CN106501416A - A kind of plastic that determines is with food ethylene oxide and the method for acetaldehyde residual quantity - Google Patents
A kind of plastic that determines is with food ethylene oxide and the method for acetaldehyde residual quantity Download PDFInfo
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Abstract
The present invention relates to a kind of method for determining plastic ethylene oxide and acetaldehyde residual quantity and food ethylene oxide residual quantity, comprises the following steps：1) plastic or food samples are crushed and mix homogeneously, weighs appropriate in ml headspace bottle, added a cover；2) determine in plastic sample whether contain in oxirane and acetaldehyde and food samples whether contain oxirane using static headspace-GC-MS combined instrument：If gaschromatographic mass spectrometry selects ion scan result to show that sample is doubtful containing sometimes, whether the abundance of ions and retention time of comparative sample and oxirane and acetaldehyde standard substance, contain oxirane and acetaldehyde in confirmatory sample；If 3) contain in confirmatory sample, its content is calculated by formula.Compared with the existing technology, method is quick, simple, and the food samples suitable for heterogeneity, can prevent from having undesirable effect consumer health containing oxirane and the plastic of acetaldehyde and the food containing oxirane from source for the present invention.
Description
[technical field]
The invention belongs to technical field of analytical chemistry, specifically a kind of measure plastic ethylene oxide and acetaldehyde
Residual quantity and the method for food ethylene oxide residual quantity.
[background technology]
Oxirane is ethylene oxide, is a kind of poisonous carcinogen, and its No. CAS is 75-21-8.It is ethylene industry
The important Organic chemical products of polyethylene and polrvinyl chloride are only second in derivant.The inverted life of oxirane in the whole world about 60%
The monomer ethylene glycol of polyester fiber, resin and antifreezing agent is produced into, there are about 13% is used for producing other polyhydric alcohol.Oxirane
Second largest purposes is ethoxy compound of the production for detergent industry.In addition, it may also be used for production fumigant and disinfectant.
Oxirane is applied for a long time in the industry of sterilization and sterilizing, be obtain so far universally acknowledged most reliable
Gaseous sterilant.The scope being related to, such as non-woven fabrics, cotton, paper-plastic packing bag, rigid container, medical devices, paper bag etc..Due to
The vapour pressure of oxirane is larger, and the penetration power to article is strong, therefore can penetrate the deep that micropore reaches article.Plastic
The oxirane of middle residual mostly is residual or sterilization residual in production process, and the source of food ethylene oxide mostly packaging material is residual
The migration that stays.
Acetaldehyde also known as acetaldehyde, are two carbon saturated aldehydes with greater activity, and its No. CAS is 75-07-0.Domestic production
Acetaldehyde is substantially all the intermediate as production acetic acid, is only used on a small quantity producing tetramethylolmethane, butanol, Chloral, three hydroxyls
The products such as methylpropane.It has been proved that acetaldehyde is a kind of powerful myotoxin, its toxicity is for British kings science institute
30 times of ethanol.The contact of low concentration can cause skin and gastrointestinal to stimulate, and Long Term Contact can cause chronic poisoning.Plastics
There is the reaction such as oxidation and degraded into branch in some of product, discharge acetaldehyde.Additionally, high temperature can cause and accelerate acetaldehyde
Release.The clear stipulaties such as France, Italy, Switzerland, the food contact material of PET materials, acetaldehyde migration in food simulants
Amount must not exceed 6mg/kg.
[content of the invention]
Present invention aim to solving above-mentioned deficiency and providing a kind of plastic that determines with epoxy second in food
Alkane and the method for acetaldehyde residual quantity, the method are quick, simple, and the food samples suitable for heterogeneity, can be from source
Prevent from having undesirable effect consumer health containing oxirane and the plastic of acetaldehyde and the food containing oxirane.
