CN109557202A - The detection method of 16 carbamides in food contact plastics - Google Patents

The detection method of 16 carbamides in food contact plastics Download PDF

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Publication number
CN109557202A
CN109557202A CN201811426410.7A CN201811426410A CN109557202A CN 109557202 A CN109557202 A CN 109557202A CN 201811426410 A CN201811426410 A CN 201811426410A CN 109557202 A CN109557202 A CN 109557202A
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solution
standard
carbamides
sample
concentration
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蔡开云
陈萍
冯向东
赵素洁
郭婷婷
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HUBEI DAOHUAXIANG LIQUOR CO Ltd
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HUBEI DAOHUAXIANG LIQUOR CO Ltd
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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
    • 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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  • Health & Medical Sciences (AREA)
  • Life Sciences & Earth Sciences (AREA)
  • Chemical & Material Sciences (AREA)
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  • Other Investigation Or Analysis Of Materials By Electrical Means (AREA)

Abstract

The invention discloses a kind of detection methods of 16 carbamides in food contact plastics, comprising the following steps: 1) preparation of standard solution accurately weighs 16 carbamide standard items, dissolved with methanol, be configured to stock solution；12 carbamides are accurately weighed, are dissolved with methanol, inner mark solution is prepared；Then the stock solution of 16 carbamides is diluted, obtains the standard solution with concentration gradient, and inner mark solution is wherein added；2) preparation of sample solution, plastic sample use methanol extraction, and sample solution is made after inner mark solution is added in obtained liquid；3) GC-MSMS scanning standard solution is used, its regression equation than drafting standard curve and is obtained with peak area ratio and concentration, then scan sample solution, the content of 16 carbamides in plastic sample is calculated.101.3~107.1%, precision RSD < 5% has good accuracy and repeatability, fully meets 16 carbamide assay requirement in food contact plastic material and product recovery of standard addition of the present invention.

