CN105277607B - A kind of method using SIFT/MS plant identifications oil and discarded meal oil - Google Patents
A kind of method using SIFT/MS plant identifications oil and discarded meal oil Download PDFInfo
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- CN105277607B CN105277607B CN201510757469.4A CN201510757469A CN105277607B CN 105277607 B CN105277607 B CN 105277607B CN 201510757469 A CN201510757469 A CN 201510757469A CN 105277607 B CN105277607 B CN 105277607B
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Abstract
The invention belongs to technical field of food safety detection, more particularly to a kind of method using SIFT/MS plant identifications oil and discarded meal oil.Present invention measure grease is by furans, acrylamide, furfural, 2 pentyl furans, methacrylaldehyde caused by thermal induction, xenobiotic pollutants citral, limonene, allyl sulfide, metacresol, 4 isopropyl toluenes, estragole, oxidative degradation products：Aldehydes such as enanthaldehyde, octanal, 2 heptenals, 3 hexenoic aldehydes, 2 octenals, (E, E) 2 decadienal, acids such as acetic acid, propionic acid, butyric acid, valeric acid, caproic acid, other oxidative degradation products such as acetone, butanone, 2 heptanone, 1,28 kinds of 3 propane diols, Isosorbide-5-Nitrae butyrolactone, propyl propionate compositions, and then plant identification oil and discarded meal oil.This method not only saves reagent cost, and without pre-concentration, without post separation, do not need standard items, there is high sensitivity, simple, quick, accurate.
Description
Technical field
It is oily and useless using SIFT/MS plant identifications more particularly to one kind the invention belongs to technical field of food safety detection
The method for abandoning meal oil.
Background technology
Detection and false distinguishing for edible oil and fat such as vegetable oil at present, mainly determine its xenobiotic pollutants and its inherently into
Divide the change of (also known as endogenous components).1. for exogenous pollution thing, what is predominantly detected is：Conventional physical and chemical index --- moisture
Content, proportion, index of refraction, acid value, peroxide value, carbonyl value, iodine number etc.；Heavy metal --- Fe, Pb, Cr, Zn, Mn and therewith phase
Electrical conductivity of pass etc.；Animal fat possibility --- cholesterol；Mineral oil stain --- C9-14What alkane and Oxidation of Fat and Oils went bad
Secondary products --- acetaldehyde；Surfactant (detergent residual) --- neopelex, mycotoxin --- Huang Qu
Mould toxin B etc..2. for endogenous components change indicator, what is predominantly detected is：D-GLAC, oxidation triglycerides, aliphatic acid
Degree of unsaturation, low carbon number aliphatic acid, grease characteristic fingerprint pattern etc..But the detection of these indexs, it is often difficult to and discarded meal
Distinguished with the similar index of oil, therefore, it is difficult to they are differentiated.And some important indexs, such as in the oil heating of discarded meal
During the material such as caused furans, furfural, 2-amyl furan, acrylamide, methacrylaldehyde, there is presently no as inspection
Survey or differential plant is oily or discards characteristics index of the meal with the oily true and false.
For oily, especially gutter oil the detection of discarded meal, it has been reported that big quantity measuring method, only domestic disclosed ground
The patent document of ditch oil detection technique has 100 more than one piece, including spectrum, chromatogram, electrical conductivity, mass spectrum, acid number, nuclear magnetic resonance, test paper
Etc. technology, although these technologies can differentiate the discarded meal oil such as gutter oil under certain conditions, due to discarded meal oil
Source is complicated, species is more, and the selectivity of most detection techniques is poor, it is difficult to is accurately detected；Some technologies then generally need
Detect multiple characteristic indexs, need a variety of analytical instrument and equipment, and detecting step is cumbersome, time-consuming longer, testing cost is inclined
Height, or the degree of accuracy be not high etc., far from adapting to quick, accurate and Site Detection demand.
Therefore, at present there is an urgent need to develop new quick, easy, reliable detection technique, for the discarded meal such as gutter oil
With the qualitative and quantitative analysis of oil.
