CN105911205B - The method that Liquid Chromatography/Mass Spectrometry detects 3 kinds of ultraviolet absorber Special migrations - Google Patents
The method that Liquid Chromatography/Mass Spectrometry detects 3 kinds of ultraviolet absorber Special migrations Download PDFInfo
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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
- G01N30/88—Integrated analysis systems specially adapted therefor, not covered by a single one of the groups G01N30/04 - G01N30/86
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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
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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
- G01N30/04—Preparation or injection of sample to be analysed
- G01N30/06—Preparation
- G01N30/14—Preparation by elimination of some components
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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
- G01N2030/022—Column chromatography characterised by the kind of separation mechanism
- G01N2030/027—Liquid chromatography
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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
- G01N2030/062—Preparation extracting sample from raw 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
- G01N30/88—Integrated analysis systems specially adapted therefor, not covered by a single one of the groups G01N30/04 - G01N30/86
- G01N2030/8809—Integrated analysis systems specially adapted therefor, not covered by a single one of the groups G01N30/04 - G01N30/86 analysis specially adapted for the sample
- G01N2030/884—Integrated analysis systems specially adapted therefor, not covered by a single one of the groups G01N30/04 - G01N30/86 analysis specially adapted for the sample organic compounds
Abstract
The present invention provides a kind of method that Liquid Chromatography/Mass Spectrometry detects 3 kinds of ultraviolet absorber Special migrations, 3 kinds of described ultraviolet absorbers are 2 cyano group 3 being present in Plastic food contact material, 3 diphenyl-ethyl acrylates, the different monooctyl ester of 2 cyano group, 3,3 xenyl acrylic acid 2, ultraviolet absorber UV 1164.The present invention determines 3 kinds of ultraviolet absorber Special migrations simultaneously by high performance liquid chromatography tandem mass spectrum method, and chromatographic isolation and linear relationship are good, and the rate of recovery and the degree of accuracy are high, fully meet the requirement of EC regulations.The inventive method is reasonable in design, with it is sensitive, accurate, quick, easy the characteristics of, solve and 2 cyano group 3 are harmful in Plastic packaging material for food and container, the problem of this 3 kinds of ultraviolet absorber Special migration detections of 3 diphenyl-ethyl acrylates, the different monooctyl ester of 2 cyano group, 3,3 xenyl acrylic acid 2, ultraviolet absorber UV 1164.
Description
Technical field
The invention belongs to chemicals detection field, it is related in food contact material and is harmful to 2- cyano group -3,3- diphenyl propylene
Acetoacetic ester, the different monooctyl esters of 2- cyano group -3,3- xenyl acrylic acid 2-, tri- kinds of ultraviolet absorbers of ultraviolet absorber UV-1164 are specific moves
The detection method of shifting amount, more particularly to one kind detect this 3 kinds of purples using high performance liquid chromatography tandem mass spectrum (HPLC-MS/MS) method
The method of outer absorbent Special migration.
Background technology
2-cyano -3,3-diphenyl ethyl acrylate, the different monooctyl esters of 2- cyano group -3,3- xenyl acrylic acid 2-, UV absorption
This 3 kinds of ultraviolet absorbers of agent UV-1164 can be widely applied to polyvinyl chloride, poly- second frequently as ultraviolet absorber class function additive
The production of the plastics such as alkene film, polypropylene screen, polyformaldehyde, polyamide.Remain or drop in Plastic food contact material correlated product
The ultraviolet absorber of solution out, can also move to during the use in food, directly be detrimental to health.Ultraviolet absorber
Mostly lower toxicity compound, but Long Term Contact may be carcinogenic.Due to the toxic side effect of these three ultraviolet absorbers, European Union exists
The regulations of (EU) NO 10/2011 of issue in 2011,0.05mg/ is limited to by the Special migration of these three ultraviolet absorbers
kg。
At present, both at home and abroad about Uvinul N35,2- cyano group -3,3- xenyl acrylic acid -2-
Different monooctyl ester and ultraviolet absorber UV-1164 detection is concentrated mainly in toiletries sample, and the detection method used has efficiently
Liquid chromatogram ultraviolet method (HPLC-UV).Lin Rui etc. establishes HPLC-UV methods and have detected UV-1164 in water, 3% acetic acid, 10% second
Migration amount in alcohol, 20% ethanol, 50% ethanol, 65% ethanol, 95% ethanol and isooctane analogies, but do not study (EU)
The D2 of the regulation defineds of NO 10/2011 --- UV-1164 migration quantity measuring method in vegetable oil food simulants, and the party
Method is only 0.5mg/kg to UV-1164 quantitative limit, it is impossible to meet the regulation UV-1164 0.05mg/kg's of (EU) NO 10/2011
Limitation requirement.It can be seen that existing detection method can not be to 2- cyano group -3,3- diphenylprops in the regulations of European Union (EU) NO 10/2011
The Special migration of olefin(e) acid ethyl ester, the 2- cyano group -3,3- different monooctyl esters of xenyl acrylic acid -2- and ultraviolet absorber UV-116 carries out method
Quantitative detection under restrictions amount.
