CN109342616A - The detection method of amide substance content in a kind of food contact material - Google Patents
The detection method of amide substance content in a kind of food contact material Download PDFInfo
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- CN109342616A CN109342616A CN201811187035.5A CN201811187035A CN109342616A CN 109342616 A CN109342616 A CN 109342616A CN 201811187035 A CN201811187035 A CN 201811187035A CN 109342616 A CN109342616 A CN 109342616A
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- sample
- mass ratio
- amide substance
- contact material
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- G—PHYSICS
- G01—MEASURING; TESTING
- G01N—INVESTIGATING OR ANALYSING MATERIALS BY DETERMINING THEIR CHEMICAL OR PHYSICAL PROPERTIES
- G01N30/00—Investigating or analysing materials by separation into components using adsorption, absorption or similar phenomena or using ion-exchange, e.g. chromatography or field flow fractionation
- G01N30/02—Column chromatography
- G01N30/04—Preparation or injection of sample to be analysed
- G01N30/06—Preparation
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- G—PHYSICS
- G01—MEASURING; TESTING
- G01N—INVESTIGATING OR ANALYSING MATERIALS BY DETERMINING THEIR CHEMICAL OR PHYSICAL PROPERTIES
- G01N30/00—Investigating or analysing materials by separation into components using adsorption, absorption or similar phenomena or using ion-exchange, e.g. chromatography or field flow fractionation
- G01N30/02—Column chromatography
Abstract
The invention discloses a kind of detection methods of amide substance content in food contact material, comprising the following steps: chooses representative sample, is cut into the fragment less than the mm of 5 mm × 5, clean container is packed into after mixing as sample;Sample purification;GC-MS analysis detection;Calculation formula is obtained after making standard curve according to peak area;The peak area of target analytes in sample is substituted into formula to calculate the content of amide substance.Analysis detection is carried out to each prepare liquid using gas chromatography tandem mass spectrometry measurement, to obtain the respectively actual measured value to amide substance in test sample.Detection method has not only filled up technological gap of the China in food contact material in the detection of amide substance, and has the characteristics that easily operated and detection accuracy is high.
Description
Technical field
The present invention relates to amide substance contents in technical field of food safety more particularly to a kind of food contact material
Detection method.
Background technique
Amide substance is the important initial monomers such as plastics, paper, ink, coating and adhesive and additive, production
In frequently as synthesis starting material, lubricant, anti-adhesion agent, emulsifier, dispersing agent, stabilizer etc..It has been reported that and shows amide substance
It can be obstructed by polymer molecule, be entered in food in a manner of permeating, migrating etc. from ink, adhesive or plastic body,
The flavor of food is not only influenced, or even endangers the health of consumer.Thus, China, Japan, the U.S. and EU countries all promulgate phase
The regulation answered goes to limit the content of amide substance in food contact material.Currently, the amide substance generallyd use in the world
Mainly there are acrylamide, Methacrylamide, oleamide, stearmide and erucyl amide etc..Amide has thorn to organism
Swash property and acute toxicity, after this substance enters human body, may cause the damage of nerve, kidney and liver, even potentially
Carcinogen.For example, acrylamide is mainly neurotoxin, but the inhereditary material of animal somatic cell and reproduction cell can also be led
Acrylamide is classified as 2 class carcinogenic substances by the damage of cause, international cancer mechanism.Caprolactam low toxicity, main function and nervous centralis,
It can cause the material injury to internal organs such as brain stems.
Therefore, the high-throughput detection technique for establishing amides in food contact material has important practical significance.Therefore
It is badly in need of exploitation simplicity, quickly measures the method for amide substance in food contact material.
Summary of the invention
It is empty the purpose of the invention is to fill up technology of the China in food contact material in the detection of amide substance
It is white, and provide it is a kind of using gas chromatography mass spectrometry chromatography simultaneously detect acrylamide in food contact material, Methacrylamide, oneself
The method of lactams, oleamide and stearmide.