Gutter oil detection method, but the actual identification result of collected method are once collected in China twice by the Ministry of Public Health
It is unsatisfactory, do not announce unified, effective, the general detection method in the whole nation also so far.
As can be seen here, although many research work have been done by the country, up to the present, also without accurately, quickly, conveniently
The oily method of the discarded meal of detection gutter oil etc..
The content of the invention
The shortcomings that primary and foremost purpose of the present invention is to overcome existing vegetable oil authentication detection technology and deficiency, there is provided one kind utilizes
The method of SIFT/MS plant identifications oil and discarded meal oil, this method are easy, quick, accurate.
The purpose of the present invention is achieved through the following technical solutions：
A kind of method using SIFT/MS plant identifications oil and discarded meal oil, comprise the following steps：
(1) detection sample is fitted into sealing container, 60~70 DEG C of heated at constant temperature 30~80 minutes are to all in container
After gas reaches the state of vapor liquid equilibrium, using in selection ion flow pipe mass spectrography (SIFT/MS) measure sealing container head space
Volatile ingredient and semi-volatility component (Semi-volatile-organic-compound)：Described volatile ingredient and
Semi-volatility component includes thermal decomposition product, xenobiotic pollutants, oxidative degradation products；
(2) component of gas componant, content, ratio identification testing sample type measured by：
Oxidative degradation products 2-HEPTANONE, 2- octenals, (E, E) -2,4- decadienals are not contained in sample when detecting, heat point
Product furans is solved, during this 6 kinds of compositions of xenobiotic pollutants citral, estragole, you can judge that detection sample is vegetable oil；Instead
It, then be determined as discarded meal oil；
Detection sample described in step (1) is vegetable oil or discarded meal oil；
Described vegetable oil is soybean oil, peanut oil, rapeseed oil, sunflower oil, tea oil, sesame oil and ready-mixed oil (by peanut
At least one of oil, rapeseed oil, soybean oil etc., which are blent, to be formed)；Described discarded meal is gutter oil, frying oil with oil and given up
Abandon at least one of animal offal oil；
Described gutter oil refers in the trench near the restaurant of dining room, the greasy floating object of the canescence above sewage, by every
Oily device is collected, then through manually refining the grease or its concise product that have been transmitted across becoming sour and should not eat again；Described frying
Old oil is to be repeatedly used for fried food at high temperature, and the deterioration reaction such as oxidation, hydrolysis, polymerization occurs, can not be further continued for edible
Grease；Described discarded animal offal oil refer to the discarded pluck collected by the market of farm produce it is refined be not suitable for eating
Animal fat；
The volume ratio (i.e. liquid-gas ratio) of detection sample and sealing container described in step (1) is preferably 1：50~100；
The quality of detection sample described in step (1) is preferably 5~25 grams；
The volume of sealing container described in step (1) is preferably 0.5~3 liter；
Thermal decomposition product described in step (1) includes furans, acrylamide, furfural, 2-amyl furan and methacrylaldehyde (5
Kind)；
Xenobiotic pollutants described in step (1) includes citral, limonene, allyl sulfide, metacresol (m-
Cresol), 4- isopropyl toluenes and estragole (6 kinds)；
Oxidative degradation products described in step (1) include aldehydes, acids and other oxidative degradation products；
Described aldehydes includes enanthaldehyde, octanal, 2- heptenals, 3- hexenoic aldehydes, 2- octenals and (E, E) -2,4- decadinene
Aldehyde (6 kinds)；
Described acids includes acetic acid, propionic acid, butyric acid, valeric acid and caproic acid (5 kinds)；
Described other oxidative degradation products (alcohol, ketone, ester) include acetone, butanone, 2-HEPTANONE, 1,3- propane diols, 1,4-
Butyrolactone and propyl propionate (6 kinds)；
SIFT/MS methods for measuring described in step (1) are：Choice ion pattern (SIM), argon gas and helium are load