The content of the invention
3 kinds of ultraviolet absorber specific transfers are detected it is an object of the invention to provide a kind of liquid matter (HPLC-MS/MS) combination method
The method of amount, 3 kinds of described ultraviolet absorbers are Uvinul N35,2- cyano group -3,3- xenyl third
The different monooctyl esters of olefin(e) acid 2-, ultraviolet absorber UV-1164.This 3 kinds of ultraviolet absorbers are present in Plastic food contact material.The party
The characteristics of method has sensitive, accurate, quick, easy, solves and 2- cyano group -3 is harmful in Plastic packaging material for food and container,
3- diphenyl-ethyl acrylates, the different monooctyl esters of 2- cyano group -3,3- xenyl acrylic acid 2-, this 3 kinds of ultraviolet absorber UV-1164 are ultraviolet
The problem of absorbent Special migration detection.
The detection method of the present invention, is realized by following steps：
First, migration test
1. food simulants:According to the rules and regulations of (EU) NO 10/2011, food simulants A：10% ethanol water (v/
V), for simulating pH ＞ 4.5 aqueous food；Food simulants B：3% acetic acid aqueous solution (w/v), for simulating pH ＜'s 4.5
Acid food；Food simulants C：20% ethanol water (v/v), for simulating spirituosity and alcohol content no more than 20%
Food；Food simulants D1:50% ethanol water (v/v), for simulating the food that spirituosity and alcohol content are more than 20%
And oil-water emulsion；Food simulants D2：Vegetable oil, for simulating the food that free-fat is contained on surface.
2. transition condition：Suitable migration test condition is selected according to product practical use shown according to the form below 1：
Table 1
3. surface-to-volume ratio：For ＜ 500mL, ＞ 10L container classes plastic products or the flat articles that can not be contained,
Described surface-to-volume ratio is：For ＜ 500mL, ＞ 10L container classes plastic products or can not contain it is flat
Product, plastic products are sheared and are put into clean glassware, with the surface area correspondence 1L food of 6dm2 food contact surfaces
The ratio of analogies；For ＞ 500mL, food simulants are then injected into away from container edge by ＜ 10L container class plastic products
At 4/5.
4. migrate：According to food contact plastic products practical use, according to " 3. surface-to-volume ratio " by selection " 1.
Food simulants " are injected into plastic products or glassware, are carried out in vessel mouthful or vessel port with surface plate or aluminium-foil paper close
It is honored as a queen, migration test is carried out by " 2. transition condition " setting migration temperature and time in baking oven or incubator.Cooled down after finishing
To room temperature, food simulants therein are transferred in clean glassware and treat subsequent treatment.
2nd, food simulates the processing of test solution
1. the processing of food simulants A, B, C, D1 test solutions：After each test solution is fully mixed, 1~2mL test solutions are pipetted to 1.5
Or in 2mL centrifuge tubes, with >=10000g centrifugal speed, 5min is centrifuged, supernatant is transferred in sample injection bottle, to be measured.
2. the processing of food simulants D2 test solutions：Food simulants D2 test solutions 10g (being accurate to 0.1g) is weighed in 50mL to have
Fill in glass centrifuge tube, be separately added into 10.0mL normal heptanes and 4.00mL acetonitriles, screw plug, mixed on turbula shaker
Afterwards, then it is placed on separating funnel oscillator 300rpm and shakes 15min, then centrifuge tube is placed in a centrifuge, with >=10000g
Centrifugal speed, centrifuges 15min, acetonitrile supernatant is transferred in sample injection bottle, to be measured.
3rd, blank test
According in two 1., the food simulation test solution that 2. method processing is not contacted with testing sample.
