CN102998387A - Method for determining ethylene glycol monomethyl ether, glycol ether, ethylene glycol ether acetate, glycol and diglycol in food wrap paper - Google Patents
Method for determining ethylene glycol monomethyl ether, glycol ether, ethylene glycol ether acetate, glycol and diglycol in food wrap paper Download PDFInfo
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Abstract
The invention discloses a method for determining ethylene glycol monomethyl ether, glycol ether, ethylene glycol ether acetate, glycol and diglycol in food wrap paper. The method disclosed by the invention comprises the following steps of: weighing and placing shredded food wrap paper into a container, adding a methanol extraction solution containing internal standard substances into the container, carrying out ultrasonic extraction, filtering extract liquor by virtue of a filter membrane, detecting filtrate by adopting a gas chromatography/mass spectrometer, monitoring in a selected ion mode and quantifying, and obtaining the contents of ethylene glycol monomethyl ether, glycol ether, ethylene glycol ether acetate, glycol and diglycol in the food wrap paper. The method disclosed by the invention has the advantages of simple pre-treatment, easiness in operation, good separating effect, accurate determination, short sample analysis time and high determination sensitivity and can realize accurate batch determination on five components in the food wrap paper at the same time.
Description
Technical field
The present invention relates to the Food Packaging technology field, be specially the method that detects glycol monoethyl ether, ethylene glycol monoethyl ether, ethyl cellosolve acetate, ethylene glycol, diethylene glycol in the food wrapper.
Background technology
Glycol monoethyl ether belongs to lower toxicity, can cause anemia, macrocyte disease, the new grain white blood cell occurs, causes the nervous centralis obstacle.Ethylene glycol monoethyl ether still can cause liver, kidney, lung damage except eye and respiratory tract are had the pungency, and hematological system changes, and genotoxicity and teratogenesis are arranged.Ethyl cellosolve acetate toxicity is very large, may cause that reproductive function is disorderly.
On July 1st, 1998, State Bureau of Environmental Protection, economic and commercial committee, Ministry of Foreign Trade and Economic Cooperation, Ministry of Public Security's dispatch ([1998] No. 089) provide " national Hazardous Waste List ", comprising materials such as ethylene glycol monomethyl ether, ethylene glycol ethyl ether and ester classes thereof.No. 255 files specify of calendar year 2001 health ministry: indoor coating bans use of the materials such as ethyl cellosolve acetate.In Dec, 2010, glycol monoethyl ether, ethylene glycol monoethyl ether are by European Union's rules " chemicals registration, assessment, license and restriction " (Regulationconcerning the Registration, Evaluation, Authorization and Restriction of Chemicals, REACH) list the 4th batch of degree of showing great attention to material (substance of Very high concern in, SVHC) inventory is classified as 2 class reproductive system toxicants.In June, 2011, ethyl cellosolve acetate is listed in the 5th batch of SVHC inventory by the REACH rules, also is classified as 2 class reproductive system toxicants.
Ethylene glycol belongs to the hypotoxicity material, but sucks, takes in or after skin absorbs health is harmful to, and can cause bronchitis, spasm, renal failure etc.The dangerous mixtures instruction 1999/45/EEC of European Union regulation forbids making spent glycol at articles for children such as toys.Because ethylene glycol very easily is brought in the toothpaste finished product as impurity with other raw material, China issued national standard " toothpaste raw material standard " (GB 22115-2008) in 2008 and provides against it as raw material of toothpaste, should be less than 0.1% with ethylene glycol and diethylene glycol sum that raw material is brought into.
After diethylene glycol oral administration or skin enter human body, can cause metabolic acidosis, anuria, acute renal failure, hepatocellular damage and serious neurology sequelae etc.Diethylene glycol worldwide repeatedly causes collective's acute poisoning event.On July 11st, 2007, State General Administration for Quality Supervision sends " about forbidding with the bulletin of diglycol as raw material of toothpaste ", requires to forbid containing the tooth paste product export and import of diglycol composition.Stipulated limiting the quantity of of the middle diglycol of glycerine (0.1% diglycol) and polyglycol (0.4% ethylene glycol and diglycol total amount) in the European Pharmacopoeia.European Union is clear in the instruction 2009/6/EEC of formal issue of in February, 2009, and the diglycol content in the cosmetics must not surpass 0.1%.