Gas, H3O+、NO+And O2 +As precursor ion, using such as the kinetic parameter of table 1 calculate survey 28 kinds of gas componant contents：
The parameter of 28 kinds of gas componants in the SIFT/MS of table 1 measure oil
The measure of SIFT/MS measure described in step (1), which operates, is preferably：
SIFT-MS first level Four bar and second level Four bar stabilization time are respectively 25ms and 10ms；Microwave power：
50W；Air is used as ion source gas；Gas flow is respectively 2 and 3KPa L/s；The gas flow of sample and capillary is respectively
0.45 and 1.3KPa L/s；Before measure, code is used according to instrument, the calibrating gas provided using company carries out precision and essence
Exactness is examined；
Described in step (1) SIFT/MS measure condition determination be preferably：Sweep time 60s；The computing relay time,
5s；Sampling period, 100ms；Presoma, 25ms；Sample inlet temperature, 120 DEG C；Carrier gas argon pressure, 200KPa；Helium pressure
Power, 0.5M Pa；The vacuum pressure of flow tube is 5Pa；
Identification testing sample type described in step (2), also comprises the following steps：
Contain higher thermal decomposition product, xenobiotic pollutants and oxidative degradation products in sample when detecting, you can judge inspection
Test sample product are gutter oil；
Contain xenobiotic pollutants, and GBL >=950ng/mL, furans >=130ng/mL, furfural in sample when detecting
When >=60ng/mL, acrylamide >=100ng/mL, you can judge that detection sample is gutter oil；
Furfural, 2-amyl furan, butyric acid, caproic acid and limonene are not contained when detecting in sample, but contains 1,3-PD
1100 >=1200ng/mL and methacrylaldehyde >=4600ng/mL, you can it is discarded animal offal oil to judge detection sample：
It is organic acid when detecting volatile component content highest composition in sample, the content of other compositions is below
During 1000ng/mL, you can judge that detection sample is frying oil；
Preferably, in described organic acid, butyric acid content highest, propionic acid take second place, acetic acid the 3rd；
It is further preferred that content >=10000ng/mL of described butyric acid, content >=8300ng/mL of propionic acid, acetic acid
Content >=4163ng/mL；
The present invention is had the following advantages relative to prior art and effect：
(1) 28 kinds of ingredient standard product are not needed and carry out qualitative and quantitative analysis, time saving cost is low.
(2) chromatogram post separation need not be carried out and as needed while 28 kinds of characteristic chemical constituents of measure.Directly obtain sealing
Shuttle headspace gas is analyzed, it is not necessary to most of material composition can be made to be difficult to be separated by chromatographic column.
(3) high sensitivity (10-12g)：Can determine nanogram level content, even below above-mentioned 28 kinds of nanogram level content into
Point, it is particularly possible to the degree of accuracy detects caused by the heated oxidation Decomposition of aliphatic acid and its micro material composition.
(4) low temperature sample introduction (≤70 DEG C)：28 compositions not destroyed under the conditions of this in surveyed grease.
(5) it is easy to use：Sample need not be extracted, is enriched with, rough segmentation or subdivision, directly carry out vapor liquid equilibrium with crude oil
For determining, this provides possibility for quick, a large amount of determination samples；SIFT-MS instruments can move, be loaded in vehicle Shang Dao cities
Field, market carry out on-site measurement, and this provides Reliable guarantee for situ appraisal vegetable oil.
(6) finding speed is fast：The time of machine practical measurement is 2 minutes on each sample, and this is provided for a large amount of determination samples
Ensure.If it is necessary, both can be with the real time measure after slightly changing.
(7) reagent costs such as standard specimen, extraction agent, chromatogram flow phase are saved.
Brief description of the drawings
Fig. 1 is the mass-to-charge ratio figure that embodiment 1 determines ion.
Embodiment
With reference to embodiment and accompanying drawing, the present invention is described in further detail, but embodiments of the present invention are unlimited
In this.