4th, high performance liquid chromatography tandem mass spectrum (HPLC-MS/MS) method is determined
Distinguished successively with the order of blank sample, calibration curve point, blank sample, testing sample by the instrument condition of determination
Sample introduction.Calibration curve o'clock is dense with 10.0,20.0,40.0,80.0,160.0,200.0 μ g/L or μ g/kg low concentrations to high concentration
Degree order sample introduction successively respectively, with various Uvinul N35s, 2- cyano group -3,3- xenyls acrylic acid -
The different monooctyl esters of 2- and ultraviolet absorber UV-1164 chromatographic peak areas make linear regression, calibration curve quantified by external standard method to concentration.Determine
Condition：
Chromatographic column：Jupiter C4Chromatographic column (250 × 4.6mm, 5 μm) or quite person；
Mobile phase A：0.1% formic acid aqueous ammonium；
Mobile phase B：Methanol；
Gradient elution program：0~6min, 71~76%B；6~7min, 76~92%B；7~15min, 92~92%B；
15~16min, 71%B；16~20min 71%B；
Sample size：2μL；
Flow velocity：1.0mL/min；
Electric spray ion source mode of operation：Cation；
Data acquisition scheme：Multiple-reaction monitoring (MRM)；
Curtain gas：40.0μL/min；
Collision gas：Medium (Medium)；
Electric spray ion source voltage：5500V；
Temperature (TEM)：700℃；
Ion source gas 1：70.0μL/min；
Ion source gas 2：70.0μL/min；
As a further improvement, above-mentioned step two 1. middle processing mode be pipette 1~2mL test solutions to 1.5 or 2mL from
In heart pipe, with >=10000g centrifugal speed, 5min is centrifuged, it is supernatant to be transferred in sample injection bottle.
As a further improvement, above-mentioned step two amount that 2. middle food simulants D2 vegetable oil is weighed is 10g；De- ester
The amount that solvent n-heptane, Extraction solvent acetonitrile are added is respectively 10mL and 4mL；The speed that concussion is extracted is 300rpm；Concussion is carried
It is 15min to take the time；Centrifuge tube centrifugal speed after concussion is >=10000g；Centrifugation time is 15min；It is transferred into sample
Be supernatant.
As a further improvement, in above-mentioned steps four high performance liquid chromatography tandem mass spectrum (HPLC-MS/MS) method measure
Condition such as table 2 below.
Table 2
2-cyano -3,3-diphenyl ethyl acrylate, the 2- cyano group -3,3- different monooctyl esters of xenyl acrylic acid -2- and ultraviolet suction
Receive agent UV-1164 retention time and parent ion under multiple-reaction monitoring pattern, daughter ion, impact energy and remove cluster voltage parameter
Such as table 3 below.
Table 3
The present invention removes solution as a result of above-mentioned technical scheme, food simulants A, B, C, D1 using high speed centrifugation
In particulate component, food simulants D2 removes glyceride using acetonitrile and the distribution of normal heptane liquid liquid, can efficiently, it is easy, soon
2-cyano -3,3-diphenyl ethyl acrylate, 2- cyano group -3,3- biphenyl in the measure Plastic packaging material for food and container of speed
The different monooctyl esters of base acrylic acid -2- and ultraviolet absorber UV-1164 Special migrations.
The present invention is to 2-cyano -3,3-diphenyl ethyl acrylate, the different monooctyl esters of 2- cyano group -3,3- xenyl acrylic acid -2-
Measure lower bound with ultraviolet absorber UV-1164 is as shown in table 4 below.
Table 4
The present invention determines 3 kinds of ultraviolet absorber Special migrations, chromatogram simultaneously by high performance liquid chromatography-tandem mass method
Separation and linear relationship are good, and the rate of recovery and the degree of accuracy are high, fully meet 2- cyanogen in the regulation subordinate lists 1 of European Union (EU) NO 10/2011
Base -3,3- diphenyl-ethyl acrylates, the different monooctyl esters of 2- cyano group -3,3- xenyl acrylic acid 2-, ultraviolet absorber UV-1164 spy
Determine migration amount limitation requirement, and be applied to the detection of actual sample.The inventive method is reasonable in design, with sensitive, accurate, fast
The characteristics of speed, simplicity, solve and 2- cyano group -3,3- diphenylacrylate second is harmful in Plastic packaging material for food and container
Ester, the different monooctyl esters of 2- cyano group -3,3- xenyl acrylic acid 2-, ultraviolet absorber UV-1164 this 3 kinds of ultraviolet absorber Special migrations
The problem of detection.
