CN105203659A - Determination method for 2-hydroxy-4-methoxybenzophenone in dried food simulant - Google Patents

Determination method for 2-hydroxy-4-methoxybenzophenone in dried food simulant Download PDF

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CN105203659A
CN105203659A CN201510590565.4A CN201510590565A CN105203659A CN 105203659 A CN105203659 A CN 105203659A CN 201510590565 A CN201510590565 A CN 201510590565A CN 105203659 A CN105203659 A CN 105203659A
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escalol
dry food
food analogies
naphthalene
assay method
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CN105203659B (en
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罗世鹏
季玮玉
张敏
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CHANGZHOU TESTING AND TECHNICAL CENTER FOR DANGEROUS GOODS AND PACKAGING
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CHANGZHOU TESTING AND TECHNICAL CENTER FOR DANGEROUS GOODS AND PACKAGING
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Abstract

The invention relates to a determination method for 2-hydroxy-4-methoxybenzophenone in dried food simulant. The method includes the steps that the dried food simulant with the mass of m is taken for preparing testing liquid containing naphthalene-d8, a standard working solution is prepared, gas chromatography-tandem triple quadrupole mass spectrometry detection is performed, and the content of 2-hydroxy-4-methoxybenzophenone in the dried food simulant is calculated according to the correction factor formula that f=(AIS*mi)/(Ai*mI) and the formula that X=(A*mS*f)/(AS*m), wherein the error of the final result can be reduced through a parallel test. The detection method for the migration amount of 2-hydroxy-4-methoxybenzophenone in the dried food simulant is established for the first time; according to the measurement method, a sample extracting solution is directly injected after passing through a concentration and filtration membrane, and no complex pretreatment like derivatization is needed.

Description

The assay method of ESCALOL 567 in a kind of dry food analogies
Technical field
The present invention relates to the assay method of ESCALOL 567 in a kind of dry food analogies.
Background technology
2009, the quick early warning system of European Union's food and feed class (RASFF) have advertised oatmeal and is subject to the event that in packaging for foodstuff printing-ink, 4-methyl benzophenone (4-MBP) and benzophenone (BP) pollute, and this shows that dry food also may suffer the pollution of the contact materials such as packaging.Accordingly, European Union's food chain and animal health standing committee have formulated the maximum migration limitation of the printing-ink packaging for foodstuff of multiple Benzophenone-type light initiator, the migration limitation defining the 2-hydroxy-4-methyl benzophenone in packaging for foodstuff printing-ink material is 6.0mg/kg, China GB9685 specifies equally, and in plastic-food contact material, the migration limitation of 2-hydroxy-4-methyl benzophenone is 6.0mg/kg.2011, in plastics regulation (EU) No.10/2011 that EU Committee puts into effect, then clear stipulaties is that modification poly-(2,6-diphenyl-p-phenylene) is as dry food analogies for the food simulants of the dry food such as starch, cereal, dried noodle, solid-state carbohydrate, nut, milk powder, bread.There is not been reported in the domestic and international detection for 2-hydroxy-4-methyl benzophenone migration amount in dry food analogies at present.Therefore set up the quantitative detecting method of 2-hydroxy-4-methyl benzophenone migration amount in dry food analogies, can effectively to test supervision to the sanitation performance of food contact material, thus protection people's is healthy and safe.
In analyte detection process, the accuracy of quantitative analysis results and the selection of sample pre-treatments step and chromatographic mass spectrometry condition closely bound up, be not only just can determine optimum chromatogram measuring condition through limited experiment, if departed to some extent the setting analyzing testing conditions, then very large error be may cause to quantitative testing result, false positive or diametrically opposite testing result even can be obtained.
Summary of the invention
The object of this invention is to provide a kind of assay method checking ESCALOL 567 in the dry food analogies that precision is high, error is little.
