CN105021725B - Liquid chromatography-tandem mass spectrometry method for detection of specific total migration of nine ultraviolet absorbers - Google Patents
Liquid chromatography-tandem mass spectrometry method for detection of specific total migration of nine ultraviolet absorbers Download PDFInfo
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Abstract
The present invention provides a liquid chromatography-tandem mass spectrometry method for detection of specific total migration of nine ultraviolet absorbers. The method is as below: soaking a sample to be measured in a food simulant, cooling to room temperature and mixing well; diluting the water-based food simulant with ethanol by 1:10, filtering by a hydrophilic PTFE filter and introducing the sample; extracting the olive oil with acetonitrile n-heptane, and filtering the lower clear liquid with a hydrophilic PTFE filter and introducing the sample; Conducting gradient elution and separation by a C8 column; and running under negative multiple reaction monitoring mode by using a mass spectrometry with electro-spray ionization source. The method has good chromatographic separation and linear relationship, high recovery and accuracy, meets the limit requirements on specific total migration of the 9 ultraviolet absorbers in EU regulations (EU) NO 10/2011, and has been applied to actual detection of samples.
Description
Technical field
The invention belongs to chemicals detection field, it is related to that harmful 9 kinds of ultraviolet absorbers in food contact material are specific to be moved
The detection method of shifting amount, more particularly, to a kind of high performance liquid chromatography tandem mass spectrum (hplc-ms/ms) method detection plastics based food connects
The method of the Special migration of 9 kinds of ultraviolet absorbers in tactile material.
Technical background
Plastic food contact material often need to add the function additives such as ultraviolet absorber (uv), antioxidant to extend correlation
The service life of product.But during product uses, the uv that these are added also can move in food, directly endanger people
The health of body.(eu) no 10/2011 regulation that European Union issued in 2011 is by the Special migration (sml) or specific of multiple uv
Gross migration [sml (t)] is limited.
At present, both at home and abroad about ultraviolet absorber detection be concentrated mainly on cosmetics, environmental water sample, biological tissue and
In food simulants class sample, the detection method of use mainly includes hplc method and hplc-ms/ms method.The relevant food of report
In product analogies, the detection method of ultraviolet absorber is all hplc method, due to the ultraviolet absorber species that detects and number simultaneously
Difference, existing detection method cannot be to the specific gross migration of 9 kinds of ultraviolet absorbers in (eu) no 10/2011 regulation subordinate list 2
Detected.
Content of the invention
In order to solve the difficulty of harmful W absorbent specific gross migration detection in Plastic packaging material for food and container
Topic, the invention provides in a kind of high performance liquid chromatography tandem mass spectrum (hplc-ms/ms) method detection Plastic food contact material
The detection method of the specific gross migration of 9 kinds of ultraviolet absorbers, the method has the characteristics that sensitive, accurate, quick, easy.
9 kinds in high performance liquid chromatography tandem mass spectrum (hplc-ms/ms) the method detection Plastic food contact material of the present invention
The method of the Special migration of ultraviolet absorber, is realized by following steps:
First, migration test
Contact the practical use of plastic according to food, inject than by food simulants according to certain surface-to-volume
To in testing sample plastic or glass drying oven, after vessel mouth or vessel port are sealed with surface plate or aluminium-foil paper,
Determine that migration temperature and migration time carry out migration test by European Union (eu) no10/2011 rules and regulations in baking oven or incubator,
It is cooled to room temperature after finishing, food simulants therein are transferred in clean glass drying oven and treats subsequent treatment.
Food simulants therein are according to (eu) no 10/2011 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 ph ＜
4.5 acid food；Food simulants c:20% ethanol water (v/v), are less than for simulating spirituosity and alcohol content
20% food；Food simulants d1:50% ethanol water (v/v), are more than 20% for simulating spirituosity and alcohol content
Food and oil-water emulsion；Food simulants d2: vegetable oil, for simulating the food that free-fat is contained on surface.
By European Union (eu) no 10/2011 rules and regulations, according to the form below 1 specifies, selects suitably to move according to product practical use
Shift test condition.
