CN105044235A - Method for detecting specific migration amounts of nine anti-oxidants in plastic products by liquid chromatography method - Google Patents
Method for detecting specific migration amounts of nine anti-oxidants in plastic products by liquid chromatography method Download PDFInfo
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Abstract
The invention provides a high performance liquid chromatography-ultraviolet detection method for simultaneously detecting specific migration amounts of nine anti-oxidants in five food simulants. The method comprises immersing a sample to be measured in food simulants, carrying out cooling to a room temperature, carrying out uniform mixture, metering a volume of the water-based food simulants by a tris(2-carboxyethyl)phosphine hydrochloride-containing tetrahydrofuran mixed solution, carrying out filtration by a hydrophilic Teflon syringe filter, carrying out sample introduction, carrying out rotary distillation nitrogen-blowing condensation on the isooctane food simulants until basic drying, metering the volume by tris(2-carboxyethyl)phosphine hydrochloride-containing methanol, carrying out filtration by the hydrophilic Teflon syringe filter and carrying out sample introduction. C8 column gradient elution separation is used, detection wavelength is 285nm and a sample size is 20 microliters. The method has good chromatographic separation and linear relationship, has high recovery rate and high accuracy, has a quantification limit satisfying limitation requirements on the total migration amount of the nine anti-oxidants in the EU NO 10/2011 regulation and has been used for detection of a practical sample.
Description
Technical field
The invention belongs to chemicals detection field, relate to the detection method of harmful 9 kinds of specific gross migrations of antioxidant in Plastic packaging for foodstuff contact material, particularly relate to a kind of detection method using high performance liquid chromatography ultraviolet (HPLC-UV) method to measure 9 kinds of antioxidant Special migrations in Plastic packaging material for food and container.
Background technology
Plastic food contact material often need add the function additive such as antioxidant, ultraviolet absorber to extend the serviceable life of correlated product.But in the process that goods use, these antioxidant be added also can move in food, the health of direct harmful to human.(EU) NO10/2011 regulation that European Union issued in 2011 is by the in addition restriction of the Special migration (SML) of multiple antioxidant or specific gross migration [SML (T)].
At present, both at home and abroad about the detection of antioxidant mainly concentrates in food, plastics, feed and food simulants class sample, the detection method of use has HPLC method and HPLC-MS/MS method.In existing related food analogies, the detection document of antioxidant only can detect the Special migration of several antioxidant in food simulants, because in the antioxidant kind that detects and European Union (EU) NO10/2011 regulation subordinate list 2, the kind of 9 kinds of antioxidant is not quite identical simultaneously, cannot detect the specific gross migration of 9 kinds of antioxidant in European Union (EU) NO10/2011 regulation.
Summary of the invention
In order to solve the difficult problem that in Plastic packaging material for food and container, the specific gross migration of harmful antioxidant detects, the detection method providing a kind of high performance liquid chromatography ultraviolet (HPLC-UV) method to detect the specific gross migration of 9 kinds of antioxidant in Plastic food contact material of the present invention, the method has sensitive, accurate, quick, easy feature.
To achieve these goals, high performance liquid chromatography ultraviolet (HPLC-UV) method of the present invention detects the detection method of the specific gross migration of 9 kinds of antioxidant in Plastic food contact material, comprises the following steps:
One, migration test
According to the practical use of Food Contact plastic products, be injected in testing sample plastic products or glassware according to certain surface-to-volume than by food simulants, after vessel mouth or vessel port seal with surface plate or aluminium-foil paper, in baking oven or incubator, determine that migration temperature and transit time carry out migration test by European Union (EU) NO10/2011 rules and regulations, after be cooled to room temperature, food simulants is wherein transferred in clean glassware and treats subsequent treatment; Wherein food simulants is divided into food simulants A, B, C, D1, D2;
Wherein food simulants is according to European Union (EU) NO10/2011 rules and regulations, food simulants A:10% ethanol water (v/v), for simulating the aqueous food of pH > 4.5; Food simulants B:3% acetic acid aqueous solution (w/v), for simulating the acid food of pH < 4.5; Food simulants C:20% ethanol water (v/v), for simulate spirituosity and alcohol content be no more than 20% food; Food simulants D1:50% ethanol water (v/v), for simulating spirituosity and the alcohol content food and the oil-water emulsion that are greater than 20%; Food simulants D2: isooctane, for simulating the food of surface containing free-fat.