The technical scheme realizing the object of the invention is as follows:
In dry food analogies, an assay method for ESCALOL 567, comprises the following steps,
Step one, gets the dry food analogies that quality is m, adds containing known quality m snaphthalene-d 8solvent extraction filter after more concentrated constant volume obtain test fluid;
Step 2, carries out gas chromatography-triple level Four bar Mass Spectrometer Method of connecting to test fluid, gets the instrument of gained to naphthalene-d 8response signal is interior mark peak area A s, the instrument getting gained is test sample peak area A to ESCALOL 567 response signal;
Step 3, produces standard working solution, prepare one group with containing quality m inaphthalene-d 8the ESCALOL 567 standard working solution of internal standard compound, then carries out gas chromatography-triple level Four bar Mass Spectrometer Method of connecting to standard working solution, according to detecting the naphthalene-d obtained 8quantitative distance values peak area A iSand corresponding quality m i, in conjunction with detecting the ESCALOL 567 quota ion peak area A obtained iand corresponding quality m i , then according to formulae discovery correction factor f; F=(A iS× m i)/(A i× m i)
Step 4, by step 2 with obtained testing result A sand A, and sample quality m in step one and added interior mark quality m s, the correction factor f obtained in integrating step three is then according to formula X=(A × m s× f)/(A s× m) calculate the content X of ESCALOL 567 in dry food analogies 1, wherein:
X represents the content of ESCALOL 567 in dry food analogies, and unit is mg/kg.
Step 5, repeats step one and carries out parallel experiment to step 4, obtain replicate test result X 2, with the arithmetic mean of twice test result, i.e. X=(X 1+ X 2)/2 are as test result.
The present invention under ion gun to internal standard compound naphthalene-d 8and ESCALOL 567 carries out cracking, obtain both one-level cracking peaks, then secondary cracking is carried out to one-level fragment, and second order ms fragment is analyzed, the present invention establishes the detection method of ESCALOL 567 migration amount in dry food analogies first, described measuring method is sample extracting solution direct injected after concentrated filter membrane, does not need to carry out the pre-treatment steps such as complicated derivatization.
Preferably, in order to make dry food analogies be uniformly dissolved, the convenient ESCALOL 567 extracted wherein, in step one during solution dry food analogies, adopts containing naphthalene-d 8methanol solution dissolve, ultrasonic instrument 5-60min is opened in course of dissolution, temperature controls at 0-100 DEG C, after preliminarily solubilised filters, a dissolution filter operation is carried out again to filter residue methanol solution, the solution that twice filtration obtains concentrates constant volume 1-10mL after merging again, and cross organic filter membrane, described organic filter sizes is 0.1 μm-0.45 μm.
Preferably, in order to reduce the error of testing result, the permissible error of parallel experiment in step 5 is 20%.
Preferably, in order to ensure the degree of accuracy of standard working solution, the standard working solution in step 3 by content be greater than 99.0% ESCALOL 567 standard items and content be greater than 99.0% naphthalene-d 8standard items and Chromatographic Pure Methanol dissolve constant volume to be made.
Preferably, in order to improve the precision of gas chromatographic detection, in step 2 and step 3, chromatographic column coating is polyglycol, polystyrene or polymethyl siloxane material, chromatogram column length is 30-60m, and chromatographic column internal diameter is 0.18mm-0.25mm, and coating thickness is 0.20-0.30 μm, sample size is 0.5-2.0 μ L, the initial temperature 80-110 DEG C of gas chromatography, keeps 0-4min, is warming up to 220-280 DEG C with the speed of 15-25 DEG C/min, keep 3-8min, flow rate of carrier gas is 0.8-1.2mL/min.
Preferably, in order to improve series connection triple level Four bar Mass Spectrometer Method accuracy, the ion gun adopted in triple level Four bar Mass Spectrometer Method of connecting in step 2 and step 3 is electron impact ion source or chemical ionization source, and described ion source temperature is 230-260 DEG C, and electron energy is 65-75eV.
Preferably, in order to improve series connection triple level Four bar Mass Spectrometer Method accuracy and security, the carrier gas adopted in triple level Four bar Mass Spectrometer Method of connecting in step 2 and step 3 to be purity be 99% ~ 99.9999% helium, carrier gas control model is constant voltage mode, constant current mode or constant linear velocity pattern, and collision gas is the nitrogen of purity 99% ~ 99.999%.
Preferably, in order to protect filament, solvent delay 3-6min in triple level Four bar Mass Spectrometer Method of connecting in step 2 and step 3.