Design a kind of method for determining plastic ethylene oxide and acetaldehyde residual quantity for achieving the above object, including with
Lower step：
1) sample pretreatment：By plastic sample comminution mix homogeneously, weigh appropriate in ml headspace bottle, add a cover；
2) using static headspace-GC-MS combined instrument determination step 1) in the sample of gained whether containing oxirane and
Acetaldehyde：If gaschromatographic mass spectrometry selects ion scan result to show that sample is doubtful containing oxirane and during acetaldehyde, comparative sample
Abundance of ions and the retention time of product and oxirane and acetaldehyde standard substance, with confirmatory sample whether containing oxirane and
Acetaldehyde；
If 3) in confirmatory sample containing oxirane and acetaldehyde, by formula calculating sample ethylene oxide and acetaldehyde
Content.
Further, step 1) in, granule mix homogeneously by plastic sample comminution into particle diameter less than 2mm.
Further, step 2) in, the condition determination of static headspace-GC-MS combined instrument is：1) head-space sampler is arranged
Condition is：Quantitative loop volume is 1mL, and the filling time is 0.2min, and equilibration time is 0.02min, and temperature is 100 DEG C, during sample introduction
Between be 1min, Sample equilibration time is 60min, and pressing time is 1min, and bottle pressure is 16psi, and gas chromatogram circulation time is
30min, furnace temperature are 90 DEG C, and transmission line temperature is 110 DEG C；2) gas chromatographic column specification is：Column length 60m, column internal diameter 0.32mm, apply
Film thickness is 0.25 μm；3) heating schedule is：Initial temperature is 40 DEG C, and then 20 DEG C/min rises to 200 DEG C, keeps 2min, then 2
DEG C/min rises to 206 DEG C, keeps 4min, then 10 DEG C/min rises to 250 DEG C, keeps 4min, and flow velocity is 1mL/min, injection port temperature
Spend for 250 DEG C, split ratio 1：1；4) mass spectrum ionization source adopts electron bombardment ionization source, and ion source temperature is 230 DEG C, and level Four bar quality is selected
Device is selected, temperature is 150 DEG C, and transmission line temperature is 250 DEG C, sweep limitss are m/z25-100, and SIM model selections ion is m/
z29、m/z43、m/z44.
Further, step 2) in, retouch in mass spectrum in the selection ion of sample, concern as to whether containing oxirane and second
Characteristic ion m/z29, m/z43, m/z44 of aldehyde standard substance, and compare their abundance ratios and retention time in the sample and be
No identical with oxirane and acetaldehyde standard substance, when containing in sample chromatogram figure oxirane and acetaldehyde position gained chromatographic peak
Above-mentioned whole 3 characteristic ions, and abundance ratio with retention time with oxirane and identical acetaldehyde standard substance when, then confirm sample
Containing oxirane and acetaldehyde in product.
Further, step 3) in, using standard curve quantified by external standard method, according to instrument readings and sample weighting amount, carry out ring
Oxidative ethane and the calculating of acetaldehyde residual quantity.
Present invention also offers a kind of method for determining food ethylene oxide residual quantity, it is characterised in that including following
Step：
1) sample pretreatment：Food samples are crushed and mix homogeneously, weighs appropriate in ml headspace bottle, added a cover；
2) 1) whether oxirane is contained in the sample of gained using static headspace-GC-MS combined instrument determination step：If
Gaschromatographic mass spectrometry select ion scan result show sample doubtful containing oxirane when, then comparative sample and oxirane mark
Whether the abundance of ions of quasi- material and retention time, contain oxirane in confirmatory sample；
If 3) contain oxirane in confirmatory sample, by the content of formula calculating sample ethylene oxide.Further
Ground, step 1) in, food samples are ground into granule of the particle diameter less than 2mm or homogenate.Further, step 2) in, static headspace gas
The condition determination of phase chromatograph-mass spectrometer is：1) head-space sampler setting condition is：Quantitative loop volume be 1mL, the filling time
For 0.2min, equilibration time is 0.02min, and temperature is 100 DEG C, and sample injection time is 1min, and Sample equilibration time is 60min, plus
The pressure time is 1min, and bottle pressure is 16psi, and gas chromatogram circulation time is 30min, and furnace temperature is 90 DEG C, and transmission line temperature is 110
℃；2) gas chromatographic column specification is：Column length 60m, column internal diameter 0.32mm, coating thickness are 0.25 μm；3) heating schedule is：Starting
40 DEG C of temperature, then 20 DEG C/min rise to 200 DEG C, keep 2min, then 2 DEG C/min rise to 206 DEG C, keep 4min, then 10 DEG C/
Min rises to 250 DEG C, keeps 4min, and flow velocity is 1mL/min, and injector temperature is 250 DEG C, split ratio 1：1；4) mass spectrum ionization source
Using electron bombardment ionization source, ion source temperature is 230 DEG C, level Four bar mass selector, and temperature is 150 DEG C, and transmission line temperature is 250
DEG C, sweep limitss are m/z25-100, and SIM model selections ion is m/z29, m/z43, m/z44.