Embodiment
The present invention is further described in conjunction with the embodiments.
Embodiment 1
First, sample-pretreating method
1st, migration test
1.1 food simulants:According to the rules and regulations of (EU) NO 10/2011, food simulants A：10% ethanol water
(v/v), for simulating pH ＞ 4.5 aqueous food；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), for simulating spirituosity and alcohol content is no more than
20% food；Food simulants D1:50% ethanol water (v/v), is 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 condition：Suitable migration test condition is selected according to product practical use shown according to the form below 5：
Table 5
1.3 surface-to-volume ratios：For ＜ 500mL, ＞ 10L container classes plastic products or the flat articles that can not be contained,
Plastic products are sheared and are put into clean glassware, with the surface area correspondence 1L food simulants of 6dm2 food contact surfaces
Ratio；For ＞ 500mL, food simulants are then injected into away from container edge 4/5 by ＜ 10L container class plastic products.
1.4 migration：The practical use of plastic products is contacted according to food, according to " 3. surface-to-volume ratio " by selection
" 1. food simulants " are injected into plastic products or glassware, are carried out in vessel mouthful or vessel port with surface plate or aluminium-foil paper
After sealing, migration test is carried out by " 2. transition condition " setting migration temperature and time in baking oven or incubator.Finish rear cold
But to room temperature, food simulants therein is transferred in clean glassware and treat subsequent treatment.
2nd, food simulates the processing of test solution
The processing of 2.1 food simulants A, B, C, D1 test solutions：After each test solution is fully mixed, 1~2mL test solutions are pipetted extremely
In 1.5 or 2mL centrifuge tubes, with >=10000g centrifugal speed, 5min is centrifuged, supernatant is transferred in sample injection bottle, to be measured.
The processing of 2.2 food simulants D2 food simulants test solutions：Weigh olive oil analogies 10g (being accurate to 0.1g) in
In 50mL tool plug glass centrifuge tubes, 10.0mL normal heptanes and 4.00mL acetonitriles are separately added into, plug is screwed, on turbula shaker
After mixing, then 300rpm concussions 15min on separating funnel oscillator is placed in, then centrifuge tube is placed in a centrifuge, with >=
10000g centrifugal speed, centrifuges 15min, acetonitrile supernatant is transferred in sample injection bottle, to be measured.
3rd, blank test
The food simulation test solution not contacted according to 2.1,2.2 methods processing in two with testing sample.
2nd, Liquid Chromatography-Tandem Mass Spectrometry (HPLC-MS/MS) method condition determination：
High performance liquid chromatography tandem mass spectrum (HPLC-MS/MS) method liquid phase chromatogram condition and part Mass Spectrometry Conditions parameter are shown in Table
6。
The liquid phase chromatogram condition of table 6 and part Mass Spectrometry Conditions
2-cyano -3,3-diphenyl ethyl acrylate, the 2- cyano group -3,3- different monooctyl esters of xenyl acrylic acid -2- and ultraviolet suction
Receive parent ions of the agent UV-1164 under multiple-reaction monitoring pattern, daughter ion, impact energy and go cluster voltage to be shown in Table 7.
Parent ion, daughter ion, impact energy under the multiple-reaction monitoring pattern of table 7 and remove cluster voltage
3rd, linear relationship and measure lower bound
The measure lower bound of this method is shown in Table 8.
The measure lower bound of the method for table 8
Take 2-cyano -3,3-diphenyl ethyl acrylate, the 2- cyano group -3,3- xenyl acrylic acid -2- of various concentrations different
Monooctyl ester and ultraviolet absorber UV-1164 mixed standard solutions (being shown in Table 9), instrument condition and low concentration as determined by this method
Order to high concentration distinguishes sample introduction successively, with various Uvinul N35s, 2- cyano group -3,3- biphenyl
The different monooctyl esters of base acrylic acid -2- and ultraviolet absorber UV-1164 chromatographic peak areas make linear regression to concentration, its concentration and chromatographic peak
Area linear relation is good, correlation coefficient r2>0.99956, it the results are shown in Table 10.