Embodiment 1
The present embodiment studies separate sources vegetable oil (different soybean oils, peanut oil, rapeseed oil, tea oil, sunflower oil, mediation
Oily (be raw material by soya-bean oil, peanut rapeseed oil)), animal offal oil, frying oil, former gutter oil, refine 86 samples such as gutter oil
The content of thermal decomposition product, xenobiotic pollutants, oxidative degradation products totally 28 kinds of components, specific method are in product：
5 grams of samples are added in 540mL vials, with the rubber seal rings for seal that can be penetrated by stainless steel syringe needle, put
Enter 65 DEG C of waters bath with thermostatic control kept for 60 minutes, require to set measure reactive ion, detection ion and used ion according to table 1
Reaction rate constant；SIFT-MS first level Four bar and second level Four bar stabilization time are respectively 25ms and 10ms；Microwave
Power：50W；Air is used as ion source gas；Gas flow is respectively 2 and 3KPa L/s；The gas flow of sample and capillary
Respectively 0.45 and 1.3KPa L/s.The sweep time of use, 60s；Computing relay time, 5s；Sampling period 100ms；Forerunner
Body, 25ms；Sample inlet temperature, 120 DEG C；Carrier gas argon pressure is 200KPa；Helium pressure, 0.5MPa；The vacuum pressure of flow tube
Power is 5Pa (Fig. 1).
As a result as shown in table 2, can be to be surveyed by determinations such as the content of its various composition and ratios according to measurement result
Sample belongs to vegetable oil or discarded meal oil：
In the 28 kinds of compositions determined, do not contained in vegetable oil oxidative degradation products 2-HEPTANONE, 2- octenals, (E, E)-
6 kinds of compositions such as 2,4- decadienals, thermal decomposition product furans, xenobiotic pollutants citral, estragole, on the contrary, discarded meal
With containing these compositions or most of composition therein in oil；Vegetable oil and discarded meal can then be differentiated with oil accordingly.Separately
Outside, other 22 compositions several times low far beyond discarded meal oil content or 1~3 in vegetable oil outside all above-mentioned 6 kinds measured
The individual order of magnitude.Therefore, vegetable oil and discarded meal oil can easily be identified according to this 2 points.
It is with the detection method between oil for different discarded meal：
Gutter oil：Higher oxidative cleavage of fatty acids thing, thermal degradation products and xenobiotic pollutants are typically contained, is often it
His the oily several times of discarded meal, especially GBL (950~1800ng/mL), furans (130~530), furfural (90~
120ng/mL), acrylamide (100~450ng/mL) is above frying oil, discards animal offal oil and distinguished；
Discarded animal offal oil：Do not contain 2-HEPTANONE, (E, E) -2,4- decadienals, 2-amyl furan, butyric acid, caproic acid,
Citral, limonene, estragole, but contain higher 1,3-PD (1100-1200ng/mL) and methacrylaldehyde (4600-
It can 5000ng/mL) be differentiated with frying oil, gutter oil etc..
Frying oil：The composition in above-mentioned 28, its Volatility Levels highest composition are organic acid, butyric acid content therein
Highest (10000-11000ng/mL), propionic acid take second place (8300-9100ng/mL), acetic acid the 3rd (4163-4600ng/mL), other
The content of composition is below 1000ng/mL.
Comparision contents (unit of the 2 28 kinds of compositions of table in vegetable oil and discarded meal oil：ng/mLng/mLng/mL)
*：In addition to label range escaping gas, remaining composition variations amplitude is 5~10%.
Embodiment 2
5 grams of unknown oil samples are added in 540mL vials, it is close with the rubber seal that can be penetrated by stainless steel syringe needle
Envelope, it is put into 65 DEG C of waters bath with thermostatic control and is being kept for 60 minutes, requires to set measure reactive ion, detection ion and adopted according to subordinate list 1
With the reaction rate constant of ion；SIFT-MS first level Four bar and second level Four bar stabilization time be respectively 25ms and
10ms；Microwave power：50W；Air is used as ion source gas；Gas flow is respectively 2 and 3KPa L/s；Sample and capillary
Gas flow is respectively 0.45 and 1.3KPa L/s.The sweep time of use, 60s；Computing relay time, 5s；Sampling period
100ms；Presoma, 25ms；Sample inlet temperature, 120 DEG C；Carrier gas argon pressure is 200KPa；Helium pressure, 0.5MPa；Stream
The vacuum pressure of pipe is 5Pa.