Further, step 2) in, retouch in mass spectrum in the selection ion of sample, concern as to whether containing oxirane standard
Characteristic ion m/z29, m/z43, m/z44 of material, and compare their abundance ratios and retention time in the sample whether with ring
Identical in oxidative ethane standard substance, when in the gained chromatographic peak of sample chromatogram figure oxirane position containing above-mentioned whole 3 features from
Son, and abundance ratio identical with oxirane standard substance with retention time when, then contain oxirane in confirmatory sample.
Further, step 3) in, using standard curve quantified by external standard method, according to instrument readings and sample weighting amount, carry out ring
The calculating of oxidative ethane residual quantity.
The present invention is compared with the existing technology, there is provided a kind of sample need not be through solvent extraction, using headspace gas chromatography
The method that GC-MS determines plastic ethylene oxide and acetaldehyde residual quantity and food ethylene oxide residual quantity, should
Method is quick, simple, and the food samples suitable for heterogeneity, can prevent containing oxirane and acetaldehyde from source
Plastic and the food containing oxirane are had undesirable effect to consumer health.Meanwhile, invention creates plastics system
Product ethylene oxide and the qualitative and quantitative approach of acetaldehyde and food ethylene oxide, for plastic oxirane test limit
1mg/kg can be reached, acetaldehyde detection limit can reach 2.5mg/kg, 5mg/kg can be reached for food oxirane test limit.
[description of the drawings]
Fig. 1 is the gas chromatogram of 1 ethylene oxide of the embodiment of the present invention and acetaldehyde；
Fig. 2 is the mass spectrum of 1 ethylene oxide of the embodiment of the present invention；
Fig. 3 is the mass spectrum of acetaldehyde in the embodiment of the present invention 1.
[specific embodiment]
The invention belongs to epoxy in plastic ethylene oxide and acetaldehyde residual quantity and food in analytical chemistry field
The measure of ethane residual quantity, its principle is：Oxirane and acetaldehyde in sample reaches gas-solid equilibrium in ml headspace bottle, then by gas
Phase chromatograph-mass spectrometer determines content, by selection ion massspectrum figure characteristic ion and the abundance of comparative sample and standard substance
Than confirming to testing result with retention time.
The invention provides a kind of method for determining plastic ethylene oxide and acetaldehyde residual quantity, including following step
Suddenly：1) sample pretreatment：Granule mix homogeneously by plastic sample comminution into particle diameter less than 2mm, weighs appropriate in top
In empty bottle, add a cover；2) whether contain epoxy second using in static headspace-GC-MS combined instrument determination step 1) sample of gained
Alkane and acetaldehyde：If gaschromatographic mass spectrometry selects ion scan result to show that sample is doubtful containing oxirane and during acetaldehyde, compare
Compared with sample and the abundance of ions and retention time of oxirane and acetaldehyde standard substance, whether to contain epoxy second in confirmatory sample
Alkane and acetaldehyde；If 3) calculate sample ethylene oxide and acetaldehyde containing oxirane and acetaldehyde by formula in confirmatory sample
Content.
Above-mentioned steps 2) in, retouch in mass spectrum in the selection ion of sample, concern as to whether containing oxirane and acetaldehyde mark
Characteristic ion m/z29, m/z43, m/z44 of quasi- material, and compare their abundance ratios and retention time in the sample whether with
Oxirane is identical with acetaldehyde standard substance, above-mentioned when containing in sample chromatogram figure oxirane and acetaldehyde position gained chromatographic peak
Whole 3 characteristic ions, and abundance ratio with retention time with oxirane and identical acetaldehyde standard substance when, then in confirmatory sample
Containing oxirane and acetaldehyde.Further, step 3) in, using standard curve quantified by external standard method, according to instrument readings and title
Sample amount, carries out the calculating of oxirane and acetaldehyde residual quantity.
