CN108732282A - The detection method of ethylene oxidic ester in vegetable oil - Google Patents
The detection method of ethylene oxidic ester in vegetable oil Download PDFInfo
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- CN108732282A CN108732282A CN201810383602.8A CN201810383602A CN108732282A CN 108732282 A CN108732282 A CN 108732282A CN 201810383602 A CN201810383602 A CN 201810383602A CN 108732282 A CN108732282 A CN 108732282A
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- 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
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- G—PHYSICS
- G01—MEASURING; TESTING
- G01N—INVESTIGATING OR ANALYSING MATERIALS BY DETERMINING THEIR CHEMICAL OR PHYSICAL PROPERTIES
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Abstract
The invention belongs to edible oil detection technique fields, are specifically related to the detection method of ethylene oxidic ester in a vegetable oil.The ethylene oxidic ester in vegetable oil is extracted by the derivative step of ring-opening reaction, hydrolysis, purification reaction and sample, then the content of ethylene oxidic ester is detected using gas chromatography-mass spectrography；Chromatographic test strip part is when gas chromatography-mass spectrography detects：Chromatographic column is the HP-5MS columns of 30m × 0.25mm × 0.25um, and chromatographic column temperature program is 85 DEG C of holding 12min, rises to 165 DEG C with 20 DEG C/min speed, keeps 10min, then rise to 300 DEG C with the speed of 20 DEG C/min, and keep 8min.The gas chromatography-mass spectrography of ethylene oxidic ester significantly improves the sensitivity of detection method by the optimization to instrument condition and pre-treating method in the detection corn oil that the present invention establishes, and detection method is simple and fast, reliable and stable.
Description
Technical field
The invention belongs to edible oil detection technique fields, are specifically related to the detection side of ethylene oxidic ester in a vegetable oil
Method.
Background technology
Ethylene oxidic ester is found to be present in food grease, is potential insecurity.Ethylene oxidic ester is a kind of
Industrial chemical has genotoxicity, can cause the formation of malignant tumour, ethylene oxidic ester amount in vegetable oil after use
It is smaller, there is certain thermal instability.Ethylene oxidic ester in food of the foreign countries to animal and plant fat and containing animal and plant fat
Research gradually increase, but domestic there has been no the report studied about ethylene oxidic ester in grease, the purpose largely studied is
The detection method for establishing an effective ethylene oxidic ester, in order in depth study the formation mechenism of ethylene oxidic ester and take
Corresponding measure is to reduce the content of ethylene oxidic ester in edible oil and fat.
Invention content
The purpose of the present invention is overcome the deficiencies of the prior art and provide the detection side of ethylene oxidic ester in a vegetable oil
Method.This method is easy to operate, and accuracy is high, safe and economical and practical.
The detection method of ethylene oxidic ester is by ring-opening reaction, hydrolysis, purification in vegetable oil of the present invention
The derivative step of reaction and sample extracts the ethylene oxidic ester in vegetable oil, then uses gas chromatography-mass spectrography to shrinking
The content of glyceride is detected；Chromatographic test strip part is when gas chromatography-mass spectrography detects：Chromatographic column is 30m × 0.25mm
The HP-5MS columns of × 0.25um, injector temperature are 250 DEG C, and chromatographic column temperature program is 85 DEG C of holding 12min, with 20 DEG C/min
Speed rises to 165 DEG C, keeps 10min, then rise to 300 DEG C with the speed of 20 DEG C/min, and keep 8min；Carrier gas is helium, no
Split sampling volume is 1.0uL, flow 1ml/min.
Wherein：
Ring-opening reaction：Into vegetable oil, the acidity of sodium bromide is added in addition internal standard substance solution, methyl tertiary butyl ether(MTBE) after being vortexed
Aqueous solution, after vortex by mixture at 45 DEG C -55 DEG C water bath with thermostatic control 10min-20min, sodium bicarbonate solution is added to terminate
N-hexane vortex is added into sample, centrifuges, upper layer is transferred in clean glass tube, 30 DEG C of -40 DEG C of nitrogen for reaction
Dry doubling is blown to be redissolved with methyl tertiary butyl ether(MTBE).