The detection method of the materials such as the glycol monoethyl ether of having reported, ethylene glycol monoethyl ether, ethyl cellosolve acetate, ethylene glycol, diethylene glycol mainly concentrates on the fields such as plastic products, toothpaste and cosmetics, waste water, coating, blood and biological tissue, employing mainly be vapor-phase chromatography or gas chromatography/mass spectrometry method.Country's inspection and quarantining for import/export industry standard (SN/T 2408-2009) adopts the gas chromatography mass spectrometry method that the migration amount of the materials such as ethylene glycol monoethyl ether in the toy is measured.For the mensuration of diglycol in the toothpaste, adopt gas chromatography and two kinds of methods of gas chromatography mass spectrometry, formulated " mensuration of diglycol in the toothpaste " (GB/T 21842-2008) national standard.And so far, there is not yet any bibliographical information and the patent that adopt the gas chromatography-mass spectrography method to measure simultaneously the materials such as glycol monoethyl ether in the food wrapper, ethylene glycol monoethyl ether, ethyl cellosolve acetate, ethylene glycol, diethylene glycol both at home and abroad.
Chinese patent CN200980154551.0 discloses " for detection of equipment and the method for glycol ", the method is utilized at alcohol dehydrogenase, ethylene glycol and diglycol and enzyme carry out multistep reaction, by being determined at the variation of light absorption or light fluorescence aspect, the ethylene glycol in mensuration household products and the medicine and the concentration of diglycol.Chinese patent CN201110080907.X discloses " detection method of a kind of glycol monoethyl ether, ethylene glycol monoethyl ether, glycol methyl ether acetate and ethylene glycol ether acetate ", the method adopts soxhlet extraction that solid sample (plastic products) is extracted 2～6h, adopt the ultrasonic extraction method that fluid sample is extracted 3～10h, be transferred to after extract is concentrated and adopt gas chromatography to separate in the volumetric flask behind the constant volume, hydrogen flame ionization detector is quantitative.The method can't realize the synchronous qualitative and quantitative analysis to object, determination complex steps, complexity, the use solvent is many, length consuming time, have a strong impact on analysis efficiency, and, only rely on retention time qualitative, the false positive problem also appears easily, be difficult to realize in the food wrapper when glycol monoethyl ether, ethylene glycol monoethyl ether, ethyl cellosolve acetate, ethylene glycol, five kinds of materials of diglycol, fast, Accurate Determining.
Along with the growing interest of the public to food-safety problem, the quality security problem of packaging material for food also becomes the focal issue that people pay close attention to, and it is on the knees of the gods that can existing detection method be applicable to the detection of glycol monoethyl ether in the packaging for foodstuff paper material, ethylene glycol monoethyl ether, ethyl cellosolve acetate, ethylene glycol, five kinds of compositions of diglycol.In view of this, set up a kind of can be simultaneously, detection method convenient, accurate, that measure glycol monoethyl ether in the packaging for foodstuff paper material, ethylene glycol monoethyl ether, ethyl cellosolve acetate, ethylene glycol, five kinds of materials of diglycol in batches has important realistic meaning.
Summary of the invention
The technical problem to be solved in the present invention provides a kind of method that detects glycol monoethyl ether in the food wrapper, ethylene glycol monoethyl ether, ethyl cellosolve acetate, ethylene glycol, diethylene glycol.The method pre-treatment is simple, easy operating, good separating effect, qualitative accurately, sample analysis time is short, detection sensitivity is high.
The invention provides a kind of method that detects glycol monoethyl ether in the food wrapper, ethylene glycol monoethyl ether, ethyl cellosolve acetate, ethylene glycol, diethylene glycol, may further comprise the steps:
Take by weighing broken food wrapper and place container, to wherein adding the methanol extraction solution that contains internal standard compound, ultrasonic extraction, extract is through membrane filtration, filtrate uses gas chromatograph/mass spectrometer to detect, internal standard method is adopted in choice ion pattern monitoring and quantitative, obtains the content of glycol monoethyl ether in the food wrapper, ethylene glycol monoethyl ether, ethyl cellosolve acetate, ethylene glycol, diethylene glycol.
Usually food wrapper to be detected is shredded and accurately take by weighing afterwards.Preferably, food wrapper is shredded into the fragment that is not more than 5mm * 5mm.
Further, described internal standard compound is phenylethyl propionate.
Further, the quality that takes by weighing of described food wrapper is 0.5～1.0g, and the volume of extraction solution is 10～20mL.Internal standard compound concentration is 0.05 μ g/mL.When using methanol extraction, ultrasonic getting final product at room temperature.Ultrasonic time 30～50min is advisable.