Present invention also offers a kind of method for determining food ethylene oxide residual quantity, comprises the following steps：1) sample
Pretreatment：Food samples are ground into granule of the particle diameter less than 2mm or homogenate mix homogeneously, are weighed in right amount in ml headspace bottle,
Add a cover；2) 1) whether oxirane is contained in the sample of gained using static headspace-GC-MS combined instrument determination step：If gas
Phase chromatographic mass spectrometry select ion scan result show sample doubtful containing oxirane when, then comparative sample and oxirane standard
Whether the abundance of ions of material and retention time, contain oxirane in confirmatory sample；If 3) contain epoxy in confirmatory sample
Ethane, then calculate the content of sample ethylene oxide by formula.
Above-mentioned steps 2) in, retouch in mass spectrum in the selection ion of sample, concern as to whether containing oxirane standard substance
Characteristic ion m/z29, m/z43, m/z44, and compare their abundance ratios and retention time in the sample whether with epoxy second
Identical in alkane standard substance, when in the gained chromatographic peak of sample chromatogram figure oxirane position contain above-mentioned whole 3 characteristic ions, and
When abundance ratio is identical with oxirane standard substance with retention time, then contain oxirane in confirmatory sample.Step 3) in, adopt
Standard curve quantified by external standard method is used, according to instrument readings and sample weighting amount, the calculating of residual ethylene oxide is carried out.
The condition determination of above-mentioned static headspace-GC-MS combined instrument is：1) head-space sampler setting condition is：Quantitative loop
Volume is 1mL, and the filling time is 0.2min, and equilibration time is 0.02min, and temperature is 100 DEG C, and sample injection time is 1min, sample
Equilibration time is 60min, and pressing time is 1min, and bottle pressure is 16psi, and gas chromatogram circulation time is 30min, and furnace temperature is 90
DEG C, transmission line temperature is 110 DEG C；2) gas chromatographic column specification is：Column length 60m, column internal diameter 0.32mm, coating thickness are 0.25 μ
m；3) heating schedule is：Initial temperature is 40 DEG C, and then 20 DEG C/min rises to 200 DEG C, keeps 2min, then 2 DEG C/min rises to 206
DEG C, 4min being kept, then 10 DEG C/min rises to 250 DEG C, keep 4min, flow velocity is 1mL/min, and injector temperature is 250 DEG C, shunting
Than 1：1；4) mass spectrum ionization source adopts electron bombardment ionization source, and ion source temperature is 230 DEG C, level Four bar mass selector, and temperature is 150
DEG C, transmission line temperature is 250 DEG C, and sweep limitss are m/z25-100, and SIM model selections ion is m/z29, m/z43, m/z44.
The present invention is made with reference to specific embodiment further explained below：
Embodiment 1：Plastic cup ethylene oxide and the measure of acetaldehyde residual quantity
1. the preparation of sample：
Plastic cup is crushed or is cut into granule of the particle diameter less than 2mm, the sample 1.0g for weighing mix homogeneously is pushed up in 20mL
In empty bottle, add a cover immediately.
2. instrument parameter is set：
1) head-space sampler condition
Head-space sampler：AgilentG1888
Quantitative ring body volume：1mL
Furnace temperature：90℃
Quantitative loop temperature：100℃
Transfer line temperature：110℃
GC circulation times：30min
Sample equilibration time：60min
Pressing time：1min
The quantitative loop filling time：0.20min
Quantitative loop equilibration time：0.02min
Sample injection time：1.00min
Bottle pressure：16psi
2) GC conditions
Gas chromatogram：Agilent,7890
Chromatographic column：Agilen,Gaspro,60m×0.32mm×0.25m
Column flow rate：1mL/min
Injector temperature：250℃
Split ratio：1:1
Temperature programming：40 DEG C of initial temperature, 20 DEG C/min are warmed up to 200 DEG C, keep 2min, 2 DEG C/min to be warmed up to 206
DEG C, keep 4min, 10 DEG C/min to be warmed up to 250 DEG C, keep 4min.
