CN101493440A - Method for measuring migration volume of phthalic ester and di(2-ethylhexyl) adipate in fatty foodstuff contact material - Google Patents
Method for measuring migration volume of phthalic ester and di(2-ethylhexyl) adipate in fatty foodstuff contact material Download PDFInfo
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Abstract
The invention belongs to the field of analytical chemistry and relates to the measurement for the transferring amount of phthalate and ethylhexyl adipate in fatty food contact materials, in particular to the use of an adsorbent chromatography colume for purifying and separating the phthalate and ethylhexyl adipate in fatty food simulant liquid, and the use of a combined gas chromatography mass spectrometry for measuring the content thereof. The pre-treatment method which is provided by the invention for the purification and separation of the adsorbent chromatography colume has the advantages of rapidity, strong selection property, small pollution, and low detection limit. The invention can achieve the measurement for the transferring amount of phthalate and ethylhexyl adipate in fatty food contact materials.
Description
Technical field
The invention belongs to the analytical chemistry field, relate to the migration amount that combined gas chromatography mass spectrometry is measured phthalic ester and hexane diacid ethylhexyl in the food contact material.Be specifically related to phthalic ester and hexane diacid ethylhexyl in the adsorbent chromatography column purification fractionation of fatty food simulated solution, combined gas chromatography mass spectrometry is measured its content.
Background technology
Phthalic ester and hexane diacid ethylhexyl are widely used plastifier, also are widely used in plastic product so far, and toxicological experiment proves that this compounds has estrogenic effect, so need the use of this compounds of monitoring.
Because plastics are used for and the container of Food Contact and packing in a large number, the method for taking to represent the food simulated solution of food quality to soak to the quality control of food contact material is carried out the compound migration and is tested.
Gui Ding food simulated solution is four kinds in the world, represents neutral food respectively, acid food, and spirituosity food and fatty foodstuff, corresponding simulating liquid are water, acetic acid solution, ethanolic solution and edible vegetable oil.Measure the migration amount of phthalic ester and hexane diacid ethylhexyl in the food contact material, actual specimen is a water, acetic acid solution, and therefore ethanolic solution and edible vegetable oil must carry out the method for purification separation at four kinds of simulated solutions.The method that can test the solution of different substrates simultaneously in the document yet there are no report, and in the use grease test of phthalic ester and hexane diacid ethylhexyl especially since the polarity of determinand and grease near being difficult to isolation of purified, therefore the detectability of test can't reduce.The method of phthalic ester and hexane diacid ethylhexyl is quick in the column chromatography purification extraction grease provided by the invention, and recovery height does not pollute instrument, and has effectively reduced detection limit.
Summary of the invention
The invention provides a kind of chromatographic column purification separation combined gas chromatography mass spectrometry and measure the migration amount of phthalic ester and hexane diacid ethylhexyl in the fatty foodstuff contact material.
The present invention adopts phthalic ester and hexane diacid ethylhexyl in the adsorbent chromatography post isolation of purified fatty foodstuff simulated solution, and combined gas chromatography mass spectrometry is measured its content.
Particular content of the present invention is:
1. adsorbent and chromatographic column are prepared
(1) adsorbent: 190 ℃-650 ℃ following baking 5h-8h, place the exsiccator cooling after, every 100g adsorbent adds the deactivation of 2mL-4mL deionized water, and is stored in the exsiccator standby.
(2) chromatographic column post loading method
In glass chromatography column, load the anhydrous sodium sulfate of 1cm-1.5cm earlier, get the 15g-20g adsorbent in the 100mL beaker, add the sherwood oil diethyl ether solution, adopt wet method dress post method to load chromatographic column, highly be 10cm-15cm, the last anhydrous sodium sulfate of inserting about 1cm-1.5cm on the upper strata.
2. the preparation of analyzing liquid sample:
(1) takes by weighing 1g-3g fatty foodstuff simulated solution in the 150mL beaker, add 10mL-30mL sherwood oil ether, shake up;
(2) sample liquid is added in the chromatographic column, draws an amount of sherwood oil ether and clean beaker, cleansing solution adds chromatographic column, discards outflow solution.
(3) use 40mL-60mL sherwood oil ether drip washing chromatographic column at twice, discard leacheate.
Add 100mL-150mL sherwood oil ether drip washing chromatographic column; Add 50mL-100mL ether drip washing chromatographic column again, merge and collect eluent in flat bottom flask; Eluent concentrates the back and is settled to 5mL with normal hexane, and is standby.