Can use triangular flask as container.The volume of triangular flask is 50～100mL.
Further, described filter membrane is the organic phase filter membrane, and specification is a kind of among 0.22 μ m, the 0.45 μ m.
Further, the condition that described use gas chromatograph/mass spectrometer detects is: adopt the DB-624 capillary chromatographic column to separate, 250 ℃ of injector temperatures, sample size 1 μ L, split ratio 1:10, post flow 1mL/min, heating schedule is: 120 ℃ keep 5min, rise to 240 ℃ with 30 ℃/min, keep 8min; The mass spectrum condition is: electron ionization sources (EI), ionization voltage 70eV, 230 ℃ of ion source temperatures; Level Four bar temperature is 150 ℃, and solvent delay 5min selects ion monitoring scan mode (SIM) quantitative; Quantitative and the qualitative selection ion of glycol monoethyl ether, ethylene glycol monoethyl ether, ethyl cellosolve acetate, ethylene glycol, diethylene glycol and internal standard compound sees Table 1 five kinds of compounds and the quantitative and qualitative selection ion of internal standard compound:
Five kinds of compounds of table 1 and the quantitative and qualitative selection ion of internal standard compound
Described DB-624 capillary chromatographic column is of a size of 60m * 0.32mm * 1.80 μ m.
A kind of method that detects glycol monoethyl ether in the food wrapper, ethylene glycol monoethyl ether, ethyl cellosolve acetate, ethylene glycol, diethylene glycol specifically may further comprise the steps:
1) takes food product wrapping paper sample, it is shredded into the fragment that is not more than 5mm * 5mm, mix;
2) accurately take by weighing about 0.5～1.0g sample, place triangular flask, adding 10～20mL internal standard compound concentration is the methanol extraction liquid of 0.05 μ g/mL, ultrasonic extraction 30～50min under the room temperature;
3) extract adopts gas chromatograph/mass spectrometer to detect behind membrane filtration:
Adopt the DB-624 capillary chromatographic column to separate, 250 ℃ of injector temperatures, sample size 1 μ L, split ratio 1:10, post flow 1mL/min, heating schedule is: 120 ℃ keep 5min, rise to 240 ℃ with 30 ℃/min, keep 8min; The mass spectrum condition is: electron ionization sources (EI), ionization voltage 70eV, 230 ℃ of ion source temperatures; Level Four bar temperature is 150 ℃, and solvent delay 5min selects ion monitoring scan mode (SIM) quantitative; Quantitative and the qualitative selection ion of glycol monoethyl ether, ethylene glycol monoethyl ether, ethyl cellosolve acetate, ethylene glycol, diethylene glycol and internal standard compound sees Table 1 five kinds of compounds and the quantitative and qualitative selection ion of internal standard compound:
Five kinds of compounds of table 1 and the quantitative and qualitative selection ion of internal standard compound
Further, calculate the content of glycol monoethyl ether in the food wrapper, ethylene glycol monoethyl ether, ethyl cellosolve acetate, ethylene glycol, diethylene glycol by following formula:
In the formula:
W---the content of component to be measured in the sample, unit is every kilogram (mg/kg) of milligram;
The peak area of A---component to be measured;
As---interior target peak area;
The intercept of b---working curve;
Ms---interior target quality in the sample solution, unit is microgram (μ g);
The slope of a---working curve;
The quality of M---sample, unit is gram (g).
The arithmetic mean of getting twice replicate determination result is final measurement result, is accurate to 0.01 milligram every kilogram (mg/kg).Twice replicate determination result's relative deviation should be not more than 10%.
The invention has the advantages that:
1, the present invention adopts the ultrasonic extraction of methanol extraction liquid, and extract is directly measured behind membrane filtration, and pre-treatment is simple, easy operating, and the solvent that uses is less, can effectively avoid the experimenter cruelly to leak for a long time in the organic solvent environment environmental protection;
2, instrument and the equipment of the present invention's use are laboratory conventional analysis equipment, and inventive method is easy to promote, and testing cost is lower;
3, the present invention adopts gas chromatography to separate first, mass spectral:mass spectrographic selection ion scan monitoring mode is quantitative, internal standard method is calculated glycol monoethyl ether, ethylene glycol monoethyl ether, ethyl cellosolve acetate, ethylene glycol, five kinds of content of material of diethylene glycol in the packaging for foodstuff paper material, when can realizing five kinds of materials, 16min measures, method weak point consuming time, highly sensitive, the recovery and repeatability satisfy fully analyzes requirement, can realize quick, accurate, batch detection to wrappage.