By European Union (EU) NO10/2011 rules and regulations, select suitable migration test condition by table 1 Suo Shi according to product practical use:
Table 1
By European Union (EU) NO10/2011 rules and regulations, surface-to-volume compares: for < 500mL, plastic products are sheared and are put into clean glassware, with 6dm by > 10L container class plastic products or can not the flat articles of splendid attire
2the ratio of the corresponding 1L food simulants of surface area of food contact surface; For the container class plastic products of > 500mL, < 10L, then food simulants is injected into apart from container edge 4/5 place.
Two, the process of food simulants
1), the process of food simulants A, B, C, D1: accurately pipette in each food simulants 5mL to the 10mL volumetric flask after migration test, just three (2-carboxyethyl) phosphonium salt hydrochlorate mixes with tetrahydrofuran, form potpourri A, in potpourri A, the massfraction of three (2-carboxyethyl) phosphonium salt hydrochlorate is 0.05%; After potpourri A constant volume food simulants, mixing, draws each food simulants 1 ~ 2mL after above-mentioned dilution with syringe, is filtered in sample injection bottle through hydrophilic polyfluortetraethylemicroporous syringe filters, to be measured;
(2), the process of food simulants D2: accurately pipette 10mL isooctane soak solution in heart bottle, add the potpourri A described in 1mL, at 45 DEG C, 130mba condition backspin inspissation is reduced to about 1mL, blow with nitrogen again and be concentrated near doing, three (2-carboxyethyl) phosphonium salt hydrochlorate is mixed with methyl alcohol, form potpourri B, three (2-carboxyethyl) phosphonium salt hydrochlorate is mixed with methanol solution, form potpourri B, in potpourri B, the massfraction of three (2-carboxyethyl) phosphonium salt hydrochlorate is 0.05%; Accurate interpolation 1mL potpourri B, after mixing, is filtered in sample injection bottle by hydrophilic polyfluortetraethylemicroporous syringe filters, to be measured.
Three, blank test
According to food simulants A, B, C, D1, D2 that (1), (2) method process in step 2 do not contact with testing sample.
Four, liquid chromatography ultraviolet (HPLC-UV) method measures
Instrument condition:
1) chromatographic column: C8 post, height × internal diameter × thickness=250mm × 4.6mm × 5 μm, or suitable person;
2) mobile phase A is the aqueous formic acid of 0.1%, and Mobile phase B is methanol solution, condition of gradient elution: 0 ~ 1.0min, 50%B; 1.0 ~ 10.0min, 50% ~ 95%B; 10.0 ~ 15.0min, 95%B; 15.0 ~ 17.0min, 95% ~ 100%B; 17.0 ~ 25.0min, 100%B; 25.0 ~ 25.1min, 100% ~ 50%B; 25.1 ~ 30min, 50%B;
3) sample size: 20 μ L;
4) flow velocity: 1mL/min;
5) determined wavelength: 285nm;
6) column temperature: 40 DEG C;
7) quantitative manner: calibration curve external standard method, obtains the migration amount of 9 kinds of antioxidant.
According to European Union's NO10/2011 rules and regulations, testing result judges whether Special migration conforms with the regulations.