To achieve the above object, the present invention adopts the following technical scheme:
The detection method of amide substance content in a kind of food contact material, specifically includes following operating procedure:
(1) sample preparation: choosing representative sample, is cut into the fragment less than the mm of 5 mm × 5, is packed into clean container after mixing
As sample, mark is sealed and carries out, sample making course must be prevented from the variation that sample was contaminated or occurred residuals content;
(2) sample purification:
Methanol solution extracts: sample that 1.00 g have been mixed weighed in 50mL stuffed conical flask, and 25ml methanol solution is added, in
After filtering, 25ml methanol solution is added into sample again by ultrasonic extraction 30min at 25 DEG C, and ultrasonic extraction 30min merges filter
Liquid, 50 DEG C of nitrogen blow close dry, 10 mL methanol solution dissolved residues of addition, quantitative, infuse after taking 1ml solution to cross 0.22 μm of miillpore filter
Enter in sample injection bottle to get prepare liquid;
Chloroform soln extracts: weighing the sample of 1.00 g mixing in 50mL stuffed conical flask, 25ml chloroform is added
After filtering, 25ml chloroform soln, ultrasonic extraction are added into sample again by solution, the ultrasonic extraction 30min at 25 DEG C
30min, merging filtrate, 50 DEG C of nitrogen blow close dry, 10 mL methanol solution dissolved residues of addition, quantitative, and 1ml solution is taken to cross 0.22 μm
It injects in sample injection bottle after miillpore filter to get prepare liquid;
(3) analysis detection: each prepare liquid of acquisition is all made of GC/MS progress analysis detection and specifically carries out prepare liquid
Machine analysis is the measured object i.e. response signal of amide substance in prepare liquid to obtain, later according to the sound of measured object in prepare liquid
Induction signal chooses the corresponding standard working solution of response and carries out chromatography, and standard working solution, which is equipped with, includes six including zero point
Concentration gradient, and in standard working solution and prepare liquid amide substance response should all in instrument linear response range, and
One blank control is set simultaneously;
(4) testing result calculates: GC/MS being obtained each parameter value substitution formula and is calculated, to obtain acyl in each prepare liquid
The actual measured value of amine substance.
GC conditions in the step (3) are as follows: chromatographic column product parameters are Agilent DB-5MS, 30 m
× 0.25mm, 0.25 μm of granularity;Carrier gas is helium;Temperature program are as follows: 1min is maintained after 60 DEG C of sample introductions, then with 10 DEG C/min
Speed be warming up to 200 DEG C, then be changed into and be warming up to 270 DEG C with the heating rate of 5 DEG C/min, maintain 5min;Sample volume is 1 μ
L;Split ratio is 5:1.
Mass Spectrometry Conditions in the step (3) are as follows: ion source is electron impact ionization mode;Electron multiplier voltage is
1.6kV;Ion source temperature is 230 DEG C;Level four bars temperature is 150 DEG C;The mass spectrometry parameters condition of 5 kinds of amides are as follows: acrylamide is protected
Stay time 4.004min, qualitative 71 m/z of ion charge-mass ratio, 44,55 m/z of quota ion charge-mass ratio;Methacrylamide retains
Time 4.729min, qualitative 85 m/z of ion charge-mass ratio, quota ion charge-mass ratio 41,69m/z;Caprolactam retention time
9.844min, qualitative 113 m/z of ion charge-mass ratio, quota ion charge-mass ratio 55,85m/z;Oleamide retention time
24.601min, qualitative ion charge-mass ratio 59m/z, quota ion charge-mass ratio 41,72m/z;Stearmide retention time
24.934min, qualitative ion charge-mass ratio 59m/z, quota ion charge-mass ratio 41,72m/z.
The calculation formula of the content of amide substance is X=[(A-A in food contact material in the step (4)0)×c×
V]/(As× M), X is the amount of migration of target analytes in sample to be tested, mg/kg in formula;A is target analytes in extracting solution
Peak area;A0For the peak area of target analytes in blank assay;As is the peak area of target analytes in standard working solution;
C is the concentration of target analytes in standard working solution, mg/L;V is determined volume, L;M is the quality of sample to be tested, kg;Meter
Blank value need to be deducted by calculating result, and be retained to three effective digitals.