Table 1
By European Union (eu) no 10/2011 rules and regulations, surface-to-volume ratio: for ＜ 500ml, ＞ 10l container class plastics
Product or the flat articles that can not contain, plastic are sheared and put in clean glass drying oven, with 6dm2Food contacts
The ratio of the corresponding 1l food simulants of the surface area in face；For ＞ 500ml, the container class plastic of ＜ 10l, then by food mould
Intend thing to be injected at container edge 4/5.
2nd, the process of food simulants
(1), the process of food simulants a, b, c, d1: after each food simulants completing migration test are fully mixed,
Accurately pipette in 1.0ml to 10ml volumetric flask, after ethanol constant volume, mix, draw each food after above-mentioned dilution with syringe
Analogies 1～2ml, filters to sample injection bottle through hydrophilic polyfluortetraethylemicroporous syringe filters, to be measured；
(2), the process of food simulants d2: weigh vegetable oil food simulants 2g (being accurate to 0.01g) and have lid in 50ml
In glass centrifuge tube, sequentially add 10ml normal heptane, 0.2ml oxolane and 10ml acetonitrile, screw lid, 300rpm shakes
20min, then stand 15min, draw lower floor acetonitrile solution 1～2ml with 2ml syringe, cross 0.45 μm of ptfe syringe filters extremely
In 2ml sample injection bottle, to be measured.
3rd, blank assay
Food simulants a, b, c, d1, the d2 not contacted with testing sample according to (1), the process of (2) method in two.
4th, high performance liquid chromatography tandem mass spectrum (hplc-ms/ms) method
Instrument condition:
1) chromatographic column: c8 post, height × internal diameter × thickness=250mm × 4.6mm × 5 μm, or suitable person；
2) mobile phase a: pure water；Mobile phase b: volume fraction is 25% isopropanol methanol solution；Condition of gradient elution: 0
～5.0min:35～90%b；5.0～10.0min:90%b；10.0～10.1min:90～100%b；10.1～13.5min:
100%b；13.5～14.0min:100 35%b；14.0 16.5min:35%b；
3) column temperature: 40 DEG C；
4) sample size: 10 μ l；
5) flow velocity before post: 1ml/min；
6) after post, tee T introduces mobile phase: 0.5% diethylamine aqueous solution；
7) introduce flow rate of mobile phase: 0.20ml/min after post；
8) electric spray ion source mode of operation: anion；
9) data acquisition scheme: multiple-reaction monitoring；
10) curtain gas: 40 μ l/min；
11) collision gas: medium；
12) electric spray ion source voltage: -4500v；
13) temperature: 700 DEG C；
14) ion source gas: gas 1,70.0 μ l/min；Gas 2,70.0 μ l/min；
15) entrance potential: -10.0v；
16) collision cell exit potential: -8.0v；
17) quantitative manner: calibration curve external standard method, obtain the migration amount of 9 kinds of ultraviolet absorbers.
According to European Union no 10/2011 rules and regulations, testing result judges whether Special migration is qualified.
The present invention due to employing above-mentioned technical scheme, food simulants a, b, c, d1 adopt ethanol dilution after, with parent
Aqueouss polytetrafluoro acetic acid syringe filters filter, and it is sweet in vegetable oil that food simulants d2 adopts the distribution of acetonitrile normal heptane liquid liquid to remove
Grease, can efficiently, easy, quickly measure in Plastic packaging material for food and container that 9 kinds of ultraviolet absorbers are specific always to be moved
Shifting amount.Quantitation in 5 kinds of food simulants for the method is limited to 0.01～0.3mg/kg；0.05～1.2mg/l, 0.25～
In the range of 6mg/l, 0.5～12mg/kg or 2.5～60mg/kg, linear relationship is good (r > 0.99535)；1～35mg/kg level
Recovery of standard addition be 80.0%～127%, relative standard deviation be 0.8%～8.0%.Result shows, the method chromatograph is divided
From with linear relationship preferably, the response rate and accuracy are high, fully meet 9 kinds of purples in European Union (eu) no 10/2011 regulation subordinate list 2
The limitation requirement of the specific gross migration of outer absorbent.The present invention is as shown in table 2 to the mensure lower bound of 9 kinds of ultraviolet absorbers:
Table 2
The present invention establish high performance liquid chromatography-tandem mass method measure food contact material in uv-24, uv-0, uv-9,
The specific gross migration [sml (t)] of 9 kinds of uv such as dhbp, uv-531, hhbp, uv-p, uv-327, uv-326.The method has sample
Product process simple and quick, chromatographic isolation effect and linear dependence is good, the response rate and accuracy higher the advantages of, the quantitation of method
Limit, can fully meet the limitation requirement of 9 kinds of ultraviolet absorbers sml (t) in European Union (eu) no 10/2011 regulation subordinate list 2, the party
Method has been applied to the detection of the specific gross migration of 9 kinds of ultraviolet absorbers in food contact material correlated product, and in polyethylene
The migration having uv-326 in the preservative film of material detects detection.This method can be widely applied in food contact material correlated product
The Management of 9 kinds of ultraviolet absorbers sml (t) and control of product quality.