3) Mass Spectrometry Conditions
Mass spectrum：Agilent,5975C
Level Four bar temperature：150℃
Ion source temperature：230℃
Transmission line temperature：250℃
Scanning of the mass spectrum scope：25～100m/z
The solvent delay time：0.5min
SIM mode parameters set：m/z29、m/z43、m/z44
3. qualitative and quantitative：
1) qualitative
Compare with the retention time at standard substance peak through sample peak, sample peak mass spectrum is compared with standard substance mass spectrum
Compared with, confirming whether chromatographic peak retention time is consistent, corresponding chromatographic peak selects characteristic ion (m/z29, m/z43, m/ in ion spectrogram
Z44) and its whether abundance ratio is consistent, so that it is determined that whether detecting determinand in sample.
2) quantitative
Using standard curve quantified by external standard method.
4. calculate
According to instrument readings and sample weighting amount, the calculating of plastic cup ethylene oxide and acetaldehyde residual quantity is carried out.
Embodiment 2：The measure of packed Semen arachidis hypogaeae ethylene oxide residual quantity
1. the preparation of sample：
Semen arachidis hypogaeae is ground into granule of the particle diameter less than 2mm, the sample 0.1g of mix homogeneously is weighed in 20mL ml headspace bottles, is stood
Add a cover.
2. instrument parameter is set：
1) head-space sampler condition
Head-space sampler：AgilentG1888
Quantitative ring body volume：1mL
Furnace temperature：90℃
Quantitative loop temperature：100℃
Transfer line temperature：110℃
GC circulation times：30min
Sample equilibration time：60min
Pressing time：1min
The quantitative loop filling time：0.20min
Quantitative loop equilibration time：0.02min
Sample injection time：1.00min
Bottle pressure：16psi
2) GC conditions
Gas chromatogram：Agilent,7890
Chromatographic column：Agilen,Gaspro,60m×0.32mm×0.25m
Column flow rate：1mL/min
Injector temperature：250℃
Split ratio：1:1
Temperature programming：40 DEG C of initial temperature, 20 DEG C/min are warmed up to 200 DEG C, keep 2min, 2 DEG C/min to be warmed up to 206
DEG C, keep 4min, 10 DEG C/min to be warmed up to 250 DEG C, keep 4min.
3) Mass Spectrometry Conditions
Mass spectrum：Agilent,5975C
Level Four bar temperature：150℃
Ion source temperature：230℃
Transmission line temperature：250℃
Scanning of the mass spectrum scope：25～100m/z
The solvent delay time：0.5min
SIM mode parameters set：m/z29、m/z43、m/z44
3. qualitative and quantitative：
1) qualitative
Compare with the retention time at standard substance peak through sample peak, sample peak mass spectrum is compared with standard substance mass spectrum
Compared with, confirming whether chromatographic peak retention time is consistent, corresponding chromatographic peak selects characteristic ion (m/z29, m/z43, m/ in ion spectrogram
Z44) and its whether abundance ratio is consistent, so that it is determined that whether detecting determinand in sample.
2) quantitative
Using standard curve quantified by external standard method.
4. calculate
According to instrument readings and sample weighting amount, the calculating of Semen arachidis hypogaeae ethylene oxide residual quantity is carried out.
Embodiment 3：The measure of solid seasoning ethylene oxide residual quantity
1. the preparation of sample：
Flavouring agent is ground into granule of the particle diameter less than 2mm, the sample 0.1g of mix homogeneously is weighed in 20mL ml headspace bottles,
Add a cover immediately.
2. instrument parameter is set：
1) head-space sampler condition
Head-space sampler：AgilentG1888
Quantitative ring body volume：1mL
Furnace temperature：90℃
Quantitative loop temperature：100℃
Transfer line temperature：110℃
GC circulation times：30min
Sample equilibration time：60min
Pressing time：1min
The quantitative loop filling time：0.20min
Quantitative loop equilibration time：0.02min
Sample injection time：1.00min
Bottle pressure：16psi
2) GC conditions
Gas chromatogram：Agilent,7890
Chromatographic column：Agilen,Gaspro,60m×0.32mm×0.25m
Column flow rate：1mL/min
Injector temperature：250℃
Split ratio：1:1
Temperature programming：40 DEG C of initial temperature, 20 DEG C/min are warmed up to 200 DEG C, keep 2min, 2 DEG C/min to be warmed up to 206
DEG C, keep 4min, 10 DEG C/min to be warmed up to 250 DEG C, keep 4min.