In addition, the present invention is 1mg/kg, rate of recovery 79.30-104.53% using the limitation that methanol solution extracts;It utilizes
The limitation that chloroform extracts is 1.1 mg/kg, rate of recovery 78.07-103.47%;Five kinds of amide substances are in 5 ~ 100 mg/
L range internal standard curve linear relationship is good, and correlation coefficient r is greater than 0.99.
The present invention has the advantages that
1, the present invention detects acrylamide in food contact material, Methacrylamide using gas chromatography mass spectrometry chromatography, in oneself simultaneously
Amide, oleamide and stearmide have filled up the blank of the relevant technologies;
2, the present invention is 1mg/kg, rate of recovery 79.30-104.53% using the limitation that methanol solution extracts;Utilize chloroform
The limitation of extraction is 1.1 mg/kg, rate of recovery 78.07-103.47%;Five kinds of amide substances are within the scope of 5 ~ 100 mg/ L
Standard curve linear relationship is good, and correlation coefficient r is greater than 0.99;
3, the present invention extracts the method simplicity of amide substance in food contact material, compared with prior art, eliminates solid
Mutually extract or be concentrated by evaporation and etc., extraction time is not only saved, operating procedure is also simplified;
4, for the retention time of the Mass Spectrometer Method of 5 kinds of amide substances all within 25 min, detection time is short in the present invention.
Specific embodiment
In order to preferably be described to the present invention, the application is for following several embodiments, and in each implementation
The feasibility of detection method and accuracy are verified in example.
Using Agilent 7890A-5975C gas chromatograph-mass spectrometer, (gas-chromatography selects Agilent 7890A, mass spectrograph to the present invention
Select Agilent 5975C) carry out sample measurement.
Embodiment one: sample to be tested --- negative plastic packing bag (negative sample)
1.1 sample preparations: choosing negative plastic food packaging materials (being free of the plastic food packaging materials of amide substance),
It is cut into the fragment less than the mm of 5 mm × 5, clean container is packed into after mixing as sample, seals and carries out mark;Choose 50mL tool
Conical flask is filled in, 1.00 g(are accurately weighed into conical flask and are accurate to 0.1 mg) above-mentioned sample.
The test of 1.2 backgrounds: randomly selecting six conical flasks in 1.1, and it is molten to be carried out methanol by every triplets for first group of sample
Liquid extracts, and second group of sample carries out chloroform soln extraction, according to step in the content of present invention (2), step (3) and step
(4) it is operated, and will finally calculate resulting each actual measured value and be listed in Table 1 below, and calculate the average value of actual measured value
With RSD(relative standard deviation) as shown in table 1, which is background values.
The background values determination data (n=6) of amide substance content in 1 negative sample of table
1.3 verifyings one: the amide substance of 10 mg/L of addition
12 conical flasks in 1.1 are randomly selected, every six are one group, add 100mg/L into each conical flask later
First group of sample is carried out methanol solution extraction by 1 mL of amide substance standard substance standard solution, and second group of sample carries out three
Chloromethanes solution extracts, and is operated according to step in the content of present invention (2), step (3) and step (4), and calculate the rate of recovery
It is as shown in table 2 with RSD.
The rate of recovery data of the amide substance of 10 mg/L of middle addition in 2 negative sample of table
1.4 verifyings two: 20 mg/L amide substances of addition
12 conical flasks in 1.1 are randomly selected, every six are one group, add 100mg/L into each conical flask later
First group of sample is carried out methanol solution extraction by 2 mL of amide substance standard substance standard solution, and second group of sample carries out three
Chloromethanes solution extracts, and is operated according to step in the content of present invention (2), step (3) and step (4), and calculate the rate of recovery
It is as shown in table 3 with RSD.