The present invention is owing to have employed above-mentioned technical scheme, food simulants A, B, C, D1 adopt containing after the dilution of 0.05%TCEP tetrahydrofuran, filter by water wettability polytetrafluoro acetic acid syringe filters, food simulants D2 adopts 0.05%TCEP tetrahydrofuran solution to keep the stability of antioxidant, and the method is quantitatively limited to 0.005 ~ 1.0mg/L in five kinds of food simulants; Aqueous-based food analogies are 3 ~ 72,0.5 ~ 12,0.3 ~ 7.2 or 0.15 ~ 3.6mg/L, and isooctane food simulants is 30 ~ 720,5 ~ 120,3 ~ 72 or good (the r of 1.5 ~ 36mg/L scope internal linear relation
2>0.9982); The recovery of standard addition of 0.3 ~ 84mg/L tri-level is 83.7% ~ 113%, and relative standard deviation is 0.8% ~ 11.2%.Result shows, the method chromatographic resolution and linear relationship better, the recovery and accuracy higher, quantitative limit meets the limitation requirement of 9 kinds of specific gross migrations of antioxidant in European Union (EU) NO10/2011 regulation subordinate list 2 completely, can efficient, easy, measure 9 kinds of specific gross migrations of antioxidant in Plastic packaging material for food and container fast.
The present invention establishes the Special migration [SML (T)] that HPLC-UV detection method measures 9 kinds of antioxidant in food contact material.The method has that sample preparation is simple and quick, chromatographic resolution effect and linear dependence is good, the recovery and accuracy comparatively advantages of higher, and the quantitative limit of method is low, can meet the limitation requirement of European Union (EU) NO10/2011 regulation completely.The method has been applied to the specific gross migration of nine kinds of antioxidant in food contact material correlated product and has detected, and can be widely used in supervision and the production quality control of nine kinds of specific gross migrations of antioxidant in food contact material correlated product.
Embodiment
Below in conjunction with embodiment, the present invention is described in further details.
Embodiment 1
High performance liquid chromatography ultraviolet (HPLC-UV) method of the present invention measures the method for 9 kinds of specific gross migrations of antioxidant in Plastic packaging material for food and container, is realized by following steps:
One, sample-pretreating method
1, migration test
1.1 food simulants: according to (EU) NO10/2011 rules and regulations, food simulants A:10% ethanol water (v/v), for simulating the aqueous food of pH > 4.5; Food simulants B:3% acetic acid aqueous solution (w/v), for simulating the acid food of pH < 4.5; Food simulants C:20% ethanol water (v/v), for simulate spirituosity and alcohol content be no more than 20% food; Food simulants D1:50% ethanol water (v/v), for simulating spirituosity and the alcohol content food and the oil-water emulsion that are greater than 20%; Food simulants D2: isooctane, for simulating the food of surface containing free-fat.
1.2 transition conditions: by European Union (EU) NO10/2011 rules and regulations, select suitable migration test condition according to table 3 Suo Shi according to product practical use:
Table 3
1.3 surface-to-volumes ratios: for < 500mL, plastic products are sheared and are put into clean glassware, with 6dm by > 10L container class plastic products or can not the flat articles of splendid attire
2the ratio of the corresponding 1L food simulants of surface area of food contact surface; For the container class plastic products of > 500mL, < 10L, then food simulants is injected into apart from container edge 4/5 place.
1.4 migrations: according to the practical use of Food Contact plastic products, be injected in plastic products or glassware according to surface-to-volume than by the food simulants selected, after vessel mouth or vessel port seal with surface plate or aluminium-foil paper, in baking oven or incubator, carry out migration test by " 2. transition condition " setting migration temperature and time.After be cooled to room temperature, food simulants is wherein transferred in clean glassware and treats subsequent treatment.