Description

The detection method of 16 carbamides in food contact plastics
Technical field
The present invention relates to detection technique fields, and in particular to a kind of food contact detection side of 16 carbamides in plastics Method.
Background technique
16 carbamides (hexadecanamide), molecular formula C16H33NO (No. CAS: 629-54-9), is a kind of Gao Rong The amides nonionic surfactant selected is suitable for preparing shampoo, bath foam and cosmetics etc..In the plastics of food contact at present Generally use oleamide, erucyl amide, stearmide as lubricant, 16 carbamides also play the role of it is similar, with layer Not poor food-safety problem is disclosed out, and food-safety problem has become the hot topic of countries in the world extensive concern. GB9685-2016 " food national safety standard food contact material and product additive use standard " regulation food contact modeling 16 carbamides must not be used in material；The relevant research of rare 16 carbamide both at home and abroad, also without specific detection method.
Summary of the invention
In order to solve the above technical problem, the present invention provides a kind of detection sides of 16 carbamides in food contact plastics Method takes GC-MSMS method, using 12 carbamides as internal standard, the content of 16 carbamides directly in detection food contact plastics.
The technical solution adopted by the present invention is that a kind of food contact detection method of 16 carbamides in plastics, including Following steps:
1) preparation of standard solution
16 carbamide standard items are accurately weighed, is dissolved with methanol, is configured to stock solution；12 carbamides are accurately weighed, It is dissolved with methanol, prepares inner mark solution；Then the stock solution of 16 carbamides is diluted, obtains the mark with concentration gradient Quasi- solution, and inner mark solution is wherein added；
2) preparation of sample solution
Plastic sample uses methanol extraction, and sample solution is made after inner mark solution is added in obtained liquid；
3) GC-MSMS scanning standard solution is used, with peak area ratio and concentration than drawing standard curve and obtaining its time Return equation, then scan sample solution, the content of 16 carbamides in plastic sample is calculated.
Further, the concentration of the stock solution is 100mg/L, and the concentration of inner mark solution is 100mg/L.
Further, in the standard solution with concentration gradient 12 carbamide of internal standard compound concentration, sample solution The concentration of middle 12 carbamide of internal standard compound is identical.
Further, in the standard solution with concentration gradient the concentration of 16 carbamides be respectively 5mg/L, 10mg/L, 20mg/L, 30mg/L and 100mg/L.
Further, it when prepared by the sample solution, after first shredding or being ground into particle of the diameter less than 2mm, is added Then methanol carries out 25~35min of ultrasonic wave extraction.
Further, in step 3), when being scanned using GC-MSMS,
Chromatographic condition: chromatographic column: ZB-WAXplus quartz capillary column (30m × 0.25mm × 0.25 μm)；Injection port temperature Degree: 250 DEG C；Temperature programming:, keeping 0min by 100 DEG C of initial column temperature, rises to 250 DEG C with 10 DEG C/min, keeps 5min；Carrier gas: helium Gas (purity > 99.999%), flow velocity 1mL/min；Input mode: Splitless injecting samples；Sample volume: 1 μ L；
Mass Spectrometry Conditions: 260 DEG C of interface temperature, mode: electron bombardment ionization source (EI) is ionized；Ionizing energy: 70eV；Solvent prolongs When: 5min.
Further, purity >=95wt% of the palmitamide standard items；12 carbamide standard items purity >= 96wt%；Methanol is chromatographically pure.
Further, the GC-MSMS instrument is the triple level four bars series connection gas chromatograph-mass spectrometers of Agilent7890A-7000B.
Further, the plastic sample is food contact plastic material or product.
The present invention uses GC-MSMS method, does internal standard with 12 carbamides, measurement food contact is used in plastic material and product 16 phosphinylidyne amine contents, through experimental analysis: the relative deviation 0.4% of qualitative analysis retention time, qualitative ion relative abundance For relative deviation 0%~5%, qualitative results are accurate and reliable；Quantitative analysis recovery of standard addition is between 101.3-107.1%, essence Density RSD < 5% has preferable accuracy, fully meets 16 phosphinylidyne amine content in food contact plastic material and product Measurement requires.
Detailed description of the invention
Fig. 1 is the total ion chromatogram that sample carries out full scan after methanol dissolves using GC-MSMS.
Fig. 2 is 16 carbamide mass spectrograms and chemical formula.
Fig. 3 is 16 carbamide standard items full scan chromatograms.
Fig. 4 is the chromatogram after sample solution carries out MRM scanning with GC-MSMS.
Fig. 5 is the chromatogram after standard sample carries out MRM scanning with GC-MSMS.
Fig. 6 is standard working curve.
Fig. 7 is the comparison figure of ethyl alcohol and methanol as solvent.Wherein Fig. 7-1 is ethyl alcohol as solvent, and Fig. 7-2 is methanol work For solvent.
Fig. 8 is the 16th phosphinylidyne amine concentration influence diagram of extraction time.
Fig. 9 is low concentration sample standard deviation figure compared with enriched sample standard deviation.Wherein Fig. 9-1 is low concentration sample Product, 9-2 are enriched sample.