The rate of recovery data of the amide substance of 20 mg/L are added in 3 negative sample of table
1.5 verifyings three: 50 mg/L amide substances of addition
12 conical flasks in 1.1 are randomly selected, every six are one group, add 1000mg/L into each conical flask later
First group of sample is carried out methanol solution extraction by 0.5 mL of amide substance standard substance standard solution, and second group of sample carries out
Chloroform soln extracts, and is operated according to step in the content of present invention (2), step (3) and step (4), and calculate recycling
Rate and RSD are as shown in table 4.
The rate of recovery data of the amide substance of 50 mg/L are added in 4 negative sample of table
Embodiment two: sample to be tested --- positive food contact material (positive sample)
2.1 sample preparations: choosing positive plastic food packaging materials (i.e. the plastic food packaging materials of amide containing substance),
It is cut into the fragment less than the mm of 5 mm × 5, clean container is packed into after mixing as sample, seals and carries out mark;Choose 50mL tool
Conical flask is filled in, 1.00 g(are accurately weighed into conical flask and are accurate to 0.1 mg) above-mentioned sample.
The test of 2.2 backgrounds: randomly selecting six conical flasks in 2.1, and first group of sample is carried out methanol by every triplets
Solution extracts, and second group of sample carries out chloroform soln extraction, according to step in the content of present invention (2), step (3) and step
(4) it is operated, and will finally calculate resulting each actual measured value and be listed in Table 5 below, and calculate the average value of actual measured value
With RSD(relative standard deviation) as shown in table 5, which is background values.
The background concentration determination data of amide substance in 5 positive sample of table
2.3 verifyings one: 10 mg/L amide substances of addition --- methanol solution extracts
Six conical flasks in 2.1 are randomly selected, 100mg/L amide substance standard substance mark is added into each conical flask
Quasi- 1 mL of solution, the method in the step of foundation summary of the invention (2) carries out the extraction of methanol solution later, then again according to step
(3) and step (4) is operated, and calculate each group measured value and RSD it is as shown in table 6.
The measurement result of 6 methanol solution of table extraction positive sample
2.4 verifyings two: 10 mg/L amide substances of addition --- chloroform soln extracts
Six conical flasks in 2.1 are randomly selected, 100mg/L amide substance standard substance mark is added into each conical flask
Quasi- 1 mL of solution, later according to summary of the invention the step of (2) in method carry out the extraction of chloroform soln, then foundation again
Step (3) and step (4) are operated, and calculate each group measured value and RSD it is as shown in table 7.
The measurement result of 7 chloroform soln of table extraction positive sample
By the verifying in the various embodiments described above it is found that detection method of the invention is applied to amides in detection food contact material
When the content of substance, detection method of the invention can determine whether out not from the size of the rate of recovery and RSD in respective verification result
It is only feasible, and accuracy is high.
In addition, though the present invention is illustrated exposure with above-described embodiment, but it is not intended to limit the invention, Ren Hesuo
Belong in technical field and has a usually intellectual, it is all according to made equivalent change in the present patent application scope of the claims and retouching,
Scope of the present invention should all be belonged to.
Claims (4)
1. the detection method of amide substance content in a kind of food contact material, it is characterised in that: it specifically includes following behaviour
Make step:
(1) sample preparation: choosing representative sample, is cut into the fragment less than the mm of 5 mm × 5, is packed into clean container after mixing
As sample, mark is sealed and carries out, sample making course must be prevented from the variation that sample was contaminated or occurred residuals content;
(2) sample purification:
Methanol solution extracts: sample that 1.00 g have been mixed weighed in 50mL stuffed conical flask, and 25ml methanol solution is added, in
After filtering, 25ml methanol solution is added into sample again by ultrasonic extraction 30min at 25 DEG C, and ultrasonic extraction 30min merges filter
Liquid, 50 DEG C of nitrogen blow close dry, 10 mL methanol solution dissolved residues of addition, quantitative, infuse after taking 1ml solution to cross 0.22 μm of miillpore filter
Enter in sample injection bottle to get prepare liquid;
Chloroform soln extracts: weighing the sample of 1.00 g mixing in 50mL stuffed conical flask, 25ml chloroform is added
After filtering, 25ml chloroform soln, ultrasonic extraction are added into sample again by solution, the ultrasonic extraction 30min at 25 DEG C
30min, merging filtrate, 50 DEG C of nitrogen blow close dry, 10 mL methanol solution dissolved residues of addition, quantitative, and 1ml solution is taken to cross 0.22 μm
It injects in sample injection bottle after miillpore filter to get prepare liquid;
(3) analysis detection: each prepare liquid of acquisition is all made of GC/MS progress analysis detection and specifically carries out prepare liquid
Machine analysis is the measured object i.e. response signal of amide substance in prepare liquid to obtain, later according to the sound of measured object in prepare liquid
Induction signal chooses the corresponding standard working solution of response and carries out chromatography, and standard working solution, which is equipped with, includes six including zero point
Concentration gradient, and in standard working solution and prepare liquid amide substance response should all in instrument linear response range, and
One blank control is set simultaneously;
(4) testing result calculates: GC/MS being obtained each parameter value substitution formula and is calculated, to obtain acyl in each prepare liquid
The actual measured value of amine substance.