Preferably, in order to improve series connection triple level Four bar Mass Spectrometer Method accuracy, in triple level Four bar Mass Spectrometer Method of connecting in step 2 and step 3, detection mode is full scan, Selective ion mode scanning or multiion reaction monitoring, and triple level Four bar Mass Spectrometer Method intermediate-resolution of connecting in step 2 and step 3 adopts unit, wide or widest resolution.
Preferably, through corresponding parameter optimization, select 226.9---->184 and 226.9---->128 two pairs of ions as internal standard compound naphthalene-d 8monitoring ion; 226.9---->184 and 226.9---->128 two pairs of ions are selected to monitor ion as ESCALOL 567.
Solution-treated condition after optimizing in foundation the present invention and the setting of best chromatogram mass spectrometry parameters, ESCALOL 567 migration amount in dry food analogies can be accurately measured, strong interference immunity, quantitative result accuracy is high, reappearance is good, detectability can reach 0.05mg/kg, can meet the limitation requirement of 5.0mg/kg in European Union and Chinese GB9685.
Embodiment
In dry food analogies, an assay method for ESCALOL 567, comprises the following steps,
Step one, gets 1g dry food analogies in conical flask, adds 50mL and contains 0.5 μ g naphthalene-d 8methanol solution, in course of dissolution at 50 DEG C ultrasonic dissolution 30min, filter after the abundant rapid solution of solution, wash filter residue with methanol solution, merging filtrate, and concentrated be settled to 5.0mL, cross the organic filter membrane of 0.2um and obtain test fluid;
Step 2, carries out gas chromatography-triple level Four bar Mass Spectrometer Method of connecting to test fluid, gets the instrument of gained to naphthalene-d 8response signal is interior mark peak area A s, the instrument getting gained is test sample peak area A to ESCALOL 567 response signal;
Step 3, produces standard working solution, prepare one group with containing the naphthalene-d of 0.5 μ g 8internal standard compound and 0.5 μ g2-hydroxyl-4-methoxy benzophenone standard working solution, then carry out gas chromatography-triple level Four bar Mass Spectrometer Method of connecting to standard working solution, according to detecting the naphthalene-d obtained 8quantitative distance values peak area A iSand corresponding quality m i0.5 μ g, in conjunction with detecting the ESCALOL 567 quota ion peak area A obtained iand corresponding quality m i 0.5 μ g, then according to formulae discovery correction factor f; F=(A iS× 0.5)/(A i× 0.5)
Wherein, in gas chromatographic detection, chromatographic column coating is polyglycol, polystyrene or polymethyl siloxane material, and chromatogram column length is 30-60m, chromatographic column internal diameter is 0.18mm-0.25mm, coating thickness is 0.20-0.30 μm, and sample size is 0.5-2.0 μ L, the initial temperature 80-110 DEG C of gas chromatography, keep 0-4min, be warming up to 220-280 DEG C with the speed of 15-25 DEG C/min, keep 3-8min, flow rate of carrier gas is 0.8-1.2mL/min;
The ion gun adopted in triple level Four bar Mass Spectrometer Method of connecting is electron impact ion source or chemical ionization source, described ion source temperature is 230-260 DEG C, electron energy is 65-75eV, carrier gas to be purity be 99% ~ 99.9999% helium, carrier gas control model is constant voltage mode, constant current mode or constant linear velocity pattern, collision gas is the nitrogen of purity 99% ~ 99.999%, detection mode is full scan, Selective ion mode scanning or multiion reaction monitoring, solvent delay 3-6min, resolution adopts unit, wide or widest resolution;
Select 226.9---->184 and 226.9---->128 two pairs of ions as internal standard compound naphthalene-d 8monitoring ion; Select 226.9---->184 and 226.9---->128 two pairs of ions as the monitoring ion of ESCALOL 567;
Step 4, by the testing result A obtained in step 2 swith the sample quality m in A and step one and added internal standard compound quality m s0.5 μ g, the correction factor f obtained in integrating step three are then according to formula X=(A × m s× f)/(A s× m) calculate the content X of ESCALOL 567 in dry food analogies 1, wherein:
M sfor naphthalene-d in test fluid 8quality, 0.5 μ g,
M is the quality of dry food analogies, 1g,
X represents the content of ESCALOL 567 in dry food analogies, and unit is mg/kg.
Step 5, repeats step one and carries out parallel experiment to step 4, obtain replicate test result X 2, with the arithmetic mean of twice test result, i.e. X=(X 1+ X 2)/2 are as test result.
