CN103235051A - Method for determining colorant solvent green 7 in dry food packaging paper - Google Patents
Method for determining colorant solvent green 7 in dry food packaging paper Download PDFInfo
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Abstract
The invention discloses a method for determining a colorant solvent green 7 in dry food packaging paper. The method comprises: standard working solution preparation, sample solution preparation, high performance liquid chromatography analysis, standard curve drawing and result calculation. According to the present invention, reversed phase ion pair high performance liquid chromatography is firstly adopted to determine a colorant solvent green 7 in dry food packaging paper, operation is simple and accurate, the target object and other impurity chromatographic peaks brought by the sample matrix can be well separated with the used chromatographic conditions, good linear correlation is provided, a detection limit is 0.96 mg/kg, an average relative standard deviation is 2.96%, a standard addition recovery rate is 83.90-106.25%, characteristics of rapidness, accuracy, high sensitivity, good repeatability, high recovery rate and the like are provided, and interference caused by the matrix can be avoided; and the method is especially suitable for determination of the colorant solvent green 7 content in dry food packaging paper.
Description
Technical field
The invention belongs to wrappage physical and chemical index detection technique field, be specifically related to the method for colorant solvent green 7 in a kind of mensuration dry food wrapping paper (mainly comprising fast food wrapping paper, candy paper, face edible paper etc.).
Background technology
The green 7(Solvent Green 7 of solvent), claim 8-hydroxyl-1,3 again, 6-pyrene trisulfonic acid trisodium is a kind of artificial synthetic sulfonic acid class dyestuff, be mainly used in painting, plastic products etc. painted, can also be used for e-Pointer, the tracer agent of Industrial Boiler etc.In view of long-term or excessive this type of material of use, can produce potential harm to health, if any colorant can cause people's allergic reaction, the colorant that has can cause organ irritation such as eyes, oral cavity, the colorant that also has can see through skin and be absorbed by the body, tangible mutagenesis is arranged, use this series products for a long time even can bring out cancer.Based on above-mentioned reason, numerous and confused legislation such as many countries such as the U.S., Japan and European Union is limited the consumption of colorant in the world.China's " hygienic standards for cosmetics " also lists solvent green 7 in the scope of temporary colorant.The molecular structural formula of solvent green 7 is as follows.
The dry food wrapping paper is important component part indispensable in the packaging for foodstuff, and its security is the very important aspect of food overall security, and the source of packaging material for food security control is raw materials for production at all.In view of solvent green 7 very likely can be used to as colorant in the production run of paper as raw materials for production.Therefore exploring a kind of detection method of solvent fast and accurately green 7, the colorant in the dry food wrapping paper is control effectively, ensure the safety in utilization of dry food wrapping paper, is very urgent and necessary.
Analysis and research report about solvent green 7 mainly concentrates on the cosmetics aspect.The analytical approach that adopts is liquid phase chromatography.People such as Sun Xiaoying, Li Ying uses the C18 reverse-phase chromatographic column respectively, be the phase that flows with acetonitrile-potassium dihydrogen phosphate buffer solution, detect with the scanning of DAD detecting device, carry out qualitative analysis with retention time in conjunction with the ultra-violet absorption spectrum of determinand, adopt external standard method to carry out quantitative test, set up the detection method of the solvent in the cosmetics green 7.But actual effect checking shows that the object appearance time is short in this method, and during actual detected, with other material in the sample very serious overlapping phenomenon is arranged, and separating effect is relatively poor.In fact, the chromatogram column length that this method adopts is 250mm, and the appearance time of solvent green 7 is more at 2min, can infer solvent green 7 basic not reservation on chromatographic column.Therefore, this method and be not suitable for solvent green 7 is detected analysis.
Summary of the invention
Goal of the invention: at the deficiencies in the prior art, the purpose of this invention is to provide a kind of method of measuring colorant solvent green 7 in the dry food wrapping paper, this method adopts reversed phase ion that high performance liquid chromatography (use diode array detector) is measured colorant solvent green 7 in the dry food wrapping paper, can fast, accurately detect the content of colorant solvent green 7 in the dry food wrapping paper, have characteristics such as the result is accurate, interference is few.