2, the process of food simulants
2.1, the process of food simulants A, B, C, D1: accurately pipette in each food simulants 5mL to the 10mL volumetric flask after migration test, three (2-carboxyethyl) phosphonium salt hydrochlorate is mixed with tetrahydrofuran, form potpourri A, in potpourri A, the massfraction of three (2-carboxyethyl) phosphonium salt hydrochlorate is 0.05%; After potpourri A constant volume food simulants, mixing, draws each food simulants 1 ~ 2mL after above-mentioned dilution with syringe, is filtered in sample injection bottle through hydrophilic polyfluortetraethylemicroporous syringe filters, to be measured;
2.2, the process of food simulants D2: accurately pipette 10mL isooctane soak solution in heart bottle, add the potpourri A described in 1mL, at 45 DEG C, 130mba condition backspin inspissation is reduced to about 1mL, blow with nitrogen again and be concentrated near doing, three (2-carboxyethyl) phosphonium salt hydrochlorate is mixed with methanol solution, form potpourri B, three (2-carboxyethyl) phosphonium salt hydrochlorate is mixed with methanol solution, form potpourri B, in potpourri B, the massfraction of three (2-carboxyethyl) phosphonium salt hydrochlorate is 0.05%; Accurate interpolation 1mL potpourri B, after mixing, is filtered in sample injection bottle by hydrophilic polyfluortetraethylemicroporous syringe filters, to be measured.
3, blank test
Test solution simulated by the food do not contacted with testing sample according to 2.1,2.2 method process.
Two, liquid chromatography ultraviolet (HPLC-UV) method condition determination:
Instrument condition:
1) chromatographic column: C8 post, height × internal diameter × thickness=250mm × 4.6mm × 5 μm, or suitable person;
2) mobile phase A is the aqueous formic acid of 0.1%, and Mobile phase B is methanol solution, condition of gradient elution: 0 ~ 1.0min, 50%B; 1.0 ~ 10.0min, 50% ~ 95%B; 10.0 ~ 15.0min, 95%B; 15.0 ~ 17.0min, 95% ~ 100%B; 17.0 ~ 25.0min, 100%B; 25.0 ~ 25.1min, 100% ~ 50%B; 25.1 ~ 30min, 50%B;
3) sample size: 20 μ L;
4) flow velocity: 1mL/min;
5) determined wavelength: 285nm;
6) column temperature: 40 DEG C;
7) quantitative manner: calibration curve external standard method calibration curve external standard method, obtains the migration amount of 9 kinds of antioxidant.
According to European Union's NO10/2011 rules and regulations, testing result judges whether Special migration conforms with the regulations.
Three, linear relationship and mensuration lower bound
The mensuration lower bound of this method is in table 4:
The mensuration lower bound (unit mg/kg) of table 4 method
Get 9 kinds of antioxidant mixed standard solutions (see table 5) to be measured of variable concentrations, by the determined instrument condition of this method and low concentration to the order sample introduction successively respectively of high concentration, with various antioxidant chromatographic peak area, linear regression is done to concentration, its concentration and chromatographic peak area linear relationship good, related coefficient is greater than 0.9982, the results are shown in Table 6.
Table 5 standard solution series concentration (unit: μ g/mL)
The range of linearity, calibration curve, the related coefficient of each antioxidant of table 6
Four, the recovery and precision test
Add 9 kinds of antioxidant mixed standard solutions of three variable concentrations levels in negative sample respectively, the average recovery of standard addition of six revision tests and precision data are in table 7.
The average recovery of standard addition of table 79 kind of antioxidant in five kinds of food simulants and precision (n=6).
The present invention detects five kinds of food simulants 10% ethanol, 3% acetic acid, 20% ethanol, 50% ethanol, the 9 kinds of specific gross migrations of antioxidant in isooctane that contact with Plastic packaging material for food by high performance liquid chromatography ultraviolet (HPLC-UV) method, the method has chromatographic resolution and linear relationship is better, the recovery and accuracy higher, quantitative limit meets the limitation requirement of 9 kinds of antioxidant Special migrations in European Union (EU) NO10/2011 regulation subordinate list 2 completely, has good using value and prospect.
