution；Standard reserving solution is being diluted 2～8 times, with methanol constant volume, the standard working solution of variable concentrations is being obtained, is shaken
Even standby；
（4）Using chromatography post separation standard working solution, from nonpolar capillary column HP-5, separated with GC, using " regardless of
Stream " sample introduction, is detected with FID；
（5）Above-mentioned testing result is sorted out by concentration proportioning, and is counted.
As further scheme of the invention：The step（1）In, rich fatty food include but is not limited to Carnis Gallus domesticus,
One kind in Carnis Sus domestica, the flesh of fish, Fructus Chaenomeliss, Fructus Mangifera Indicae.
As further scheme of the invention：The step（4）In, the GC conditions, injector temperature：200
℃；Initial column temperature：30 DEG C of constant temperature 2min；And temperature programming：20 DEG C/min to 80 DEG C；Side program heats up：2 DEG C/min is extremely
160℃；Three-level temperature programming：8 DEG C/min to 250 DEG C；Final temperature：Keep 10min；1 μ L of sampling volume；Sample introduction pattern：No
Shunting；H2：Air=1:100；250 DEG C of detector temperature.
Compared with prior art, the invention has the beneficial effects as follows：
The inventive method realizes the detection of the radiation-processed food of fatty acids by simple step, effective detection raw meat and
Rich in the composition in food after fatty fruit radiation treatment and content, accurately, versatility is good for testing result, can be used as detection spoke
Penetrate the means of food.
Specific embodiment
Below in conjunction with the embodiment of the present invention, to the embodiment of the present invention in technical scheme be clearly and completely described,
Obviously, described embodiment is only a part of embodiment of the invention, rather than whole embodiment.In based on the present invention
Embodiment, the every other embodiment obtained under the premise of creative work is not made by those of ordinary skill in the art, all
Belong to the scope of protection of the invention.
Embodiment 1
The detection method of fatty acid irradiated products in Carnis Sus domestica, step are as follows：
（1）Weigh rich fatty food samples, be processed rubbing process, after allowing, carry out radiation treatment, add pentane and
The mixed solvent of propanol, stirs, and is transferred in glass tubing, is then centrifuged for 30min, separates upper oil phase and lower floor's material,
Add again above-mentioned mixed solvent extracted twice, merge three upper oil phases, less than 42 DEG C carried out with Rotary Evaporators dense
Contracting, is subsequently adding pentane, and adds anhydrous sodium sulfate to be dried, and constantly vibrate, be filtered to remove anhydrous sodium sulfate, 42 DEG C
Concentrated in vacuo, removing solvent is below carried out；
（2）Fat-extraction liquid concentrated in vacuo is transferred in weighed sealing test tube, N2Stream drying sample to constant weight, i.e.,
Be obtained in food samples or fat-extraction liquid in fat content；
（3）Measure fat-extraction liquid to be placed in volumetric flask, add methanol ultrasonic dissolution, be cooled to room temperature, with methanol constant volume, prepare
Into standard reserving solution；Standard reserving solution is being diluted 2～8 times, with methanol constant volume, the standard working solution of variable concentrations is being obtained, is shaken
Even standby；
（4）Using chromatography post separation standard working solution, from nonpolar capillary column HP-5, separated with GC, using " regardless of
Stream " sample introduction, is detected with FID；
GC conditions, injector temperature：200℃；Initial column temperature：30 DEG C of constant temperature 2min；And temperature programming：20 DEG C/min is extremely
80℃；Side program heats up：2 DEG C/min to 160 DEG C；Three-level temperature programming：8 DEG C/min to 250 DEG C；Final temperature：Keep
10min；1 μ L of sampling volume；Sample introduction pattern：Do not shunt；H2：Air=1:100；250 DEG C of detector temperature；
（5）Above-mentioned testing result is sorted out by concentration proportioning, and is counted.