3. combined gas chromatography mass spectrometry is measured:
Advancing bar mouth temperature can be 200 ℃-300 ℃, and temperature programme can be to press expression:
80 ℃ of initial temperature are warmed up to 170 ℃ by 40 ℃ of per minutes, are warmed up to 270 ℃ by 10 ℃ of per minutes again.
The mass spectrum collection can be adopted full scan mode (Scan pattern), also can adopt and select ionic means (SIM pattern).
Embodiment
Embodiment one: the mensuration of butyl phthalate and di (2-ethylhexyl) phthalate in the olive oil
1. adsorbent and chromatographic column are prepared
(1) silica gel: after 300 ℃ of baking 5h placed the exsiccator cooling, every 100g silica gel added the deactivation of 2mL deionized water, and is stored in the exsiccator standby.
(2) chromatographic column post loading method
Loading the 1cm anhydrous sodium sulfate earlier in glass chromatography column, get 20g silica gel in the 100mL beaker, add the sherwood oil diethyl ether solution, adopt wet method dress post method to load chromatographic column, highly is 15cm, inserts about 1cm anhydrous sodium sulfate at last on the upper strata.
2. the preparation of sample liquid
(1) takes by weighing the 2g olive oil in the 150mL beaker, add 20mL sherwood oil ether, shake up;
(2) sample liquid is added in the chromatographic column, draws 5mL sherwood oil ether and clean beaker;
(3) with 60mL sherwood oil ether drip washing chromatographic column;
(4) add 100mL sherwood oil ether drip washing chromatographic column again;
(5) add 60 ether drip washing chromatographic columns again;
(6) eluent concentrates near doing, and normal hexane is settled to 5mL, and is standby.
3. setting instrument parameter
(1) gas chromatograph condition
Gas chromatograph: Agilent 6890
Chromatographic column: HP-5MS capillary column 0.25mm * 30m * 0.25 μ m
Injector temperature: 270 ℃
Transmission line temperature: 270 ℃
Flow rate of carrier gas: 1.0mL/min, constant current
Sample introduction pattern: split sampling not
Sampling volume: 1 μ L
Temperature programme: 80 ℃ of initial temperature, be warmed up to 170 ℃ by 40 ℃ of per minutes, be warmed up to 270 ℃ by 10 ℃ of per minutes again.
(2) mass spectrum condition
Solvent delay: 5min
Acquisition mode: Scan pattern
Samplo?Rato：2
Ion source temperature: 230 ℃
Quadrupole rod temperature: 150 ℃
4. qualitative and quantitative
(1) qualitative
Retention time through sample peak and standard items peak is compared, and the comparison of comparing of sample peak mass spectrogram and standard substance mass spectrogram determines whether detect determinand in the sample.
(2) quantitative
Adopt the typical curve external standard method quantitative:
The butyl phthalate quota ion is 149, and qualitative ion is 223,205.
Phthalic acid diethylhexyl quota ion is 149, and qualitative ion is 167,279.
Embodiment two: the mensuration of phthalic acid ester in the different ninth of the ten Heavenly Stems and the different certain herbaceous plants with big flowers ester of phthalic acid in the peanut oil
1. adsorbent and chromatographic column are prepared
(1) silica gel: after 300 ℃ of baking 5h placed the exsiccator cooling, every 100g silica gel added the deactivation of 2mL deionized water, and is stored in the exsiccator standby.
(2) chromatographic column post loading method
Loading the 1cm anhydrous sodium sulfate earlier in glass chromatography column, get 20g silica gel in the 100mL beaker, add the sherwood oil diethyl ether solution, adopt wet method dress post method to load chromatographic column, highly is 15cm, inserts about 1cm anhydrous sodium sulfate at last on the upper strata.
2. the preparation of sample liquid
(1) takes by weighing 2g peanut oil in the 150mL beaker, add 20mL sherwood oil ether, shake up;
(2) sample liquid is added in the chromatographic column, draws 5mL sherwood oil ether and clean beaker;
(3) use 60mL sherwood oil ether drip washing chromatographic column at twice;
(4) add 100mL sherwood oil ether drip washing chromatographic column again;
(5) add 60mL ether drip washing chromatographic column again;
(6) eluent concentrates near doing, and normal hexane is settled to 5mL, and is standby.