Description of drawings
Fig. 1 is the chromatogram of glycol monoethyl ether, ethylene glycol monoethyl ether, ethyl cellosolve acetate, ethylene glycol, diethylene glycol in the food wrapper that detects of embodiment 1.
Embodiment
The present invention will be described in more detail in following embodiment, but not limit the present invention.
Instrument of the present invention and reagent, material
6890N/5975 gas chromatograph-mass spectrometer (GCMS) (U.S. Agilent company) is equipped with automatic sampler, enhanced chemical workstation, has selection ion detection (SIM) function.KQ-500DE ultrasonic generator (Kunshan Ultrasonic Instruments Co., Ltd.); Electronic balance (METTLER TOLEDO company, sensibility reciprocal 0.1mg); 0.22 μ m, 0.45 μ m organic phase filter membrane; Fixing is the DB-624 capillary chromatographic column (60m * 0.32mm * 1.80 μ m) of 6% cyanogen propyl group phenyl/94% dimethyl polysiloxane mutually; Glass apparatus commonly used.
Methyl alcohol, chromatographically pure.Glycol monoethyl ether, ethylene glycol monoethyl ether, ethyl cellosolve acetate, ethylene glycol, diethylene glycol are analyzed pure.Phenylethyl propionate (CAS:122-70-3): interior mark, purity 〉=99%.
Reagent and solution preparation
Primary standard storing solution: take by weighing respectively 0.5g(and be accurate to 0.1mg) glycol monoethyl ether, ethylene glycol monoethyl ether, ethyl cellosolve acetate, ethylene glycol, diethylene glycol, place same 100mL volumetric flask, with methyl alcohol dissolving and constant volume, be mixed with the primary standard storing solution that each target substance concentration is 5mg/mL.
Secondary standard storing solution: accurately pipette 10mL primary standard storing solution, place the 100mL volumetric flask, with methanol constant volume, be mixed with the secondary standard storing solution that each target substance concentration is 0.5mg/mL.
Mark storing solution in the one-level: accurately take by weighing 10mg(and be accurate to 0.1mg) phenylethyl propionate in beaker with being transferred in the 100mL volumetric flask, with methanol constant volume after the methyl alcohol dissolving.
Extraction solution: accurately pipette in the one-level of 0.5mL the mark storing solution in the 1000mL volumetric flask, after the methanol constant volume as extraction solution.
Standard operation solution: accurately pipette the secondary standard storing solution of 0.01mL, 0.025mL, 0.05mL, 0.1mL, 0.25mL, 0.5mL, place the 100mL volumetric flask, use respectively the extraction solution constant volume, namely get the series standard working solution.The series standard solution concentration of preparation is: 0.1 μ g/mL, 0.25 μ g/mL, 0.5 μ g/mL, 1 μ g/mL, 2.5 μ g/mL, 5 μ g/mL.
A kind of method that detects glycol monoethyl ether in the food wrapper, ethylene glycol monoethyl ether, ethyl cellosolve acetate, ethylene glycol, diethylene glycol specifically may further comprise the steps:
1) takes food product wrapping paper sample, it is shredded into the fragment that is not more than 5mm * 5mm, mix;
2) accurately take by weighing about 0.5～1.0g sample, place 50～100mL triangular flask, adding 10～20mL internal standard compound concentration is the methanol extraction liquid of 0.05 μ g/mL, ultrasonic extraction 30min under the room temperature;
3) extract adopts gas chromatograph/mass spectrometer to detect behind membrane filtration:
Adopt DB-624 capillary chromatographic column (60m * 0.32mm * 1.80 μ m) to separate 250 ℃ of injector temperatures, sample size 1 μ L, split ratio 1:10, post flow 1mL/min, heating schedule is: 120 ℃ keep 5min, rise to 240 ℃ with 30 ℃/min, keep 8min; The mass spectrum condition is: electron ionization sources (EI), ionization voltage 70eV, 230 ℃ of ion source temperatures; Level Four bar temperature is 150 ℃, and solvent delay 5min selects ion monitoring scan mode (SIM) quantitative; Quantitative and the qualitative selection ion of glycol monoethyl ether, ethylene glycol monoethyl ether, ethyl cellosolve acetate, ethylene glycol, diethylene glycol and internal standard compound sees Table 1 five kinds of compounds and the quantitative and qualitative selection ion of internal standard compound:
Five kinds of compounds of table 1 and the quantitative and qualitative selection ion of internal standard compound
Calculate the content of glycol monoethyl ether in the food wrapper, ethylene glycol monoethyl ether, ethyl cellosolve acetate, ethylene glycol, diethylene glycol by following formula:
In the formula:
W---the content of component to be measured in the sample, unit is every kilogram (mg/kg) of milligram;
The peak area of A---component to be measured;
As---interior target peak area;
The intercept of b---working curve;
Ms---interior target quality in the sample solution, unit is microgram (μ g);
The slope of a---working curve;
The quality of M---sample, unit is gram (g).