2. the detection method of amide substance content, feature exist in a kind of food contact material according to claim 1
In the GC conditions in the step (3) are as follows: chromatographic column product parameters be Agilent DB-5MS, 30 m ×
0.25mm, 0.25 μm of granularity;Carrier gas is helium;Temperature program are as follows: 1min is maintained after 60 DEG C of sample introductions, then with 10 DEG C/min's
Speed is warming up to 200 DEG C, then is changed into and is warming up to 270 DEG C with the heating rate of 5 DEG C/min, maintains 5min;Sample volume is 1 μ L;
Split ratio is 5:1.
3. the detection method of amide substance content, feature exist in a kind of food contact material according to claim 1
In the Mass Spectrometry Conditions in the step (3) are as follows: ion source is electron impact ionization mode;Electron multiplier voltage is
1.6kV;Ion source temperature is 230 DEG C;Level four bars temperature is 150 DEG C;The mass spectrometry parameters condition of 5 kinds of amides are as follows: acrylamide is protected
Stay time 4.004min, qualitative 71 m/z of ion charge-mass ratio, 44,55 m/z of quota ion charge-mass ratio;Methacrylamide retains
Time 4.729min, qualitative 85 m/z of ion charge-mass ratio, quota ion charge-mass ratio 41,69m/z;Caprolactam retention time
9.844min, qualitative 113 m/z of ion charge-mass ratio, quota ion charge-mass ratio 55,85m/z;Oleamide retention time
24.601min, qualitative ion charge-mass ratio 59m/z, quota ion charge-mass ratio 41,72m/z;Stearmide retention time
24.934min, qualitative ion charge-mass ratio 59m/z, quota ion charge-mass ratio 41,72m/z.
4. the detection method of amide substance content, feature exist in a kind of food contact material according to claim 1
In the calculation formula of the content of amide substance is X=[(A-A in food contact material in the step (4)0)×c×V]/(As
× M), X is the amount of migration of target analytes in sample to be tested, mg/kg in formula;A is the peak area of target analytes in extracting solution;
A0For the peak area of target analytes in blank assay;As is the peak area of target analytes in standard working solution;C is standard
The concentration of target analytes, mg/L in working solution;V is determined volume, L;M is the quality of sample to be tested, kg;Calculated result needs
Blank value is deducted, and is retained to three effective digitals.
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Cited By (1)
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CN110470756A (en) * | 2019-08-12 | 2019-11-19 | 华南理工大学 | The method and its application of the organic chloro thing DCP content of nocuousness of PAE wet strength agent in a kind of measurement paper for daily use |
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EP2842614A1 (en) * | 2013-08-30 | 2015-03-04 | Biotage AB | Sample preparation method for analysis of acrylamide |
CN103512996A (en) * | 2013-10-22 | 2014-01-15 | 广州广电计量检测股份有限公司 | Analysis method for amide compounds |
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GANG LV等: "Method for determination of fatty acid amides in polyethylene packaging", 《JOURNAL OF CHROMATOGRAPHY A》 * |
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