Claims (3)
1. 9 kinds of antioxidant specific transfer metering methods in liquid chromatography for measuring plastic products, wherein 9 medium ultraviolet absorbing agents come from Plastic packaging material for food and container, it is characterized in that the method comprises the following steps:
One, migration test
According to the practical use of Food Contact plastic products, be injected in plastic products or glassware according to surface-to-volume than by food simulants, after vessel mouth or vessel port seal with surface plate or aluminium-foil paper, in baking oven or incubator, determine that migration temperature and transit time carry out migration test by European Union's NO10/2011 rules and regulations, after be cooled to room temperature, food simulants is wherein transferred in clean glassware and treats subsequent treatment; Wherein food simulants is divided into food simulants A, B, C, D1, D2;
Two, the process of food simulants
(1), the process of food simulants A, B, C, D1: accurately pipette in each food simulants 5mL to the 10mL volumetric flask after migration test, three (2-carboxyethyl) phosphonium salt hydrochlorate is mixed with tetrahydrofuran, form potpourri A, in potpourri A, the massfraction of three (2-carboxyethyl) phosphonium salt hydrochlorate is 0.05%; After potpourri A constant volume food simulants, mixing, draws each food simulants 1 ~ 2mL after above-mentioned dilution with syringe, is filtered in sample injection bottle through hydrophilic polyfluortetraethylemicroporous syringe filters, to be measured;
(2), the process of food simulants D2: accurately pipette 10mL isooctane soak solution in heart bottle, add the potpourri A described in 1mL, at 45 DEG C, 130mba condition backspin inspissation is reduced to about 1mL, blow with nitrogen again and be concentrated near doing, mixed with methyl alcohol by three (2-carboxyethyl) phosphonium salt hydrochlorate, form potpourri B, in potpourri B, the massfraction of three (2-carboxyethyl) phosphonium salt hydrochlorate is 0.05%; Accurate interpolation 1mL potpourri B, after mixing, is filtered in sample injection bottle by hydrophilic polyfluortetraethylemicroporous syringe filters, to be measured;
Three, blank test
According to the food simulants that (1), (2) method process in step 2 do not contact with testing sample;
Four, liquid chromatography ultraviolet method measures
Instrument condition:
1) chromatographic column: C8 post, height × internal diameter × thickness=250mm × 4.6mm × 5 μm, or suitable person;
2) mobile phase A is the aqueous formic acid of 0.1%, and Mobile phase B is methanol solution, condition of gradient elution: 0 ~ 1.0min, 50%B; 1.0 ~ 10.0min, 50% ~ 95%B; 10.0 ~ 15.0min, 95%B; 15.0 ~ 17.0min, 95% ~ 100%B; 17.0 ~ 25.0min, 100%B; 25.0 ~ 25.1min, 100% ~ 50%B; 25.1 ~ 30min, 50%B;
3) sample size: 20 μ L;
4) flow velocity: 1mL/min;
5) determined wavelength: 285nm;
6) column temperature: 40 DEG C;
7) quantitative manner: calibration curve external standard method, obtains 9 kinds of antioxidant migration amounts.
2. 9 kinds of antioxidant specific transfer metering methods in liquid chromatography for measuring plastic products according to claim 1, it is characterized in that, 9 kinds of antioxidant are respectively: n-propyl gallate, Octyl gallate, dodecyl gallate, antioxidant RC1726, antioxidant 1520, antioxidant Ionoxwsp, antioxidant ZKF, antioxidant 425, antioxidant 2246.
3. 9 kinds of antioxidant specific transfer metering methods in liquid chromatography for measuring plastic products according to claim 1, it is characterized in that the food simulants described in migration experiment and surface-to-volume ratio are according to European Union NO10/2011 rules and regulations, food simulants is respectively: 10% ethanol, 3% acetic acid, 20% ethanol, 50% ethanol, isooctane.
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| CN114324727A (en) * | 2021-11-25 | 2022-04-12 | 上海浦景化工技术股份有限公司 | Method for detecting upper limit of total migration volume of glycolic acid and oligomers thereof in PGA food packaging material |
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