Hydrolysis：What is obtained to ring-opening reaction redissolves the mixed solution that sulfuric acid and methanol are added in solution, is vortexed to molten
Solution, then reacts 16h-17h at a temperature of 39-41 DEG C, after having reacted, saturated sodium bicarbonate solution is added into sample solution,
It is reacted with terminating, nitrogen is blown to 1ml-1.5ml at a temperature of 30 DEG C -40 DEG C, obtains liquid to be clean.
Wherein the mixed solution of sulfuric acid and methanol is in pipette, extract 1.8ml sulfuric acid to 100ml volumetric flasks and using first
Alcohol is settled to graduation mark.
Purification reaction：Metabisulfite solution and n-hexane are added in the liquid to be clean obtained to hydrolysis and mixes,
1200r-1250r centrifuges 2min-3min, and n-hexane is discarded after layering, abandons n-hexane after being used in combination n-hexane repeated washing primary
It goes；Then the mixed solution of ethyl acetate and ether is added toward aqueous layer, is centrifuged, upper solution is gone to equipped with anhydrous sulphur
In the centrifuge tube of sour magnesium, repeats extraction three times, be purified reaction extracting solution.
The derivative of sample：Phenylboric acid solution is added into purification reaction extracting solution, vortex 10s-15s stands 5min-
6min, nitrogen is blown to absolutely dry at 30 DEG C -40 DEG C, and n-hexane is then added and redissolves, and vortex 10s-15s is used immediately to abundant dissolving
Membrane filtration is transferred to gas chromatography-mass spectrum sample introduction bottle.
Internal standard substance solution in ring-opening reaction is chromatographically pure level isopropanol.
The content of ethylene oxidic ester in vegetable oil is detected using gas chromatography-mass spectrography, specifically includes following step
Suddenly：
(1) graticule is established
Different gradient standard specimens are configured, external standard, the same below sample treatment of internal standard are added into test tube；With ethylene oxidic ester external standard
Abscissa is done with target concentration ratio in ethylene oxidic ester, is done with ethylene oxidic ester external standard and target peak area ratio in ethylene oxidic ester
Ordinate makes linear equation；
It is designated as linoleic acid ethylene oxidic ester outside it；Inside it is designated as deuterated linoleic acid ethylene oxidic ester.
(2) it calculates
Ethylene oxidic ester result
Wherein：
Chromatographic test strip part is when gas chromatography-mass spectrography detects：Chromatographic column is the HP- of 30m × 0.25mm × 0.25um
5MS columns；Injector temperature is 250 DEG C；Chromatographic column temperature program is 85 DEG C of holding 12min, and 165 are risen to 20 DEG C/min speed
DEG C, 10min is kept, then 300 DEG C are risen to the speed of 20 DEG C/min, and keep 8min；Carrier gas is helium；Splitless injecting samples volume
For 1.0uL, flow 1ml/min.
Mass Spectrometer Method condition is when gas chromatography-mass spectrography detects：Ion source is electron impact mode (EI), transmission line temperature
Degree is 300 DEG C, 230 DEG C of ion source temperature；150 DEG C of mass spectrograph level four bars mass analyzer temperature, solvent delay 7min；Select from
Sub- monitoring pattern (SIM) parameter is the phenyl boronic acid derivative (m/z) 240 (quota ion) of 1.3-MBPD；147；242；It is (qualitative
Ion)；2.3-MBPD-d5 phenyl boronic acid derivative (m/z) 245 (quota ion)；150；247 (qualitative ions).
In formula described in step (2) in X representing samples ethylene oxidic ester mass fraction, A240Indicate glycidol
The corresponding peak area of ester external standard derivative, A245Indicate that the corresponding peak area of ethylene oxidic ester internal standard derivative, IS are indicated to be added and be waited for
Internal standard absolute magnitude in sample, W indicate to wait for that the quality of test sample, a indicate that the slope of ethylene oxidic ester standard curve, b indicate contracting
The intercept of water glyceride standard curve.