Embodiment 2
The detection method of fatty acid irradiated products in Fructus Chaenomeliss, step are as follows：
（1）Weigh rich fatty food samples, be processed rubbing process, after allowing, carry out radiation treatment, add pentane and
The mixed solvent of propanol, stirs, and is transferred in glass tubing, is then centrifuged for 20min, separates upper oil phase and lower floor's material,
Add again above-mentioned mixed solvent extracted twice, merge three upper oil phases, less than 42 DEG C carried out with Rotary Evaporators dense
Contracting, is subsequently adding pentane, and adds anhydrous sodium sulfate to be dried, and constantly vibrate, be filtered to remove anhydrous sodium sulfate, 42 DEG C
Concentrated in vacuo, removing solvent is below carried out；
（2）Fat-extraction liquid concentrated in vacuo is transferred in weighed sealing test tube, N2Stream drying sample to constant weight, i.e.,
Be obtained in food samples or fat-extraction liquid in fat content；
（3）Measure fat-extraction liquid to be placed in volumetric flask, add methanol ultrasonic dissolution, be cooled to room temperature, with methanol constant volume, prepare
Into standard reserving solution；Standard reserving solution is being diluted 2～8 times, with methanol constant volume, the standard working solution of variable concentrations is being obtained, is shaken
Even standby；
（4）Using chromatography post separation standard working solution, from nonpolar capillary column HP-5, separated with GC, using " regardless of
Stream " sample introduction, is detected with FID；
GC conditions, injector temperature：200℃；Initial column temperature：30 DEG C of constant temperature 2min；And temperature programming：20 DEG C/min is extremely
80℃；Side program heats up：2 DEG C/min to 160 DEG C；Three-level temperature programming：8 DEG C/min to 250 DEG C；Final temperature：Keep
10min；1 μ L of sampling volume；Sample introduction pattern：Do not shunt；H2：Air=1:100；250 DEG C of detector temperature；
（5）Above-mentioned testing result is sorted out by concentration proportioning, and is counted.
It is obvious to a person skilled in the art that the invention is not restricted to the details of above-mentioned one exemplary embodiment, Er Qie
In the case of spirit or essential attributes without departing substantially from the present invention, the present invention can be realized in other specific forms.Therefore, no matter
From the point of view of which point, embodiment all should be regarded as exemplary, and be nonrestrictive, the scope of the present invention is by appended power
Profit is required rather than described above is limited, it is intended that all in the implication and scope of the equivalency of claim by falling
Change is included in the present invention.
Claims (3)
1. a kind of detection method of fatty acid irradiated products in food, it is characterised in that comprise the following steps：
（1）Weigh rich fatty food samples, be processed rubbing process, after allowing, carry out radiation treatment, add pentane and
The mixed solvent of propanol, stirs, and is transferred in glass tubing, is then centrifuged for 20～30min, separates upper oil phase and lower floor's thing
Matter, adds above-mentioned mixed solvent to be extracted twice again, merges three upper oil phases, and less than 42 DEG C are carried out with Rotary Evaporators
Concentration, is subsequently adding pentane, and adds anhydrous sodium sulfate to be dried, and constantly vibrate, be filtered to remove anhydrous sodium sulfate, and 42
Concentrated in vacuo, removing solvent is carried out below DEG C；
（2）Fat-extraction liquid concentrated in vacuo is transferred in weighed sealing test tube, N2Stream drying sample to constant weight, i.e.,
Be obtained in food samples or fat-extraction liquid in fat content；
（3）Measure fat-extraction liquid to be placed in volumetric flask, add methanol ultrasonic dissolution, be cooled to room temperature, with methanol constant volume, prepare
Into standard reserving solution；Standard reserving solution is being diluted 2～8 times, with methanol constant volume, the standard working solution of variable concentrations is being obtained, is shaken
Even standby；
（4）Using chromatography post separation standard working solution, from nonpolar capillary column HP-5, separated with GC, using " regardless of
Stream " sample introduction, is detected with FID；
（5）Above-mentioned testing result is sorted out by concentration proportioning, and is counted.