3) Mass Spectrometry Conditions
Mass spectrum：Agilent,5975C
Level Four bar temperature：150℃
Ion source temperature：230℃
Transmission line temperature：250℃
Scanning of the mass spectrum scope：25～100m/z
The solvent delay time：0.5min
SIM mode parameters set：m/z29、m/z43、m/z44
3. qualitative and quantitative：
1) qualitative
Compare with the retention time at standard substance peak through sample peak, sample peak mass spectrum is compared with standard substance mass spectrum
Compared with, confirming whether chromatographic peak retention time is consistent, corresponding chromatographic peak selects characteristic ion (m/z29, m/z43, m/ in ion spectrogram
Z44) and its whether abundance ratio is consistent, so that it is determined that whether detecting determinand in sample.
2) quantitative
Using standard curve quantified by external standard method.
4. calculate
According to instrument readings and sample weighting amount, the calculating of material ethylene oxide residual quantity is seasoned.
The present invention is not limited by above-mentioned embodiment, other any spirit and principle without departing from the present invention
Lower made change, modification, replacement, combination, simplification, should be equivalent substitute mode, be included in the protection model of the present invention
Within enclosing.
Claims (10)
1. a kind of method for determining plastic ethylene oxide and acetaldehyde residual quantity, it is characterised in that comprise the following steps：
1) sample pretreatment：By plastic sample comminution mix homogeneously, weigh appropriate in ml headspace bottle, add a cover；
2) whether oxirane and acetaldehyde are contained using in static headspace-GC-MS combined instrument determination step 1) sample of gained：
If gaschromatographic mass spectrometry selects ion scan result to show that sample is doubtful containing oxirane and during acetaldehyde, comparative sample and ring
Whether the abundance of ions and retention time of oxidative ethane and acetaldehyde standard substance, contain oxirane and acetaldehyde in confirmatory sample；
If 3) in confirmatory sample containing oxirane and acetaldehyde, by containing for formula calculating sample ethylene oxide and acetaldehyde
Amount.
2. the method for claim 1, it is characterised in that：Step 1) in, plastic sample comminution is less than into particle diameter
The granule mix homogeneously of 2mm.
3. the method for claim 1, it is characterised in that step 2) in, the measure of static headspace-GC-MS combined instrument
Condition is：
1) head-space sampler setting condition is：Quantitative loop volume is 1mL, and the filling time is 0.2min, and equilibration time is
0.02min, temperature are 100 DEG C, and sample injection time is 1min, and Sample equilibration time is 60min, and pressing time is 1min, and bottle pressure is
16psi, gas chromatogram circulation time are 30min, and furnace temperature is 90 DEG C, and transmission line temperature is 110 DEG C；
2) gas chromatographic column specification is：Column length 60m, column internal diameter 0.32mm, coating thickness are 0.25 μm；
3) heating schedule is：Initial temperature is 40 DEG C, and then 20 DEG C/min rises to 200 DEG C, keeps 2min, then 2 DEG C/min rises to
206 DEG C, 4min is kept, then 10 DEG C/min rises to 250 DEG C, keep 4min, flow velocity is 1mL/min, and injector temperature is 250 DEG C,
Split ratio 1：1；
4) mass spectrum ionization source adopts electron bombardment ionization source, and ion source temperature is 230 DEG C, level Four bar mass selector, and temperature is 150
DEG C, transmission line temperature is 250 DEG C, and sweep limitss are m/z25-100, and SIM model selections ion is m/z29, m/z43, m/z44.