The arithmetic mean of getting twice replicate determination result is final measurement result, is accurate to 0.01 milligram every kilogram (mg/kg).Twice replicate determination result's relative deviation should be not more than 10%.
Fig. 1 is the chromatogram of glycol monoethyl ether, ethylene glycol monoethyl ether, ethyl cellosolve acetate, ethylene glycol, diethylene glycol in the food wrapper that detects of embodiment 1.
Embodiment 2
According to the method for embodiment 1, take by weighing the 0.5g sample in the 50mL triangular flask, add the ultrasonic 30min of 10mL extract, extract is measured behind 0.22 μ m organic phase membrane filtration.A certain brand food wrapper is measured three times every day, continuous detecting three days, the experimental result that obtains is as shown in table 2 ethylene glycol repeated experiment result, table 3 diethylene glycol repeated experiment result.
Table 2 ethylene glycol repeated experiment result (mg/kg)
Table 3 diethylene glycol repeated experiment result (mg/kg)
From table 2 and table 3, can find out: the RSD＜5% of repeatability in a few days, in the daytime the RSD＜4% of repeatability, illustrate this method can the Accurate Measurement food wrapper in the content of glycol monoethyl ether, ethylene glycol monoethyl ether, ethyl cellosolve acetate, ethylene glycol, five kinds of materials of diethylene glycol.
Embodiment 3
Method according to embodiment 1, take by weighing the 1.0g sample in the 100mL triangular flask, add the ultrasonic 30min of 20mL extract, extract is measured behind 0.45 μ m organic phase membrane filtration, obtains the content of glycol monoethyl ether in the sample, ethylene glycol monoethyl ether, ethyl cellosolve acetate, ethylene glycol, five kinds of materials of diethylene glycol.Accurately add the mixed sample of five kinds of components to be measured in a certain brand food wrapper of known glycol monoethyl ether, ethylene glycol monoethyl ether, ethyl cellosolve acetate, ethylene glycol, five kinds of content of material of diethylene glycol, record five kinds of component concentration values to be measured under basic, normal, high three mark-on levels.Each horizontal parallel is measured three samples, averages and carries out the calculating of recovery of standard addition.Test result sees Table the recovery experimental result of 7 five kinds of components to be measured.
The recovery experimental result of five kinds of components to be measured of table 7
The result of table 7 shows that the recovery of glycol monoethyl ether is 100.76%-110.01%, the recovery of ethylene glycol monoethyl ether is 85.72%-104.07%, the recovery of ethyl cellosolve acetate is 80.72%-87.31%, the recovery of ethylene glycol is 97.95%-108.34%, the recovery of diethylene glycol is 102.71%-112.40%, the recovery that shows the inventive method is higher, satisfies the quantitative test requirement.
With the standard specimen continuous sample introduction of least concentration 10 times, count standard deviation by the concentration value that records, detectability (LOD) is tried to achieve with three times of standard deviations, the detectability of this method glycol monoethyl ether, ethylene glycol monoethyl ether, ethyl cellosolve acetate, ethylene glycol, five kinds of materials of diethylene glycol is respectively 0.028 μ g/mL, 0.024 μ g/mL, 0.014 μ g/mL, 0.037 μ g/mL and 0.038 μ g/mL, shows that the sensitivity of method is higher.
Embodiment 4
Method according to embodiment 1, glycol monoethyl ether, ethylene glycol monoethyl ether, ethyl cellosolve acetate, ethylene glycol and diethylene glycol in the packaging for foodstuff paper material of 20 kinds of different brands are measured, wherein detect diethylene glycol in 4 wrapping paper materials, 2 packaging for foodstuff paper material only detect ethylene glycol, and all brand packaging for foodstuff paper material all do not detect glycol monoethyl ether, ethylene glycol monoethyl ether and ethyl cellosolve acetate.Testing result is as shown in table 8 below:
The above embodiment of the present invention only is for example of the present invention clearly is described, is not the restriction to embodiments of the present invention.For those of ordinary skill in the field, can also make other changes in different forms on the basis of the above description.Here can't give all embodiments exhaustive.Everyly belong to the row that apparent variation that technical scheme of the present invention extends out or change still are in protection scope of the present invention.