Specific embodiment
With reference to embodiment, the present invention is described in further details.
Embodiment 1
The present invention provides a kind of high performance liquid chromatography tandem mass spectrum (hplc-ms/ms) method detection plastics based food contact material
The method of the Special migration of 9 kinds of ultraviolet absorbers in material, is realized by following steps:
First, sample-pretreating method
1st, migration test
1.1 food simulants: according to (eu) no 10/2011 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 ph ＜
4.5 acid food；Food simulants c:20% ethanol water (v/v), are less than for simulating spirituosity and alcohol content
20% food；Food simulants d1:50% ethanol water (v/v), are more than 20% for simulating spirituosity and alcohol content
Food and oil-water emulsion；Food simulants d2: vegetable oil, for simulating the food that free-fat is contained on surface.
1.2 transition conditions: according to (eu) no 10/2011 rules and regulations, selected according to product practical use shown according to the form below
Suitable migration test condition (table 3):
Table 3
1.3 surface-to-volume ratios: for ＜ 500ml, ＞ 10l container class plastic or the flat articles that can not contain,
Plastic is sheared and puts in clean glass drying oven, 1l food simulants are corresponded to the surface area of 6dm2 food contact surface
Ratio；For ＞ 500ml, the container class plastic of ＜ 10l, then food simulants are injected at container edge 4/5.
1.4 migrations: contact the practical use of plastic according to food, according to surface-to-volume than each food that will select
Analogies are injected in testing sample plastic or glass drying oven, are carried out with surface plate or aluminium-foil paper in vessel mouth or vessel port
After sealing, set migration temperature and time by transition condition in baking oven or incubator and carry out migration test.It is cooled to after finishing
Room temperature, food simulants therein is transferred in clean glass drying oven and treats subsequent treatment.
2nd, the process of food simulants
The process of 2.1 food simulants a, b, c, d1: after each food simulants completing migration test are fully mixed, accurate
Really pipette in 1.0ml to 10ml volumetric flask, after ethanol constant volume, mix, draw each food mould after above-mentioned dilution with syringe
Intend thing 1～2ml, filter to sample injection bottle through hydrophilic polyfluortetraethylemicroporous syringe filters, to be measured；
The process of 2.2 food simulants d2: weigh vegetable oil food simulants 2g (being accurate to 0.01g) and have lid glass in 50ml
In glass centrifuge tube, sequentially add 10ml normal heptane, 0.2ml oxolane and 10ml acetonitrile, screw lid, 300rpm shakes
20min, then stand 15min, draw lower floor acetonitrile solution 1～2ml with 2ml syringe, cross 0.45 μm of ptfe syringe filters extremely
In 2ml sample injection bottle, to be measured.
3rd, blank assay
The food simulants not contacted with testing sample according to 2.1,2.2 method process.
2nd, high performance liquid chromatography tandem mass spectrum (hplc-ms/ms) method condition determination:
Liquid phase chromatogram condition and part Mass Spectrometry Conditions parameter are shown in Table 4, the retention time of 9 kinds of ultraviolet absorbers and reacting more
Parent ion under monitoring pattern, daughter ion, impact energy and go cluster voltage parameter to be shown in Table 5.