3. setting instrument parameter
(1) gas chromatograph condition
Gas chromatograph: Agilent 6890
Chromatographic column: HP-5MS capillary column 0.25mm * 30m * 0.25 μ m
Injector temperature: 290 ℃
Transmission line temperature: 290 ℃
Flow rate of carrier gas: 1.0mL/min, constant current
Sample introduction pattern: split sampling not
Sampling volume: 1 μ L
Temperature programme: 80 ℃ of initial temperature, be warmed up to 170 ℃ by 40 ℃ of per minutes, be warmed up to 290 ℃ by 10 ℃ of per minutes again.
(2) mass spectrum condition
Solvent delay: 5min
Acquisition mode: Scan pattern
Sample?Rate：2
Ion source temperature: 230 ℃
Quadrupole rod temperature: 150 ℃
4. qualitative and quantitative
(1) qualitative
Retention time through sample peak and standard items peak is compared, and the comparison of comparing of sample peak mass spectrogram and standard substance mass spectrogram determines whether detect determinand in the sample.
(2) quantitative
Adopt the typical curve external standard method quantitative:
Phthalic acid ester quota ion in the different ninth of the ten Heavenly Stems is 293, and qualitative ion is 149.
The different certain herbaceous plants with big flowers ester of phthalic acid quota ion is 307, and qualitative ion is 149.
Embodiment three: the mensuration of O-phthalic allyl propionate in the rapeseed oil
1. adsorbent and chromatographic column are prepared
(1) silica gel: after 300 ℃ of baking 5h placed the exsiccator cooling, every 100g silica gel added the deactivation of 2mL deionized water, and is stored in the exsiccator standby.
(2) chromatographic column post loading method;
Loading the 1cm anhydrous sodium sulfate earlier in glass chromatography column, get 20g silica gel in the 100mL beaker, add the sherwood oil diethyl ether solution, adopt wet method dress post method to load chromatographic column, highly is 15cm, inserts about 1cm anhydrous sodium sulfate at last on the upper strata.
2. the preparation of sample liquid:
(1) takes by weighing the 1g rapeseed oil in the 150mL beaker, add 10mL sherwood oil ether, shake up;
(2) sample liquid is added in the chromatographic column, draws 5mL sherwood oil ether and clean beaker;
(3) use 60mL sherwood oil ether drip washing chromatographic column at twice;
(4) add 100mL sherwood oil ether drip washing chromatographic column again;
(5) add 60mL ether drip washing chromatographic column again;
(6) eluent concentrates near doing, and normal hexane is settled to 5mL, and is standby.
3. setting instrument parameter
(1) gas chromatograph condition
Gas chromatograph: Agilent 6890
Chromatographic column: HP-5MS capillary column 0.25mm * 30m * 0.25 μ m
Injector temperature: 280 ℃
Transmission line temperature: 280 ℃
Flow rate of carrier gas: 1.0mL/min, constant current
Sample introduction pattern: split sampling not
Sampling volume: 1 μ L
Temperature programme: 80 ℃ of initial temperature, be warmed up to 170 ℃ by 40 ℃ of per minutes, be warmed up to 280 ℃ by 10 ℃ of per minutes again.
(2) mass spectrum condition
Solvent delay: 5min
Acquisition mode: the SIM pattern, gathering ion is 149,189,132
Ion source temperature: 230 ℃
Quadrupole rod temperature: 150 ℃
4. qualitative and quantitative
(1) qualitative
Retention time through sample peak and standard items peak is compared, and sample peak mass spectrogram and standard substance mass spectrogram are compared, and determines whether detect determinand in the sample.
(2) quantitative
Adopt the typical curve external standard method quantitative:
O-phthalic allyl propionate quota ion is 147, and qualitative ion is 132,189.
Embodiment four: the mensuration of O-phthalic allyl propionate in the sunflower oil
1. adsorbent and chromatographic column are prepared
(1) florisil silica: after 650 ℃ of baking 5h placed the exsiccator cooling, every 100g florisil silica added the deactivation of 2mL deionized water, and is stored in the exsiccator standby.
(2) chromatographic column post loading method
Loading the 1cm anhydrous sodium sulfate earlier in glass chromatography column, get the 20g florisil silica in the 100mL beaker, add the sherwood oil diethyl ether solution, adopt wet method dress post method to load chromatographic column, highly is 15cm, inserts about 1cm anhydrous sodium sulfate at last on the upper strata.
2. the preparation of sample liquid:
(1) takes by weighing the 1g sunflower oil in the 150mL beaker, add 10mL sherwood oil ether, shake up;
(2) sample liquid is added in the chromatographic column, draws 5mL sherwood oil ether and clean beaker;
(3) use 60mL sherwood oil ether drip washing chromatographic column at twice;
(4) add 100mL sherwood oil ether drip washing chromatographic column again;
(5) add 60mL ether drip washing chromatographic column again;
(6) eluent concentrates near doing, and normal hexane is settled to 5mL, and is standby.