2. the detection method of fatty acid irradiated products in food according to claim 1, it is characterised in that the step
Suddenly（1）In, rich fatty food includes but is not limited to the one kind in Carnis Gallus domesticus, Carnis Sus domestica, the flesh of fish, Fructus Chaenomeliss, Fructus Mangifera Indicae.
3. the detection method of fatty acid irradiated products in food according to claim 1, it is characterised in that the step
Suddenly（4）In, the GC conditions, injector temperature：200℃；Initial column temperature：30 DEG C of constant temperature 2min；And temperature programming：20
DEG C/min to 80 DEG C；Side program heats up：2 DEG C/min to 160 DEG C；Three-level temperature programming：8 DEG C/min to 250 DEG C；Most final temperature
Degree：Keep 10min；1 μ L of sampling volume；Sample introduction pattern：Do not shunt；H2：Air=1:100；250 DEG C of detector temperature.
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| CN201610943972.3A CN106501432A (en) | 2016-11-02 | 2016-11-02 | A kind of detection method of fatty acid irradiated products in food |
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| CN201610943972.3A CN106501432A (en) | 2016-11-02 | 2016-11-02 | A kind of detection method of fatty acid irradiated products in food |
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Citations (5)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| FR2695208A1 (en) * | 1992-08-25 | 1994-03-04 | Inocosm Laboratoires | Analysing volatile prods. using adsorbent cartridge - esp. for determn. of alkane(s) formed in peroxidation of cell membrane unsatd. fatty acid(s) |
| WO2002100991A2 (en) * | 2001-06-13 | 2002-12-19 | Biorama 2000 S.R.L. | Mono-, di- and triglycerides or their mixtures containing trans-fatty acid residues and method of their formation |
| CN101793877A (en) * | 2009-11-26 | 2010-08-04 | 天津出入境检验检疫局动植物与食品检测中心 | Method for detecting fatty acid irradiated products in food |
| CN101793878A (en) * | 2009-11-26 | 2010-08-04 | 天津出入境检验检疫局动植物与食品检测中心 | Detection method for specific radiolysis product of fat-containing food treated by ionizing radiation exposure |
| CN104569266A (en) * | 2014-12-31 | 2015-04-29 | 北京市农林科学院 | Method for quickly detecting content of 2-DCB (2-dodecylcyclobutanone) in irradiated foods containing fat |
-
2016
- 2016-11-02 CN CN201610943972.3A patent/CN106501432A/en active Pending
Patent Citations (5)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| FR2695208A1 (en) * | 1992-08-25 | 1994-03-04 | Inocosm Laboratoires | Analysing volatile prods. using adsorbent cartridge - esp. for determn. of alkane(s) formed in peroxidation of cell membrane unsatd. fatty acid(s) |
| WO2002100991A2 (en) * | 2001-06-13 | 2002-12-19 | Biorama 2000 S.R.L. | Mono-, di- and triglycerides or their mixtures containing trans-fatty acid residues and method of their formation |
| CN101793877A (en) * | 2009-11-26 | 2010-08-04 | 天津出入境检验检疫局动植物与食品检测中心 | Method for detecting fatty acid irradiated products in food |
| CN101793878A (en) * | 2009-11-26 | 2010-08-04 | 天津出入境检验检疫局动植物与食品检测中心 | Detection method for specific radiolysis product of fat-containing food treated by ionizing radiation exposure |
| CN104569266A (en) * | 2014-12-31 | 2015-04-29 | 北京市农林科学院 | Method for quickly detecting content of 2-DCB (2-dodecylcyclobutanone) in irradiated foods containing fat |
Non-Patent Citations (3)
| Title |
|---|
| ISMAIL YILMAZ 等: "Effects of gamma irradiation on trans fatty acid composition in ground beef", 《FOOD CONTROL》 * |
| PETER LEMBKE等: "Characterization of Irradiated Food by SFE and GC-MSD", 《J. AGRIC. FOOD CHEM.》 * |
| 李安: "含脂辐照食品的气相色谱检测及鉴定技术研究", 《中国优秀硕士学位论文全文数据库 工程科技Ⅰ辑》 * |
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