As a preferred technical solution, the detection method of ethylene oxidic ester in vegetable oil of the present invention, specifically
Include the following steps：
(1) ring-opening reaction：100mg (± 0.01mg) vegetable oil is weighed first with in screw-topped glass tube, is distinguished
60ul internal standard substance solutions are added, add 2.0ml methyl tertiary butyl ether(MTBE)s, the acid of 30ul sodium bromides is added into sample by vortex 10s
Property aqueous solution, after vortex by mixture on 50 DEG C of large capacity isothermal vibration devices water bath with thermostatic control 15min, be added 3ml's 0.6%
2ml n-hexane vortex 15s are added into sample to terminate reaction for sodium bicarbonate solution, centrifuge, upper layer is transferred to totally
Glass tube in, 35 DEG C of nitrogen be blown to it is dry, be used in combination 1ml methyl tertiary butyl ether(MTBE)s redissolve.
(2) hydrolysis：1.8ml sulfuric acid/methanol solution is added in solution toward redissolving, vortex 10s is to being completely dissolved, then
It places it on shaking table and reacts 16h at a temperature of 39-41 DEG C, after having reacted, 0.5ml unsaturated carbonate hydrogen is added into sample solution
Sodium solution, vortex 10s, to terminate reaction.Nitrogen is blown to 1ml or so at a temperature of 35 DEG C, to remove the organic solvent in solution, so
It is to be clean afterwards.
(3) purification reaction：2ml metabisulfite solutions and 2ml n-hexanes are sequentially added into liquid to be clean, vortex 10s is abundant
It is uniformly mixed, 1200r centrifuges 2min, and n-hexane is discarded after being layered, and n-hexane repeated washing is used in combination, and once (n-hexane needs whole
It discards).Then 1ml ethylacetate/ether mixed solutions are added toward aqueous layer, vortex 10s is mixed well, and is centrifuged, and upper layer is molten
Liquid is gone in the centrifuge tube equipped with a small amount of anhydrous magnesium sulfate, is repeated extraction three times, is waited for derivative reaction.
(4) derivatization reaction：200ul phenylboric acid solution is added into purification reaction extracting solution, vortex 10s stands 5min.
35 DEG C of nitrogen are blown to absolutely dry, and 500ul n-hexanes are then added and redissolve, vortex 10s is shifted with membrane filtration immediately to abundant dissolving
To sample introduction bottle (band interpolation pipe).
(5) graticule is established：Different gradient standard specimens (500ppb, 2ppm, 4ppm, 8ppm, 12ppm, 15ppm) are configured, to examination
60ul external standards, the same below sample treatment of 60ul internal standards are added in pipe；It is dense with ethylene oxidic ester external standard and target in ethylene oxidic ester
Degree ratio does abscissa, does ordinate with target peak area ratio in ethylene oxidic ester external standard and ethylene oxidic ester, makes linear equation.
(6) result calculates：Ethylene oxidic ester result calculates
In the step (5), into standard specimen a concentration of 98ppm；It is diluted successively with n-hexane, is configured to different ladders
Degree.
1 ethylene oxidic ester standard curve table of table
Fig. 3 is the standard curve of ethylene oxidic ester in the present invention；With target in ethylene oxidic ester external standard and ethylene oxidic ester
Peak area ratio is ordinate, using target concentration ratio in ethylene oxidic ester external standard and ethylene oxidic ester as abscissa, it follows that mark
Directrix curve functional relation is y=0.6225x+0.2228, linearly dependent coefficient R2=0.9993；This shows that standard curve has
Preferable linear dependence；IS is definite value 0.12, it follows that a 0.6225；B is 0.2228.
In the step (6), the mass fraction of ethylene oxidic ester, (unit mg/kg) in X-- samples
A240The corresponding peak area of-ethylene oxidic ester external standard derivative (m/z 240)；
A245The corresponding peak area of-ethylene oxidic ester internal standard derivative (m/z 245)；
Internal standard absolute magnitude (ug) in IS-addition sample to be tested；
W-waits for the quality (g) of test sample；
The slope of a-ethylene oxidic ester standard curve；
The intercept of b-ethylene oxidic ester standard curve.