Table 4 liquid phase chromatogram condition and part Mass Spectrometry Conditions
Parent ion under multiple-reaction monitoring pattern for the 59 kinds of ultraviolet absorbers of table, daughter ion, impact energy and remove cluster voltage
3rd, linear relationship and mensure lower bound
The mensure lower bound of this method is shown in Table 6:
The mensure lower bound of table 6 method
Take 9 kinds of ultraviolet absorber mixed standard solutions (being shown in Table 7) to be measured of variable concentrations, or according to 2.2 operation, and add
Plus a series of mixed standard solution (being shown in Table 8), and processed according to 2.2 operation, then standard solution or working solution are pressed
Instrument condition determined by this method from low concentration to the order of high concentration respectively sample introduction successively, with various ultraviolet absorber chromatographs
Peak area makees linear regression to concentration, and its concentration is good with chromatographic peak area linear relationship, and correlation coefficient is all higher than 0.99535,
The results are shown in Table 9.
The standard liquid series concentration (unit: μ g/ml) of table 7 food simulants a, b, c, d1
The standard working solution series concentration (unit: mg/kg) of table 8 food simulants d2
The range of linearity in 5 kinds of food simulants for the 99 kinds of uv of table, correlation coefficient, linear equation
4th, the response rate and precision test
Add 9 kinds of ultraviolet absorber mixed standard solutions of three variable concentrations levels, six weights respectively in negative sample
The average recovery of standard addition that retrial is tested and precision data are shown in Table 10.
Average recovery of standard addition in five kinds of food simulants for the 10 9 kinds of ultraviolet absorbers of table and precision (n=6).
The inventive method soaks testing sample by food simulants, is cooled to room temperature and mixes, aqueous-based food analogies
Press 1:10 dilution, sample introduction after filtering through hydrophilic polytetrafluoro acetic acid syringe filters with ethanol；Olive oil acetonitrile normal heptane carries
After taking, lower clear liquid sample introduction after the filtration of hydrophilic polytetrafluoro acetic acid syringe filters.Use c8Post is gradient elution separation；Mass spectrum tool electricity
Esi ion source, runs under anion multiple-reaction monitoring pattern.The method chromatographic isolation and linear relationship preferably, the response rate and
Accuracy is high, fully meets the limitation requirement to the specific gross migration of 9 kinds of ultraviolet absorbers for European Union (eu) no 10/2011 regulation,
And it is applied to the detection of actual sample.
Claims (2)
1. the method for the specific gross migration of 9 kinds of ultraviolet absorbers of Liquid Chromatography/Mass Spectrometry detection, in wherein 9, ultraviolet absorber comes from and moulds
It is characterised in that being realized by following steps in material based food packing materials and containers for foods:
First, migration test
Contact the practical use of plastic according to food, be injected into plastic according to surface-to-volume than by food simulants
Or in glass drying oven, after glass drying oven mouth or plastic vessel port are sealed with surface plate or aluminium-foil paper, in baking oven or
Determine that migration temperature and migration time carry out migration test by European Union no 10/2011 rules and regulations in incubator, cool down after finishing
To room temperature, food simulants therein are transferred in clean glass drying oven and treats subsequent treatment；Wherein food simulants are divided into food
Product analogies a, b, c, d1, d2；
2nd, the process of test solution simulated by food
(1) process of food simulants a, b, c, d1 test solution: will be fully mixed to food simulants a, b, c, d1 of completing migration test