The standard liquid series concentration unit of table 9：μ g/L or μ g/kga
aOlive oil food simulants
The range of linearity of table 10, calibration curve, coefficient correlation
4th, the rate of recovery and precision test
2-cyano -3,3-diphenyl ethyl acrylate, the 2- cyanogen of three various concentrations levels are added in negative sample respectively
Base -3,3- different monooctyl esters of xenyl acrylic acid -2- and ultraviolet absorber UV-1164 mixed standard solutions, it is flat that six repetitions are tested
Equal recovery of standard addition and precision data are shown in Table 11.
Average recovery of standard addition and precision (n=6) in 11 5 kinds of food simulants of table
Claims (1)
1. a kind of liquid MS detects the method for 3 kinds of ultraviolet absorber Special migrations, 3 kinds of described ultraviolet absorber spies
Surely come from Plastic packaging material for food and container, respectively Uvinul N35,2- cyano group-
3, the 3- different monooctyl esters of xenyl acrylic acid 2-, ultraviolet absorber UV-1164, it is characterised in that realized by following steps：
First, migration test
The practical use of plastic products is contacted according to food, according to surface-to-volume than the food simulants of selection are injected into modeling
In material products container or glassware, sealed in glassware mouthful or plastic products vessel port with surface plate or aluminium-foil paper
Afterwards, migration test is carried out by transition condition setting migration temperature and time in baking oven or incubator, room temperature is cooled to after finishing,
Food simulants test solution therein is transferred in clean glassware and treats subsequent treatment；Wherein food simulants are divided into food mould
Intend thing A, B, C, D1, D2；
2nd, the processing of food simulants test solution
(1) processing of food simulants A, B, C, D1 test solutions：After each test solution is fully mixed, pipette 1~2mL test solutions to 1.5 or
In 2mL centrifuge tubes, with >=10000g centrifugal speed, 5min is centrifuged, supernatant is transferred in sample injection bottle, to be measured；
(2) processing of food simulants D2 test solutions：Food simulants D2 test solutions 10g is weighed in 50mL tool plug glass centrifuge tubes,
10.0mL normal heptanes and 4.00mL acetonitriles are separately added into, after being mixed on turbula shaker, then is placed on separating funnel oscillator
300rpm shakes 15min, then centrifuge tube is placed in a centrifuge, and with >=10000g centrifugal speed, centrifuges on 15min, acetonitrile
Clear liquid is transferred in sample injection bottle, to be measured；
3rd, blank test
Food simulants A, B, C, D1, D2 that method processing according to (1) in step 2, (2) is not contacted with testing sample；
4th, liquid chromatography tandem mass spectrometry is determined
Entered successively respectively with the order of blank sample, calibration curve point, blank sample, testing sample by the instrument condition of determination
Sample, calibration curve o'clock is entered successively respectively with 10.0,20.0,40.0,80.0,160.0,200.0 μ g/L or μ g/kg concentration order
Sample, with various Uvinul N35s, 2- cyano group -3,3- different monooctyl esters of xenyl acrylic acid -2- and ultraviolet suction
Receive agent UV-1164 chromatographic peak areas and make linear regression, calibration curve quantified by external standard method to concentration；
Condition determination：
Condition determination is as follows：
Chromatographic column：Jupiter C4Chromatographic column, 250 × 4.6mm, 5 μm；
Mobile phase A：0.1% formic acid aqueous ammonium；
Mobile phase B：Methanol；
Gradient elution program：0~6min, 71~76%B；6~7min, 76~92%B；7~15min, 92~92%B；15~
16min, 71%B；16~20min 71%B；
Sample size：2μL；
Flow velocity：1.0mL/min；
Electric spray ion source mode of operation：Cation；
Data acquisition scheme：Multiple-reaction monitoring；
Curtain gas：40.0μL/min；
Collision gas：It is medium；
Electric spray ion source voltage：5500V；
Temperature：700℃；
Ion source gas 1：70.0μL/min；
Ion source gas 2：70.0μL/min；
The food simulants A：10% ethanol water, food simulants B：3% acetic acid aqueous solution, food simulants C：20%
Ethanol water, food simulants D1：50% ethanol water, food simulants D2：Vegetable oil；
Surface-to-volume ratio described in step one is：For ＜ 500mL, ＞ 10L container classes plastic products or it can not contain
Flat articles, plastic products are sheared and are put into clean glassware, with the surface area correspondence 1L of 6dm2 food contact surfaces
The ratio of food simulants；For ＞ 500mL and ＜ 10L container class plastic products, then food simulants are injected into away from appearance
At device edge 4/5.
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