Compared with prior art, the present invention having the advantages that：
The gas chromatography-mass spectrography of ethylene oxidic ester in the detection corn oil that the present invention establishes, by instrument condition and
The optimization of pre-treating method significantly improves the sensitivity of detection method, and detection method is simple and fast, reliable and stable.
Description of the drawings
Fig. 1 is the gas chromatography-mass spectrum figure of embodiment 1；
Fig. 2 is the gas chromatography-mass spectrum figure of embodiment 2；
Fig. 3 is the canonical plotting of ethylene oxidic ester in the present invention.
Specific implementation mode
The invention will be further described with reference to embodiments.
Embodiment 1
(1) 0.1083g corn oils are weighed first with in screw-topped glass tube, and it is molten to be separately added into 60ul internal standard compounds
Liquid, adds 2.0ML methyl tertiary butyl ether(MTBE)s, vortex 10s, is added the acidic aqueous solution of 30ul sodium bromides into sample, after vortex
By mixture on 50 DEG C of large capacity isothermal vibration devices water bath with thermostatic control 15min, be added 0.6% sodium bicarbonate solutions of 3ml to terminate
2ml n-hexane vortex 15s are added into sample for reaction, centrifuge, upper layer are moved in dry glass tube, 35 DEG C of nitrogen are blown
To doing, 1ml methyl tertiary butyl ether(MTBE)s is used in combination to redissolve.
(2) 1.8ml sulfuric acid/methanol solution is added into redissolution solution, then vortex 10s is placed it in being completely dissolved
16h is reacted at a temperature of 40 ± 1 DEG C on shaking table, after having reacted, 0.5ml saturated sodium bicarbonate solutions are added into sample solution,
Vortex 10s, to terminate reaction.Nitrogen is blown to 1ml or so at a temperature of 35 DEG C, to remove the organic solvent in solution, then waits for net
Change.
(3) 2ml metabisulfite solutions and 2ml n-hexanes are sequentially added into liquid to be clean, vortex 10s is sufficiently mixed uniformly,
1200r centrifuges 2min, and n-hexane is discarded after being layered, and is used in combination n-hexane repeated washing primary (n-hexane need to be discarded all).So
1ml ethylacetate/ether mixed solutions are added toward aqueous layer afterwards, vortex 10s is mixed well, and centrifuges, upper solution is gone to dress
In the centrifuge tube for having a small amount of anhydrous magnesium sulfate, repeats extraction three times, wait for derivative reaction.
(4) 200ul phenylboric acid solution is added into purification reaction extracting solution, vortex 10s stands 5min.35 DEG C of nitrogen are blown
It is extremely absolutely dry, 500ul n-hexanes are then added and redissolve, vortex 10s is transferred to sample introduction bottle with membrane filtration immediately to abundant dissolving
(band interpolation pipe) sample introduction carries out chromatography-mass spectroscopy detection, from spectrogram it can be seen that A240It is 7015.58；A245It is 19657.29；Therefore
X=0.239.
Embodiment 2
(1) 0.1108g corn oils are weighed first with in screw-topped glass tube, and it is molten to be separately added into 60ul internal standard compounds
Liquid, adds 2.0ML methyl tertiary butyl ether(MTBE)s, vortex 10s, is added the acidic aqueous solution of 30ul sodium bromides into sample, after vortex
By mixture on 50 DEG C of large capacity isothermal vibration devices water bath with thermostatic control 15min, be added 0.6% sodium bicarbonate solutions of 3ML to terminate
2ML n-hexane vortex 15s are added into sample for reaction, centrifuge, upper layer are moved in dry glass tube, 35 DEG C of nitrogen are blown
To doing, 1ML methyl tertiary butyl ether(MTBE)s is used in combination to redissolve.
(2) 1.8ml sulfuric acid/methanol solution is added into redissolution solution, then vortex 10s is placed it in being completely dissolved
16h is reacted at a temperature of 40 ± 1 DEG C on shaking table, after having reacted, 0.5ml saturated sodium bicarbonate solutions are added into sample solution,
Vortex 10s, to terminate reaction.Nitrogen is blown to 1ml or so at a temperature of 35 DEG C, to remove the organic solvent in solution, then waits for net
Change.