When measuring the 1,3-PD 1150ng/mL in oil sample, methacrylaldehyde 4610ng/mL, but furfural, 2- amyl groups are not contained
Furans, butyric acid, caproic acid, limonene, according to table 2, it can be determined that the sample is discarded animal offal oil, is consistent with actual result.
Embodiment 3
5 grams of unknown oil samples are added in 540mL vials, it is close with the rubber seal that can be penetrated by stainless steel syringe needle
Envelope, it is put into 65 DEG C of waters bath with thermostatic control and is being kept for 60 minutes, assay method is the same as embodiment 1.
When measuring the GBL 1100ng/mL in the unknown oil sample, furans 140ng/mL, furfural 120ng/mL, third
Acrylamide 400ng/mL, citral 380ng/mL, estragole 30ng/mL, 4- isopropyl toluene 3000ng/mL, Ke Yican
Judge that the oil sample belongs to trench oils and discards meal oil according to table 2, be consistent with actual result.
Embodiment 4
5 grams of unknown oil samples are added in 540mL vials, it is close with the rubber seal that can be penetrated by stainless steel syringe needle
Envelope, it is put into 65 DEG C of waters bath with thermostatic control and is being kept for 60 minutes, assay method is the same as embodiment 1.
Do not detected in the unknown oil sample 2-HEPTANONE, (E, E) -2,4- decadienals, 2- octenals, furans, citral,
6 kinds of compositions of methyl pepper powder, the oil sample that can break accordingly with table 2 belongs to common vegetable oil rather than discarded meal oil, with actual knot
Fruit is consistent.
Embodiment 5
25 grams of unknown oil samples are added in the stainless steel cylinders of 3L, it is close with the rubber seal that can be penetrated by stainless steel syringe needle
Envelope, it is put into 65 DEG C of waters bath with thermostatic control and is being kept for 60 minutes, assay method is the same as embodiment 1.
When measuring in 28 in the unknown oil sample in volatility or half volatile material, its butyric acid content highest
(10050ng/mL), propionic acid take second place (8500ng/mL), acetic acid the 3rd (4463ng/mL), and the content of other compositions is below
900ng/mL.It can judge that the oil sample belongs to frying oil class and discards meal oil with table 2 accordingly, be consistent with actual result.
Above-described embodiment is the preferable embodiment of the present invention, but embodiments of the present invention are not by above-described embodiment
Limitation, other any Spirit Essences without departing from the present invention with made under principle change, modification, replacement, combine, simplification,
Equivalent substitute mode is should be, is included within protection scope of the present invention.
Claims (10)
- A kind of 1. method using SIFT/MS plant identifications oil and discarded meal oil, it is characterised in that comprise the following steps：(1) detection sample is fitted into sealing container, 60~70 DEG C of heated at constant temperature 30~80 minutes to gas all in container After the state for reaching vapor liquid equilibrium, the volatile ingredient and semi-volatility component in sealing container head space are determined using SIFT/MS： Described volatile ingredient and semi-volatility component include thermal decomposition product, xenobiotic pollutants, oxidative degradation products；(2) component of gas componant, content, ratio identification testing sample type measured by：Oxidative degradation products 2-HEPTANONE, 2- octenals, (E, E) -2,4- decadienals are not contained in sample when detecting, thermal decomposition production Thing furans, during this 6 kinds of compositions of xenobiotic pollutants citral, estragole, judge that detection sample is vegetable oil；Conversely, then sentence It is set to discarded meal oil.
- 2. the method according to claim 1 using SIFT/MS plant identifications oil and discarded meal oil, it is characterised in that：The volume ratio of detection sample and sealing container described in step (1) is 1：50~100.
- 3. the method according to claim 1 using SIFT/MS plant identifications oil and discarded meal oil, it is characterised in that：Thermal decomposition product described in step (1) includes furans, acrylamide, furfural, 2-amyl furan and methacrylaldehyde.
- 4. the method according to claim 1 using SIFT/MS plant identifications oil and discarded meal oil, it is characterised in that：Xenobiotic pollutants described in step (1) includes citral, limonene, allyl sulfide, metacresol, 4- isopropyl first Benzene and estragole.