In the invention process process, collision energy is shown in as following table 1:
Table 1 naphthalene-d 8with the collision energy of ESCALOL 567
The present invention establishes the detection method of ESCALOL 567 migration amount in dry food analogies first, described measuring method is sample extracting solution direct injected after concentrated filter membrane, do not need to carry out the pre-treatment steps such as complicated derivatization, ESCALOL 567 migration amount in dry food analogies can be accurately measured, strong interference immunity, quantitative result accuracy is high, and reappearance is good.
Be below the preferred parameter in specific embodiments of the invention:
GC conditions:
1) chromatographic column: coating is polymethyl siloxane material, chromatogram column length is 30m; Chromatographic column internal diameter is 0.25mm; Coating thickness is: 0.25 μm;
2) sample size: 1.0 μ L;
3) temperature programme condition: initial temperature 100 DEG C, keeps 3min, is warming up to 280 DEG C with the speed of 15 DEG C/min, keeps 5min;
4) flow rate of carrier gas: 1.0mL/min.
Series connection triple quadrupole bar Mass Spectrometry Conditions:
1) ion gun: electronics bombardment (EI);
2) ion source temperature: 250 DEG C;
3) electron energy: 70eV;
4) carrier gas control model: constant current mode;
5) detection mode: the scanning of full scan (SCAN), Selective ion mode (SIM) or multiion reaction monitoring (MRM);
6) solvent delay: 4min;
7) carrier gas: purity is the helium of 99.9992%;
8) auxiliary heating temperature: 300 DEG C;
9) gas is collided: the nitrogen of purity 99.999%;
10) resolution: unit resolution;
11) collision energy is shown in as following table 2:
Table 2 naphthalene-d 8with the collision energy of ESCALOL 567
Additive process is adopted to detect precision and the recovery of this method:
Carry out sample pre-treatments by step of the present invention after to add ESCALOL 567 be respectively 0.05mg/kg, 0.50mg/kg, 5.00mg/kg tri-levels in not containing the dry food analogies of ESCALOL 567 and measure, repeat to add to each level and measure 6 times, and carry out the recovery and precision calculating, the recovery and Precision test result refer to table 3.
Table 32-hydroxyl-4-methoxy benzophenone TIANZHU XINGNAO Capsul and precision in dry food analogies
As can be seen from Table 3, the recovery of this method and precision good.The recovery that method measures all kinds of analogies is up to 89% ~ 98%; Precision is less than 8%, and accurately and reliably, precision is high for quantitative result.
As can be seen from above-described embodiment and accuracy test, the present invention establishes the detection method of ESCALOL 567 migration amount in dry food analogies first, described measuring method is sample extracting solution direct injected after concentrated filter membrane, does not need to carry out the pre-treatment steps such as complicated derivatization.In addition, according to optimizing rear Pretreatment in the present invention, and the setting of best chromatogram mass spectrometry parameters, ESCALOL 567 migration amount in dry food analogies can be accurately measured, strong interference immunity, quantitative result accuracy is high, and reappearance is good, detectability can reach 0.05mg/kg, can meet the limitation requirement of 5.0mg/kg in European Union and Chinese GB9685.
The foregoing is only the preferred embodiment of invention; not thereby the scope of the claims of the present invention is limited; every utilize description of the present invention to do equivalent structure or equivalent flow process conversion; or be directly or indirectly used in other relevant technical fields, be all in like manner included in scope of patent protection of the present invention.

Claims (10)

1. the assay method of ESCALOL 567 in dry food analogies, is characterized in that: comprise the following steps,
Step one, gets the dry food analogies that quality is m, adds containing known quality m snaphthalene-d 8solvent extraction filter after more concentrated constant volume obtain test fluid;
Step 2, carries out gas chromatography-triple level Four bar Mass Spectrometer Method of connecting to test fluid, gets the instrument of gained to naphthalene-d 8response signal is interior mark peak area A s, the instrument getting gained is test sample peak area A to ESCALOL 567 response signal;
Step 3, produces standard working solution, prepare one group with containing quality m inaphthalene-d 8the ESCALOL 567 standard working solution of internal standard compound, then carries out gas chromatography-triple level Four bar Mass Spectrometer Method of connecting to standard working solution, according to detecting the naphthalene-d obtained 8quantitative distance values peak area A iSand corresponding quality m i, in conjunction with detecting the ESCALOL 567 quota ion peak area A obtained iand corresponding quality m i, then according to formulae discovery correction factor f; F=(A iS× m i)/(A i× m i)
Step 4, by step 2 with obtained testing result A sand A, and sample quality m in step one and added interior mark quality m s, the correction factor f obtained in integrating step three is then according to formula X=(A × m s× f)/(A s× m) calculate the content X of ESCALOL 567 in dry food analogies 1, wherein:
X represents the content of ESCALOL 567 in dry food analogies, and unit is mg/kg.