(3) 2ml metabisulfite solutions and 2ml n-hexanes are sequentially added into liquid to be clean, vortex 10s is sufficiently mixed uniformly,
1200r centrifuges 2min, and n-hexane is discarded after being layered, and is used in combination n-hexane repeated washing primary (n-hexane need to be discarded all).So
1ml ethylacetate/ether mixed solutions are added toward aqueous layer afterwards, vortex 10s is mixed well, and centrifuges, upper solution is gone to dress
In the centrifuge tube for having a small amount of anhydrous magnesium sulfate, repeats extraction three times, wait for derivative reaction.
(4) 200ul phenylboric acid solution is added into purification reaction extracting solution, vortex 10s stands 5min.35 DEG C of nitrogen are blown
It is extremely absolutely dry, 500ul n-hexanes are then added and redissolve, vortex 10s is transferred to sample introduction bottle with membrane filtration immediately to abundant dissolving
(band interpolation pipe) sample introduction carries out chromatography-mass spectroscopy detection, from spectrogram it can be seen that A240It is 6975.52；A245It is 22054.81；Therefore
X=0.163.
Claims (9)
1. the detection method of ethylene oxidic ester in a vegetable oil, it is characterised in that：Pass through ring-opening reaction, hydrolysis, purification
The derivative step of reaction and sample extracts the ethylene oxidic ester in vegetable oil, then uses gas chromatography-mass spectrography to shrinking
The content of glyceride is detected；Chromatographic test strip part is when gas chromatography-mass spectrography detects：Chromatographic column is 30m × 0.25mm
The HP-5MS columns of × 0.25um, injector temperature are 250 DEG C, and chromatographic column temperature program is 85 DEG C of holding 12min, with 20 DEG C/min
Speed rises to 165 DEG C, keeps 10min, then rise to 300 DEG C with the speed of 20 DEG C/min, and keep 8min；Carrier gas is helium, no
Split sampling volume is 1.0uL, flow 1ml/min.
2. the detection method of ethylene oxidic ester in vegetable oil according to claim 1, it is characterised in that：Ring-opening reaction：To
The acidic aqueous solution of sodium bromide is added in addition internal standard substance solution, methyl tertiary butyl ether(MTBE) in vegetable oil after being vortexed, will mixing after vortex
Object water bath with thermostatic control 10min-20min at 45 DEG C -55 DEG C, be added sodium bicarbonate solution terminate reaction, be added into sample just oneself
Alkane is vortexed, and centrifuges, upper layer is transferred in clean glass tube, 30 DEG C of -40 DEG C of nitrogen are blown to dry doubling methyl tertbutyl
Ether redissolves.
3. the detection method of ethylene oxidic ester in vegetable oil according to claim 1, it is characterised in that：Hydrolysis：To
What ring-opening reaction obtained redissolves the mixed solution that sulfuric acid and methanol are added in solution, is vortexed to dissolving, then in 39-41 DEG C of temperature
Lower reaction 16h-17h, after having reacted, saturated sodium bicarbonate solution is added into sample solution, is reacted with terminating, 30 DEG C -40 DEG C
At a temperature of nitrogen be blown to 1ml-1.5ml, obtain liquid to be clean.
4. the detection method of ethylene oxidic ester in vegetable oil according to claim 1, it is characterised in that：Purification reaction：To
Metabisulfite solution and n-hexane are added in the liquid to be clean that hydrolysis obtains and mixes, 1200r-1250r centrifuges 2min-
3min discards n-hexane after layering, all discards n-hexane after being used in combination n-hexane repeated washing primary；Then add toward aqueous layer
Enter the mixed solution of ethyl acetate and ether, centrifuged after mixing, upper solution is gone in the centrifuge tube equipped with anhydrous magnesium sulfate,
It repeats extraction three times, is purified reaction extracting solution.