4. the method for claim 1, it is characterised in that：Step 2) in, retouch in mass spectrum in the selection ion of sample, close
Note whether characteristic ion m/z29, m/z43, m/z44 containing oxirane and acetaldehyde standard substance, and compare them in sample
In abundance ratio whether identical with oxirane and acetaldehyde standard substance with retention time, when sample chromatogram figure oxirane and
Contain above-mentioned whole 3 characteristic ions, and abundance ratio and retention time and oxirane and acetaldehyde in the gained chromatographic peak of acetaldehyde position
When standard substance is identical, then containing oxirane and acetaldehyde in confirmatory sample.
5. the method for claim 1, it is characterised in that：Step 3) in, using standard curve quantified by external standard method, according to instrument
Device reading and sample weighting amount, carry out the calculating of oxirane and acetaldehyde residual quantity.
6. a kind of determine food ethylene oxide residual quantity method, it is characterised in that comprise the following steps：
1) sample pretreatment：Food samples are crushed and mix homogeneously, weighs appropriate in ml headspace bottle, added a cover；
2) 1) whether oxirane is contained in the sample of gained using static headspace-GC-MS combined instrument determination step：If gas phase
Chromatographic mass spectrometry select ion scan result show sample doubtful containing oxirane when, then comparative sample and oxirane reference material
Whether the abundance of ions of matter and retention time, contain oxirane in confirmatory sample；
If 3) contain oxirane in confirmatory sample, by the content of formula calculating sample ethylene oxide.
7. method as claimed in claim 6, it is characterised in that：Step 1) in, food samples are ground into particle diameter less than 2mm's
Granule or homogenate.
8. method as claimed in claim 6, it is characterised in that step 2) in, the measure of static headspace-GC-MS combined instrument
Condition is：
1) head-space sampler setting condition is：Quantitative loop volume is 1mL, and the filling time is 0.2min, and equilibration time is
0.02min, temperature are 100 DEG C, and sample injection time is 1min, and Sample equilibration time is 60min, and pressing time is 1min, and bottle pressure is
16psi, gas chromatogram circulation time are 30min, and furnace temperature is 90 DEG C, and transmission line temperature is 110 DEG C；
2) gas chromatographic column specification is：Column length 60m, column internal diameter 0.32mm, coating thickness are 0.25 μm；
3) heating schedule is：40 DEG C of initial temperature, then 20 DEG C/min rise to 200 DEG C, keep 2min, then 2 DEG C/min rise to 206
DEG C, 4min being kept, then 10 DEG C/min rises to 250 DEG C, keep 4min, flow velocity is 1mL/min, and injector temperature is 250 DEG C, shunting
Than 1：1；
4) mass spectrum ionization source adopts electron bombardment ionization source, and ion source temperature is 230 DEG C, level Four bar mass selector, and temperature is 150
DEG C, transmission line temperature is 250 DEG C, and sweep limitss are m/z25-100, and SIM model selections ion is m/z29, m/z43, m/z44.
9. method as claimed in claim 6, it is characterised in that：Step 2) in, retouch in mass spectrum in the selection ion of sample, close
Note whether characteristic ion m/z29, m/z43, m/z44 containing oxirane standard substance, and compare their in the sample rich
Whether degree ratio is identical with oxirane standard substance with retention time, when sample chromatogram figure oxirane position gained chromatographic peak
In contain above-mentioned whole 3 characteristic ions, and abundance ratio identical with oxirane standard substance with retention time when, then confirmatory sample
In contain oxirane.
10. method as claimed in claim 6, it is characterised in that：Step 3) in, using standard curve quantified by external standard method, according to
Instrument readings and sample weighting amount, carry out the calculating of residual ethylene oxide.
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| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| CN201611125865.6A CN106501416A (en) | 2016-12-09 | 2016-12-09 | A kind of plastic that determines is with food ethylene oxide and the method for acetaldehyde residual quantity |
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| CN201611125865.6A CN106501416A (en) | 2016-12-09 | 2016-12-09 | A kind of plastic that determines is with food ethylene oxide and the method for acetaldehyde residual quantity |
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| CN (1) | CN106501416A (en) |
Cited By (3)
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| CN114527207A (en) * | 2022-01-26 | 2022-05-24 | 中联品检(佛山)检验技术有限公司 | System and method for detecting residual quantity of ethylene oxide in non-woven fabric |
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