Claims (10)
1. a method that detects glycol monoethyl ether in the food wrapper, ethylene glycol monoethyl ether, ethyl cellosolve acetate, ethylene glycol, diethylene glycol is characterized in that, may further comprise the steps:
Take by weighing broken food wrapper and place container, to wherein adding the methanol extraction solution that contains internal standard compound, ultrasonic extraction, extract is through membrane filtration, filtrate uses gas chromatograph/mass spectrometer to detect, internal standard method is adopted in choice ion pattern monitoring and quantitative, obtains the content of glycol monoethyl ether in the food wrapper, ethylene glycol monoethyl ether, ethyl cellosolve acetate, ethylene glycol, diethylene glycol.
2. method according to claim 1 is characterized in that, food wrapper is shredded into the fragment that is not more than 5mm * 5mm, obtains broken food wrapper.
3. method according to claim 1 is characterized in that, described internal standard compound is phenylethyl propionate.
4. method according to claim 1 is characterized in that, the quality that takes by weighing of described food wrapper is 0.5～1.0g, and the volume of extraction solution is 10～20mL.
5. method according to claim 1 is characterized in that, internal standard compound concentration is 0.05 μ g/mL.
6. method according to claim 1 is characterized in that, and is at room temperature ultrasonic, ultrasonic time 30～50min.
7. method according to claim 1 is characterized in that, described filter membrane is the organic phase filter membrane, and specification is a kind of among 0.22 μ m, the 0.45 μ m.
8. method according to claim 1, it is characterized in that, the condition that described use gas chromatograph/mass spectrometer detects is: adopt the DB-624 capillary chromatographic column to separate, 250 ℃ of injector temperatures, sample size 1 μ L, split ratio 1:10, post flow 1mL/min, heating schedule is: 120 ℃ keep 5min, rise to 240 ℃ with 30 ℃/min, keep 8min; The mass spectrum condition is: electron ionization sources (EI), ionization voltage 70eV, 230 ℃ of ion source temperatures; Level Four bar temperature is 150 ℃, and solvent delay 5min selects ion monitoring scan mode (SIM) quantitative; Quantitative and the qualitative selection ion of glycol monoethyl ether, ethylene glycol monoethyl ether, ethyl cellosolve acetate, ethylene glycol, diethylene glycol and internal standard compound sees the following form:
9. method according to claim 1 is characterized in that, specifically may further comprise the steps:
1) takes food product wrapping paper sample, it is shredded into the fragment that is not more than 5mm * 5mm, mix;
2) accurately take by weighing about 0.5～1.0g sample, place triangular flask, adding 10～20mL internal standard compound concentration is the methanol extraction liquid of 0.05 μ g/mL, ultrasonic extraction 30～50min under the room temperature;
3) extract adopts gas chromatograph/mass spectrometer to detect behind membrane filtration:
Adopt the DB-624 capillary chromatographic column to separate, 250 ℃ of injector temperatures, sample size 1 μ L, split ratio 1:10, post flow 1mL/min, heating schedule is: 120 ℃ keep 5min, rise to 240 ℃ with 30 ℃/min, keep 8min; The mass spectrum condition is: electron ionization sources (EI), ionization voltage 70eV, 230 ℃ of ion source temperatures; Level Four bar temperature is 150 ℃, and solvent delay 5min selects ion monitoring scan mode (SIM) quantitative; Quantitative and the qualitative selection ion of glycol monoethyl ether, ethylene glycol monoethyl ether, ethyl cellosolve acetate, ethylene glycol, diethylene glycol and internal standard compound sees the following form:
10. according to claim 1 or 9 described methods, it is characterized in that, calculate the content of glycol monoethyl ether in the food wrapper, ethylene glycol monoethyl ether, ethyl cellosolve acetate, ethylene glycol, diethylene glycol by following formula:
In the formula:
W---the content of component to be measured in the sample, unit is every kilogram (mg/kg) of milligram;
The peak area of A---component to be measured;
As---interior target peak area;
The intercept of b---working curve;
Ms---interior target quality in the sample solution, unit is microgram (μ g);
The slope of a---working curve;
The quality of M---sample, unit is gram (g).
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