3. setting instrument parameter
(1) gas chromatograph condition
Gas chromatograph: Agilent 6890
Chromatographic column: HP-5MS capillary column 0.25mm * 30m * 0.25 μ m
Injector temperature: 280 ℃
Transmission line temperature: 280 ℃
Flow rate of carrier gas: 1.0mL/min, constant current
Sample introduction pattern: split sampling not
Sampling volume: 1 μ L
Temperature programme: 80 ℃ of initial temperature, be warmed up to 170 ℃ by 40 ℃ of per minutes, be warmed up to 280 ℃ by 10 ℃ of per minutes again.
(2) mass spectrum condition
Solvent delay: 5min
Acquisition mode: the SIM pattern, gathering ion is 149,189,132
Ion source temperature: 230 ℃
Quadrupole rod temperature: 150 ℃
4. qualitative and quantitative
(1) qualitative
Retention time through sample peak and standard items peak is compared, and sample peak mass spectrogram and standard substance mass spectrogram are compared, and determines whether detect determinand in the sample.
(2) quantitative
Adopt the typical curve external standard method quantitative:
O-phthalic allyl propionate quota ion is 147, and qualitative ion is 132,189.
Embodiment five: the mensuration of O-phthalic allyl propionate in the corn oil
1. adsorbent and chromatographic column are prepared
(1) aluminium oxide: after 190 ℃ of baking 5h placed the exsiccator cooling, every 100g aluminium oxide added the deactivation of 2mL deionized water, and is stored in the exsiccator standby.
(2) chromatographic column post loading method
Loading the 1cm anhydrous sodium sulfate earlier in glass chromatography column, get the 20g aluminium oxide in the 100mL beaker, add the sherwood oil diethyl ether solution, adopt wet method dress post method to load chromatographic column, highly is 15cm, inserts about 1cm anhydrous sodium sulfate at last on the upper strata.
2. the preparation of sample liquid
(1) takes by weighing 1g corn oil in the 150mL beaker, add 10mL sherwood oil ether, shake up;
(2) sample liquid is added in the chromatographic column, draws 5mL sherwood oil ether and clean beaker;
(3) use 60mL sherwood oil ether drip washing chromatographic column at twice;
(4) add 100mL sherwood oil ether drip washing chromatographic column again;
(5) add 60mL ether drip washing chromatographic column again;
(6) eluent concentrates near doing, and normal hexane is settled to 5mL, and is standby.
3. setting instrument parameter
(1) gas chromatograph condition
Gas chromatograph: Agilent 6890
Chromatographic column: HP-5MS capillary column 0.25mm * 30m * 0.25 μ m
Injector temperature: 280 ℃
Transmission line temperature: 280 ℃
Flow rate of carrier gas: 1.0mL/min, constant current
Sample introduction pattern: split sampling not
Sampling volume: 1 μ L
Temperature programme: 80 ℃ of initial temperature, be warmed up to 170 ℃ by 40 ℃ of per minutes, be warmed up to 280 ℃ by 10 ℃ of per minutes again.
(2) mass spectrum condition
Solvent delay: 5min
Acquisition mode: the SIM pattern, gathering ion is 149,189,132
Ion source temperature: 230 ℃
Quadrupole rod temperature: 150 ℃
4. qualitative and quantitative
(1) qualitative
Retention time through sample peak and standard items peak is compared, and sample peak mass spectrogram and standard substance mass spectrogram are compared, and determines whether detect determinand in the sample.
(2) quantitative
Adopt the typical curve external standard method quantitative:
O-phthalic allyl propionate quota ion is 147, and qualitative ion is 132,189.