- 5. the method according to claim 1 using SIFT/MS plant identifications oil and discarded meal oil, it is characterised in that：Oxidative degradation products described in step (1) include aldehydes, acids and other oxidative degradation products；Described aldehydes includes enanthaldehyde, octanal, 2- heptenals, 3- hexenoic aldehydes, 2- octenals and (E, E) -2,4- decadienals；Described acids includes acetic acid, propionic acid, butyric acid, valeric acid and caproic acid；Described other oxidative degradation products include acetone, butanone, 2-HEPTANONE, 1,3- propane diols, 1,4- butyrolactone and propionic acid third Ester.
- 6. the method according to claim 1 using SIFT/MS plant identifications oil and discarded meal oil, it is characterised in that：SIFT/MS methods for measuring described in step (1) are：Choice ion pattern, argon gas and helium are carrier gas, H3O+、NO+ And O2 +As precursor ion, calculated using following kinetic parameter and survey 28 kinds of gas componant contents：
- 7. the method according to claim 1 using SIFT/MS plant identifications oil and discarded meal oil, it is characterised in that：The measure of SIFT/MS measure described in step (1), which operates, is：SIFT-MS first level Four bar and second level Four bar stabilization time are respectively 25ms and 10ms；Microwave power：50W； Air is used as ion source gas；Gas flow is respectively 2 and 3KPa L/s；The gas flow of sample and capillary is respectively 0.45 With 1.3KPa L/s.
- 8. the method according to claim 1 using SIFT/MS plant identifications oil and discarded meal oil, it is characterised in that：Described in step (1) SIFT/MS measure condition determination be：Sweep time 60s；Computing relay time, 5s；Sampling week Phase, 100ms；Presoma, 25ms；Sample inlet temperature, 120 DEG C；Carrier gas argon pressure, 200KPa；Helium pressure, 0.5M Pa； The vacuum pressure of flow tube is 5Pa.
- 9. the method according to claim 1 using SIFT/MS plant identifications oil and discarded meal oil, it is characterised in that：Identification testing sample type described in step (2), also comprises the following steps：Contain xenobiotic pollutants, and GBL >=950ng/mL in sample when detecting, furans >=130ng/mL, furfural >= When 60ng/mL, acrylamide >=100ng/mL, judge that detection sample is gutter oil；Furfural, 2-amyl furan, butyric acid, caproic acid and limonene are not contained in sample when detecting, but contains 1,3-PD 1100 >=1200ng/mL and methacrylaldehyde >=4600ng/mL, judge that detection sample is animal offal oil：It is organic acid when detecting volatile component content highest composition in sample, the content of other compositions is below 1000ng/ During mL, judge that detection sample is frying oil.
- 10. the method according to claim 9 using SIFT/MS plant identifications oil and discarded meal oil, it is characterised in that：In described organic acid, butyric acid content highest, propionic acid take second place, acetic acid the 3rd.
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Citations (2)
| Publication number | Priority date | Publication date | Assignee | Title |
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| CN102272602A (en) * | 2008-10-31 | 2011-12-07 | 生物梅里埃公司 | Methods for the isolation and identification of microorganisms |
| CN103033571A (en) * | 2012-09-17 | 2013-04-10 | 福建中烟工业有限责任公司 | Method for measuring arsenic form in tobacco |
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| JPH067127B2 (en) * | 1985-08-26 | 1994-01-26 | 徳山曹達株式会社 | Carbonyl sulfide analysis method |
| NZ520019A (en) * | 2002-07-05 | 2005-02-25 | Syft Technologies Ltd | A method of assaying the antioxidant activity of pure compounds, extracts and biological fluids using SIFT-MS technology |
| NZ534909A (en) * | 2004-08-26 | 2005-10-28 | Syft Technologies Ltd | A method of assaying the antioxidant activity of oils and lipids using SIFT-MS technology |
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| CN102272602A (en) * | 2008-10-31 | 2011-12-07 | 生物梅里埃公司 | Methods for the isolation and identification of microorganisms |
| CN103033571A (en) * | 2012-09-17 | 2013-04-10 | 福建中烟工业有限责任公司 | Method for measuring arsenic form in tobacco |
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