Figure 10 is the selection chromatography of ions figure for carrying out detection acquisition to sample using method of the invention.
Specific embodiment
Below with reference to examples and drawings 1-10, the present invention is furture elucidated.
1..1 sample, reagent and instrument
Sample: ldpe resin several pieces
Reagent: palmitamide standard items (purity >=95%)；12 carbamide standard items (purity >=96%)；Methanol, color It composes pure；
Instrument: the triple level four bars series connection gas chromatograph-mass spectrometers of Agilent7890A-7000B；Supersonic generator.
1..2 experiment condition
Chromatographic condition: chromatographic column: ZB-WAXplus quartz capillary column (30m × 0.25mm × 0.25 μm)；Injection port temperature Degree: 260 DEG C；Temperature programming:, keeping 0min by 100 DEG C of initial column temperature, rises to 250 DEG C with 10 DEG C/min, keeps 5min,；Carrier gas: Helium (purity > 99.999%), flow velocity 1mL/min；Input mode: Splitless injecting samples sample volume: 1 μ L.
Mass Spectrometry Conditions: 250 DEG C of interface temperature, mode: electron bombardment ionization source (EI) is ionized；Ionizing energy: 70eV；Solvent prolongs When: 4min.
1..3 experimental method
1..3..1 the preparation of standard solution
1. the preparation of 16 carbamide standard solution of
Stock solution: 16 carbamide of 0.01g is accurately weighed, is dissolved with methanol, is settled in 100mL volumetric flask, is configured to Concentration is the stock solution of 100mg/L.
2. the preparation of 12 carbamide of internal standard
12 carbamide of 0.01g is accurately weighed, is dissolved with methanol, is settled in 100mL volumetric flask, being configured to concentration is The solution of 100mg/L.Above-mentioned standard solution saves backup under room temperature.
1..3..2 qualitative analysis
Appropriate amount of sample is taken, is extracted with proper amount of methanol, extract liquor is taken to carry out full scan with GC-MSMS, total ion chromatogram is shown in Fig. 1.Find out from Fig. 1 total ion chromatogram, 14.956 chromatographic peak of retention time is it is obvious that extract its mass spectrogram, by composing library Retrieval, compound are 16 carbamides, and matching degree 95%, mass spectrogram and chemical formula are shown in Fig. 2.It is qualitative in order to further verify its Accuracy, taken under same experimental condition 200mg/L 16 carbamide standard solution carry out full scan, total ion chromatography Figure is shown in Fig. 3.By comparing to retention time and mass spectrogram, determine that the substance is 16 carbamides.Divide from the mass spectrogram of diagram Analysis, characteristic ion 59.1.Relative deviation of retention time is 0.4%, and mass spectrometry parameter is shown in Table 1.
Table 1
1..3..3 quantitative analysis
1..3..3..1 Selection of internal standard
It is required according to Selection of internal standard, chooses diisopropyl phthalate and 12 carbamides do Experimental comparison, adjacent benzene Dioctyl phthalate diisopropyl ester differs greatly with 16 carbamide retention times, and characteristic ion mass number differs greatly, and discomfort is fit to do this reality Test internal standard；12 carbamides can be with object good separating effect, and retention time is close with object, and characteristic ion is identical, therefore It chooses 12 carbamides and makees internal standard.
For the accuracy for guaranteeing quantitative result, by the test of product ion and collision energy, the MRM after optimization is scanned, Mass spectrum quantitative parameter is shown in Table 2:
Table 2
Sample and standard specimen are carried out respectively plus internal standard is tested.Accurately weigh 0.5g (being accurate to 0.0001g) low density polyethylene Alkene, ultrasonic 30min are added after 5mL methanol ultrasonic extraction 30min and are added after 50 μ L internal standards are shaken up using liquid, carried out with GC-MSMS MRM scanning.As a result see Fig. 4.
Taking 5mL concentration is that the 16 carbamide standard samples of 100mg/L use GC- after 50 μ L internal standards of addition are shaken up using liquid MSMS carries out MRM scanning.As a result see Fig. 5.
Internal standard good separating effect is done with 12 carbamides it can be seen from above-mentioned Fig. 4 and Fig. 5, retention time is close, analysis Time is suitable.
1..3..3..2 the drafting of standard curve
The preparation of standard working solution: 16 carbamide deposit of 0.5mL, 1.0mL, 2.0mL, 3.0mL, 10.0mL is taken respectively Liquid with methanol constant volume to 10mL, is added the 12 carbamide inner mark solutions of 100 μ L, mixes spare in 10mL volumetric flask.
The drafting of standard working curve: it carries out the standard curve working solution of each concentration to carry out MRM with GC-MSMS sweeping It retouches, with peak area ratio and concentration than drawing standard curve and obtaining its regression equation.The standard curve drawn out is shown in Fig. 6, Middle object and internal standard compound peak area ratio are Y-axis, and object and internal standard compound concentration proportion are X-axis.It will be appreciated from fig. 6 that it is returned Equation is Y=0.99958233*X-1.837201, coefficient R2=0.99958, it is seen that the linear relationship of the standard curve compared with It is good, meet the requirement of analysis.It is shown by experimental result, the range of linearity are as follows: 5mg/L~100mg/L.
1..3..4 the selection of solvent