Step 5, repeats step one and carries out parallel experiment to step 4, obtain replicate test result X 2, with the arithmetic mean of twice test result, i.e. X=(X 1+ X 2)/2 are as test result.
2. the assay method of ESCALOL 567 in a kind of dry food analogies according to claim 1, is characterized in that: in step one during solution dry food analogies, adopts containing naphthalene-d 8methanol solution dissolve, ultrasonic instrument 5-60min is opened in course of dissolution, temperature controls at 0-100 DEG C, after preliminarily solubilised filters, a dissolution filter operation is carried out again to filter residue, the solution that twice filtration obtains concentrates constant volume 1-10mL after merging again, and cross organic filter membrane, described organic filter sizes is 0.1 μm-0.45 μm.
3. the assay method of ESCALOL 567 in a kind of dry food analogies according to claim 1, is characterized in that: the permissible error of parallel experiment in step 5 is 20%.
4. the assay method of ESCALOL 567 in a kind of dry food analogies according to claim 1, is characterized in that: the standard working solution in step 3 by content be greater than 99.0% ESCALOL 567 standard items and content be greater than 99.0% naphthalene-d 8standard items and Chromatographic Pure Methanol dissolve constant volume to be made.
5. the assay method of ESCALOL 567 in a kind of dry food analogies according to claim 1, it is characterized in that: in step 2 and step 3, chromatographic column coating is polyglycol, polystyrene or polymethyl siloxane material, chromatogram column length is 30-60m, chromatographic column internal diameter is 0.18mm-0.25mm, coating thickness is 0.20-0.30 μm, sample size is 0.5-2.0 μ L, the initial temperature 80-110 DEG C of gas chromatography, keep 0-4min, 220-280 DEG C is warming up to the speed of 15-25 DEG C/min, keep 3-8min, flow rate of carrier gas is 0.8-1.2mL/min.
6. the assay method of ESCALOL 567 in a kind of dry food analogies according to claim 1 to 5 any one, it is characterized in that: the ion gun adopted in triple level Four bar Mass Spectrometer Method of connecting in step 2 and step 3 is electron impact ion source or chemical ionization source, described ion source temperature is 230-260 DEG C, and electron energy is 65-75eV.
7. the assay method of ESCALOL 567 in a kind of dry food analogies according to claim 6, it is characterized in that: the carrier gas adopted in triple level Four bar Mass Spectrometer Method of connecting in step 2 and step 3 to be purity be 99% ~ 99.9999% helium, carrier gas control model is constant voltage mode, constant current mode or constant linear velocity pattern, and collision gas is the nitrogen of purity 99% ~ 99.999%.
8. the assay method of ESCALOL 567 in a kind of dry food analogies according to claim 7, is characterized in that: solvent delay 3-6min in triple level Four bar Mass Spectrometer Method of connecting in step 2 and step 3.
9. the assay method of ESCALOL 567 in a kind of dry food analogies according to claim 8, it is characterized in that: in triple level Four bar Mass Spectrometer Method of connecting in step 2 and step 3, detection mode is full scan, Selective ion mode scanning or multiion reaction monitoring, triple level Four bar Mass Spectrometer Method intermediate-resolution of connecting in step 2 and step 3 adopts unit, wide or widest resolution.
10. the assay method of ESCALOL 567 in a kind of dry food analogies according to claim 9, is characterized in that: select 226.9---->184 and 226.9---->128 two pairs of ions as internal standard compound naphthalene-d 8monitoring ion; 226.9---->184 and 226.9---->128 two pairs of ions are selected to monitor ion as ESCALOL 567.
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