Claims (10)
1. method of measuring the migration amount of phthalic ester and hexane diacid ethylhexyl in the fatty foodstuff contact material, it is characterized in that: with phthalic ester and hexane diacid ethylhexyl in the adsorbent chromatography column purification fractionation of fatty food simulated solution, combined gas chromatography mass spectrometry is measured its content, wherein
(1) phthalic ester and hexane diacid ethylhexyl may further comprise the steps in the said adsorbent chromatography column purification fractionation of fatty food simulated solution:
A. adsorbent and chromatographic column are prepared
A. adsorbent is in 190 ℃-650 ℃ following baking 5h-8h, place the exsiccator cooling after, every 100g adsorbent adds the deactivation of 2mL-4mL deionized water, and is stored in the exsiccator standby;
B. chromatographic column post loading method
In glass chromatography column, load the anhydrous sodium sulfate of 1cm-1.5cm earlier, get the 15g-20g adsorbent in the 100mL beaker, add the sherwood oil diethyl ether solution, adopt wet method dress post method to load chromatographic column, highly be 10cm-15cm, the last anhydrous sodium sulfate of inserting 1cm-1.5cm on the upper strata;
B. the preparation of analyzing liquid sample
A. take by weighing 1g-3g fatty foodstuff simulated solution in the 150mL beaker, add 10mL-30mL sherwood oil ether, shake up;
B. sample liquid is added in the chromatographic column, draws the sherwood oil ether and clean beaker, cleansing solution adds chromatographic column, discards outflow solution;
C. use 40mL-60mL sherwood oil ether drip washing chromatographic column at twice, discard leacheate; Add 100mL-150mL sherwood oil ether drip washing chromatographic column, add 50mL-100mL ether drip washing chromatographic column again, merge and collect eluent in flat bottom flask; Eluent concentrates the back and is settled to 5mL with normal hexane, and is standby;
(2) gas chromatography combined with mass spectrometry determination and analysis sample liquid
A. the gas chromatography injector temperature is set at 200 ℃-300 ℃, and temperature programme is 80 ℃ of initial temperature, is warmed up to 170 ℃ by 40 ℃ of per minutes, is warmed up to 200 ℃-300 ℃ by 10 ℃ of per minutes again, sample introduction;
B. the full scan mode is adopted in the mass spectrum collection.
2. the method for claim 1 is characterized in that the fatty foodstuff simulated solution is an olive oil, rapeseed oil, the triglyceride of synthetic.
3. method according to claim 1 is characterized in that the fatty foodstuff simulated solution is edible oil and fat.
4. method according to claim 1, it is characterized in that phthalic ester is a Methyl Benzene-o-dicarboxylate, ethyl phthalate, butyl phthalate, the phthalic acid isobutyl ester, the phthalic acid pentyl ester, the own ester of phthalic acid, di (2-ethylhexyl) phthalate, octyl phthalate, phthalic acid ester in the different ninth of the ten Heavenly Stems, the different certain herbaceous plants with big flowers ester of phthalic acid, O-phthalic allyl propionate.
5. method according to claim 1 is characterized in that adsorbent is a silica gel.
6. method according to claim 1 is characterized in that adsorbent is a florisil silica, aluminium oxide, chromatography C18.
7. method according to claim 1 is characterized in that in glass chromatography column the anhydrous sodium sulfate of filling 1cm earlier, the last anhydrous sodium sulfate of inserting 1cm on the glass chromatography column upper strata.
8. method according to claim 1 is characterized in that the sherwood oil diethyl ether solution is that volume ratio is 5: 1-1: 1.
9. method according to claim 1 is characterized in that mass spectrum collection employing selection ionic means.
10. edible oil and fat according to claim 3 is characterized in that edible oil and fat are peanut oil, corn oil, sunflower oil.
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| CN104535666A (en) * | 2015-02-11 | 2015-04-22 | 浙江中烟工业有限责任公司 | A method of measuring migration amounts of eighteen phthalic acid esters in a conveyor belt by adopting a gas chromatography-mass spectrometry instrument |
| CN104535666B (en) * | 2015-02-11 | 2016-01-27 | 浙江中烟工业有限责任公司 | A kind of method adopting gas chromatograph-mass spectrometer (GCMS) to measure 18 kinds of phthalic ester migration amounts in travelling belt |
| CN104833734A (en) * | 2015-03-30 | 2015-08-12 | 上海安谱实验科技股份有限公司 | Method for detection of transfer volume of phthalic acid ester matters in food package material |
| CN105004818A (en) * | 2015-07-29 | 2015-10-28 | 齐国良 | Detection method for plasticizers in foods containing oils and fats |
| CN112305110A (en) * | 2020-10-26 | 2021-02-02 | 舟山新诺佳生物工程有限责任公司 | Detection method suitable for ethyl ester type and glyceride type fish oil product plasticizers |
| CN112305110B (en) * | 2020-10-26 | 2022-08-12 | 舟山新诺佳生物工程有限责任公司 | Detection method suitable for ethyl ester type and glyceride type fish oil product plasticizers |
| CN112730662A (en) * | 2020-12-22 | 2021-04-30 | 中华人民共和国乌鲁木齐海关 | Method for simultaneously determining phthalate and adipate plasticizers in textile solid waste |
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