20 parts of sample 0.5g (being accurate to 0.0001g) is accurately weighed, is divided into two groups, every group 10 parts, first group of every part of difference Be added 5mL methanol, second group every part be separately added into 5mL EtOH Sonicate 30min, add after 50 μ L internal standards are shaken up using liquid, supply GC-MSMS analysis.Test results are shown in figure 7.Solvent is done by Fig. 7 analysis methanol and ethyl alcohol does the mean value of solvent there are significance differences It is different, and methanol does solvent mean value and does solvent mean value greater than ethyl alcohol, it was demonstrated that methanol recovery rate is higher, selects methanol as extractant.
1..3..5 the determination of extraction time
This experimental selection supersonic generator extracts object.It is low to accurately weigh 0.5g (being accurate to 0.0001g) It 6 parts of density polyethylene, is separately added into 5mL methanol and is added after ultrasound 0min, 15min, 30min, 45min, 60min, 90min respectively After 50 μ L internal standards are shaken up using liquid, MRM scanning is carried out with GC-MSMS.Test results are shown in figure 8, as shown in Figure 8, ultrasound 16 phosphinylidyne amine concentration of 30min is higher, and with the increase of ultrasonic time, the increase of 16 phosphinylidyne amine concentrations is unobvious, thus selects 30min is best ultrasonic time.
1..3..6 the processing and measurement of sample
It accurately weighs sample 0.5g (being accurate to 0.0001g), 5mL methanol is added, ultrasonic 30min, 50 μ L internal standards, which are added, to be made After being shaken up with liquid, MRM scanning is carried out with GC-MSMS.Blank test is done simultaneously.Other samples need to be cut into fragment or with pulverizer powder Broken, diameter is less than 2mm.
1..3..7 result calculates
16 phosphinylidyne amine contents are calculated as follows in sample:
X=(ρ-ρ0)×V/m
The content mg/kg of C: ten six carbamides；
ρ: sample solution concentration mg/L；
ρ0: blank mg/L
V: solvent volume mL；
M: sample mass g.
According to the above method, the result for measuring 10 samples see the table below 3.
Table 3
Sample number Sample mass g Solvent volume mL Sample solution concentration g/L Blank mg/L The content mg/kg of 16 carbamides
1 0.5040 5 5.4754 2.2753 31.7470
2 0.5005 5 7.3487 2.2753 50.6833
3 0.5099 5 9.2677 2.2753 68.5664
4 0.5022 5 9.9232 2.2753 76.1440
5 0.5031 5 7.4243 2.2753 51.1727
6 0.4994 5 11.9238 2.2753 96.6009
7 0.5024 5 20.5699 2.2753 182.0721
8 0.5031 5 19.6585 2.2753 172.7609
9 0.5096 5 17.4534 2.2753 148.9217
10 0.5018 5 13.6268 2.2753 113.1078
Recovery of standard addition
Sample about 5.0g (being accurate to 0.0001g) is weighed, 100mL methanol is added, ultrasonic extraction 30 minutes, takes 5mL respectively It 7 parts of extract liquor, wherein 6 parts are added not same amount standard specimen, then is separately added into after 50 μ L internal standards are shaken up using liquid, is analyzed for GC-MSMS. Measurement result and rate of recovery calculated result are shown in Table 4
The different scalar quantity rate of recovery experiments of table 4
Seen by table 4, for the rate of recovery of different scalar quantities between 101.3%~107.1%, the rate of recovery is very high, illustrates this Test method correctness is high.
2..5 precision
Two samples are weighed respectively, every group 20 (identical in quality), are tested by 1.3.6 item, low concentration sample test The precision that the precision of method the results are shown in Table 5 enriched sample test methods the results are shown in Table 6
Table 5
Table 6
It is for statistical analysis to above data, as a result see figure, by above 5 table of table, 6 Fig. 9 it can be concluded that, two groups of data Significant difference is not present in standard deviation, and the RSD value tested in experiment is respectively 2.1% and 0.8% (< 5%, difference pole is not significant), Illustrate that this method is suitable for the detection of various concentration sample, which has repeatability well.
For the elimination unstable bring error of gas chromatograph sampling amount, the repeatability and reproducibility of testing result is improved, This method uses internal standard method standard curve standard measure.This method selects 12 carbamides to do internal standard, fully meets the choosing of internal standard compound Select requirement, 1, be free of the substance in sample；2, chemical property and object are close；3, it is kept completely separate with object.
And stearic amide and oleamide can be detected using this method simultaneously, using the acquisition of above-mentioned qualitative method Select chromatography of ions figure as shown in Figure 10, in which: peak 1 is internal standard lauramide (retention time: 9.732.)；Peak 2 is 16 carbon Amide (retention time: 14.839)；Peak 3 is stearic amide (retention time: 19.851)；Peak 4 is oleamide (when reservation Between: 20.733).The quantitative analysis method of stearic amide and oleamide can be established simultaneously.
The above embodiments are only the preferred technical solution of the present invention, and are not construed as limitation of the invention, this hair Bright protection scope should be with the technical solution of claim record, technical characteristic in the technical solution recorded including claim Equivalents are protection scope.Equivalent replacement i.e. within this range is improved, also within protection scope of the present invention.