5. the detection method of ethylene oxidic ester in vegetable oil according to claim 1, it is characterised in that：The derivative of sample：
Phenylboric acid solution is added into purification reaction extracting solution, vortex 10s-15s stands 5min-6min, nitrogen at 30 DEG C -40 DEG C
Be blown to it is absolutely dry, then be added n-hexane redissolve, vortex 10s-15s to dissolve, with membrane filtration be transferred to gas chromatography-mass spectrum into
Sample bottle.
6. the detection method of ethylene oxidic ester in vegetable oil according to claim 1, it is characterised in that：Using gas phase color
Spectrum-mass spectrography, which is detected the content of ethylene oxidic ester in vegetable oil, to be included the following steps：
(1) graticule is established
Different gradient standard specimens are configured, external standard, the same below sample treatment of internal standard are added into test tube；With ethylene oxidic ester external standard and contracting
Target concentration ratio does abscissa in water glyceride, and vertical seat is done with target peak area ratio in ethylene oxidic ester external standard and ethylene oxidic ester
Mark makes linear equation；
(2) it calculates
Ethylene oxidic ester result
7. the detection method of ethylene oxidic ester in vegetable oil according to claim 2, it is characterised in that：Institute in ring-opening reaction
The internal standard substance solution stated is chromatographically pure level isopropanol.
8. the detection method of ethylene oxidic ester in vegetable oil according to claim 6, it is characterised in that：Gas-chromatography-matter
Mass Spectrometer Method condition is when spectrometry detects：Ion source is electron impact mode, and transmission line temperature is 300 DEG C, ion source temperature 230
DEG C, 150 DEG C of mass spectrograph level four bars mass analyzer temperature, solvent delay 7min.
9. the detection method of ethylene oxidic ester in vegetable oil according to claim 6, it is characterised in that：Institute in step (2)
In the formula stated in X representing samples ethylene oxidic ester mass fraction, A240Indicate the corresponding peak of ethylene oxidic ester external standard derivative
Area, A245Indicate that the corresponding peak area of ethylene oxidic ester internal standard derivative, IS indicate that the internal standard being added in sample to be tested is absolute
Amount, W indicate to wait for that the quality of test sample, a indicate that the slope of ethylene oxidic ester standard curve, b indicate ethylene oxidic ester standard curve
Intercept.
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Cited By (3)
| Publication number | Priority date | Publication date | Assignee | Title |
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| CN110308218A (en) * | 2019-05-31 | 2019-10-08 | 浙江大学 | Evaluate the hemoglobin adduct detection method and application of exposure in glycidol and its ester body |
| CN112255349A (en) * | 2020-10-14 | 2021-01-22 | 青岛天祥食品集团有限公司 | Rapid detection method for detecting glycidol and glycidyl ester in edible vegetable oil |
| RU2789504C1 (en) * | 2022-01-12 | 2023-02-03 | Федеральное государственное бюджетное учреждение "Всероссийский государственный Центр качества и стандартизации лекарственных средств для животных и кормов" (ФГБУ "ВГНКИ") | Method for preparing food samples for the quantitative determination of the content of 3-monochloropropanediol (3-mcpd) and glycidol by gas-liquid chromatography with mass spectrometric detection (gc-ms) |
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Cited By (4)
| Publication number | Priority date | Publication date | Assignee | Title |
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| CN110308218A (en) * | 2019-05-31 | 2019-10-08 | 浙江大学 | Evaluate the hemoglobin adduct detection method and application of exposure in glycidol and its ester body |
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| CN112255349A (en) * | 2020-10-14 | 2021-01-22 | 青岛天祥食品集团有限公司 | Rapid detection method for detecting glycidol and glycidyl ester in edible vegetable oil |
| RU2789504C1 (en) * | 2022-01-12 | 2023-02-03 | Федеральное государственное бюджетное учреждение "Всероссийский государственный Центр качества и стандартизации лекарственных средств для животных и кормов" (ФГБУ "ВГНКИ") | Method for preparing food samples for the quantitative determination of the content of 3-monochloropropanediol (3-mcpd) and glycidol by gas-liquid chromatography with mass spectrometric detection (gc-ms) |
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