After even, accurately pipette in 1.0ml to 10ml volumetric flask, after ethanol constant volume, mix, drawn with syringe each after above-mentioned dilution
Food simulants 1～2ml, filters to sample injection bottle through hydrophilic polyfluortetraethylemicroporous syringe filters, to be measured；
(2) process of food simulants d2 test solution: be accurate to 0.01g and weigh vegetable oil food simulants 2g in 50ml tool cover glass
In centrifuge tube, sequentially add 10ml normal heptane, 0.2ml oxolane and 10ml acetonitrile, screw lid, 300rpm shakes 20min,
Stand 15min again, draw lower floor acetonitrile solution 1～2ml with 2ml syringe, cross 0.45 μm of politef syringe filters extremely
In 2ml sample injection bottle, to be measured；
3rd, blank assay
Process food simulants a, b, c, d1, the d2 not carrying out migration test according to (1), (2) method in step 2；
4th, liquid chromatography tandem mass spectrometry measures
Instrument condition:
1) chromatographic column: c8 post, height × internal diameter × thickness=250mm × 4.6mm × 5 μm；
2) mobile phase a: pure water；Mobile phase b: volume fraction is 25% isopropanol methanol solution；Condition of gradient elution: 0～
5.0min:35～90%b；5.0～10.0min:90%b；10.0～10.1min:90～100%b；10.1～13.5min:
100%b；13.5～14.0min:100 35%b；14.0 16.5min:35%b；
3) column temperature: 40 DEG C；
4) sample size: 10 μ l；
5) flow velocity before post: 1ml/min；
6) after post, tee T introduces mobile phase: 0.5% diethylamine aqueous solution；
7) introduce flow rate of mobile phase: 0.20ml/min after post；
8) electric spray ion source mode of operation: anion；
9) data acquisition scheme: multiple-reaction monitoring；
10) curtain gas: 40 μ l/min；
11) collision gas: medium；
12) electric spray ion source voltage: -4500v；
13) temperature: 700 DEG C；
14) ion source gas: gas 1,70.0 μ l/min；Gas 2,70.0 μ l/min；
15) entrance potential: -10.0v；
16) collision cell exit potential: -8.0v；
17) quantitative manner: calibration curve external standard method, obtain the migration amount of 9 kinds of ultraviolet absorbers；
9 kinds of described ultraviolet absorbers are respectively as follows: 2,2'- dihydroxy -4- methoxy benzophenone, 2,4- dihydroxy hexichol first
Ketone, ESCALOL 567,4,4'- dihydroxy benaophenonel, Octabenzone, 2- bis-
Hydroxyl -4- hexyloxy benzophenone, 2- (2'- hydroxyl -5'- aminomethyl phenyl) benzotriazole, 2- (3,5- di-t-butyl -2- oxybenzene
Base), 2- (5- chloro- 2- benzotriazole base) -6- Butylated Hydroxytoluene.
2. the method that Liquid Chromatography/Mass Spectrometry according to claim 1 detects the specific gross migration of 9 kinds of ultraviolet absorbers, its feature
It is the food simulants described in migration test and surface-to-volume than according to European Union no 10/2011 rules and regulations, food mould
Intend thing and be respectively as follows: 10% ethanol, 3% acetic acid, 20% ethanol, 50% ethanol, vegetable oil.
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| CN105911205B (en) * | 2016-04-25 | 2017-10-10 | 中华人民共和国台州出入境检验检疫局 | The method that Liquid Chromatography/Mass Spectrometry detects 3 kinds of ultraviolet absorber Special migrations |
| CN105911189B (en) * | 2016-04-25 | 2018-04-20 | 中华人民共和国台州出入境检验检疫局 | The method of 4 species amino benzenes derivates Special migration of liquid chromatography and mass spectrometry |
| CN106353444B (en) * | 2016-11-03 | 2018-03-23 | 广州中科检测技术服务有限公司 | The detection method of the methoxy benzophenone of 2 hydroxyl 4 and butyl methoxydibenzoylmethise in soil |
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| CN104198640B (en) * | 2014-09-10 | 2016-06-08 | 宁波检验检疫科学技术研究院 | In food contact material, aldehydes matter migrates to the assay method of oiliness analogies |
| CN104483428B (en) * | 2014-12-09 | 2016-03-09 | 浙江出入境检验检疫局检验检疫技术中心 | The LC-MS detection method of textile benzophenone anti-ultraviolet finishing agent |
| CN104502474B (en) * | 2014-12-10 | 2016-03-09 | 浙江出入境检验检疫局检验检疫技术中心 | The liquid phase chromatography detection method of benzophenone anti-ultraviolet finishing agent in textile |
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