Claims (10)

1. the detection method of 16 carbamides in a kind of food contact plastics, which comprises the following steps:
1) preparation of standard solution
16 carbamide standard items are accurately weighed, is dissolved with methanol, is configured to stock solution；12 carbamides are accurately weighed, first is used Alcohol dissolution, prepares inner mark solution；Then the stock solution of 16 carbamides is diluted, obtains having the standard of concentration gradient molten Liquid, and inner mark solution 0.05mL is wherein added；
2) preparation of sample solution
Plastic sample uses methanol extraction, and sample solution is made after inner mark solution is added in obtained liquid；
3) GC-MSMS scanning standard solution is used, with peak area ratio and concentration than drawing standard curve and obtaining its recurrence side Journey, then sample solution is scanned, the content of 16 carbamides in plastic sample is calculated.
2. according to the method described in claim 1, it is characterized by: the concentration of the stock solution is 100mg/L.
3. according to the method described in claim 1, it is characterized by: the concentration of inner mark solution is 100mg/L.
4. according to the method described in claim 1, it is characterized by: internal standard compound ten in the standard solution with concentration gradient The concentration of two carbamides, the concentration of 12 carbamide of internal standard compound is identical in sample solution.
5. according to the method described in claim 1, it is characterized by: 16 phosphinylidynes in the standard solution with concentration gradient The concentration of amine is respectively 5mg/L, 10mg/L, 20mg/L, 30mg/L and 100mg/L.
6. according to the method described in claim 1, it is characterized by: first shredding or being ground into when prepared by the sample solution After particle of the diameter less than 2mm, methanol is added, then carries out 25~35min of ultrasonic wave extraction.
7. according to the method described in claim 1, it is characterized by: in step 3), when being scanned using GC-MSMS,
Chromatographic condition: chromatographic column: ZB-WAXplus quartz capillary column；Injector temperature: 250 DEG C；Temperature programming: initial column temperature 100 DEG C, 0min is kept, 250 DEG C is risen to 10 DEG C/min, keeps 5min；Carrier gas: helium, flow velocity 1mL/min；Input mode: no Split sampling；Sample volume: 1 μ L；
Mass Spectrometry Conditions: 260 DEG C of interface temperature, mode: electron bombardment ionization source is ionized；Ionizing energy: 70eV；Solvent delay: 5min.
8. according to the method described in claim 1, it is characterized by: purity >=95wt% of the palmitamide standard items；12 Carbamide standard items purity >=96wt%；Methanol is chromatographically pure.
9. according to the method described in claim 1, it is characterized by: the GC-MSMS instrument is Agilent7890A-7000B Triple level four bars series connection gas chromatograph-mass spectrometers.
10. according to the method described in claim 1, it is characterized by: the plastic sample be food contact with plastic material or Product.
CN201811426410.7A 2018-11-27 2018-11-27 The detection method of 16 carbamides in food contact plastics Pending CN109557202A (en)

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Cited By (1)

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Application publication date: 20190402