Technical scheme: in order to realize the foregoing invention purpose, the technical solution used in the present invention is as follows:
A kind of method of measuring colorant solvent green 7 in the dry food wrapping paper may further comprise the steps:
(1) preparation of standard operation solution: be standard items with solvent green 7, use water as solvent, be configured to standard operation solution through stepwise dilution;
(2) preparation of sample solution: accurately take by weighing a certain amount of dry food wrapping paper sample, shred, with the ultrasonic extraction of certain amount of solvent, extract is crossed the water filter membrane, get sample solution;
(3) efficient liquid phase chromatographic analysis: standard operation solution and sample solution are detected analysis with having diode array detector high performance liquid chromatograph (HPLC);
(4) typical curve is drawn and result's calculating.
In the step (1), the standard operation solution concentration is respectively 0.1～0.3mg/L, 0.5～1.5mg/L, 1.0～3.0mg/L, 5～15mg/L and 10～30mg/L, concrete preparation process is: accurately take by weighing 0.1～0.3g reference material solvent green 7, earlier with aqueous dispersion, dissolving, water is settled in the volumetric flask of 100mL again, obtains the standard reserving solution that concentration is 1000～3000mg/L.Accurately pipette 10 μ L, 25 μ L, 50 μ L, 250 μ L and 500 μ L standard reserving solutions more respectively, water is cooked in the volumetric flask that solvent is settled to 100mL.
In the step (2), the preparation of described sample solution, specifically may further comprise the steps: take by weighing 0.5g sample (being accurate to 0.1 mg), it is cut into the following fragment of 5mm * 5mm, place 50mL tool plug triangular flask, accurately pipette 10mL extraction solvent water, ultrasonic extraction 20min gets an amount of extract centrifugal 5min in centrifuge tube, gets supernatant liquor, behind 0.45 μ m water membrane filtration, obtain sample solution.
In the step (3), the liquid-phase chromatographic analysis condition is: chromatographic column is the C18 chromatographic column, and specification is 150mm(length) * the 4.6mm(internal diameter) * 5.0 μ m(filler granularities); Column temperature is 30 ℃; Flow velocity is 1.0mL/min; Sample size is 10 μ L; Mobile phase A is methyl alcohol, and Mobile phase B is that (wherein ion-pairing agent is tetrabutyl ammonium hydrogen phosphate to ion-pairing agent solution, or the TBAH aqueous solution, and its concentration is 5 mmol/L～15 mmol/L.), adopt isocratic elution (wherein volume ratio V/V is 45%/55%～55%/45%); The detection wavelength of DAD detecting device is 246nm; Be about 10 min analysis time.
In the step (4), described typical curve is drawn and the result is calculated as follows: the concentration with solvent in the working solution green 7 is horizontal ordinate, is ordinate with the peak area of green 7 ion-pair compounds of solvent in the chromatogram, carries out regretional analysis, obtains typical curve; With the chromatographic peak area of green 7 ion-pair compounds of solvent in the sample solution that records under the same terms, the substitution working curve converts and tries to achieve the content of solvent green 7 in the sample.
Beneficial effect: compared with prior art, the method of colorant solvent green 7 in the mensuration dry food wrapping paper of the present invention, extraction obtains colorant 7 from the dry food wrapping paper earlier, recycling itself and ion-pairing agent form ion-pair compound, thereby can utilize the DAD detecting device that it is carried out qualitative affirmation and quantitatively detect.This method has proposed the employing reversed phase ion first colorant solvent green 7 in the high-performance liquid chromatogram determination dry food wrapping paper has been measured, have fast, accurately, characteristics such as sensitivity height, and can evade the interference that matrix is brought, be particularly suitable for measuring the content of colorant solvent green 7 in the dry food wrapping paper.
Description of drawings
Fig. 1 is the chromatogram of standard operation solution;
Fig. 2 is the chromatogram of typical sample;
Fig. 3 is the chromatogram of typical mark-on sample;
Fig. 4 is the spectrogram of green 7 ion-pair compounds of solvent.
Embodiment
Below in conjunction with specific embodiment the present invention is done further explanation.
A kind of method of measuring colorant solvent green 7 in the dry food wrapping paper, detailed process is as follows:
(1) preparation of standard operation solution
It is green 7 accurately to take by weighing 0.2g reference material solvent, earlier with low amounts of water disperse, dissolving, water is settled in the volumetric flask of 100mL again, obtains the standard reserving solution that concentration is 2000mg/L.Accurately pipette 10 μ L, 25 μ L, 50 μ L, 250 μ L and 500 μ L standard reserving solutions more respectively, water is settled in the volumetric flask of 100mL.This series standard working solution concentration is respectively 0.2mg/L, 0.5mg/L, 1.0mg/L, 5.0mg/L and 10mg/L.Standard operation solution needs matching while using.
(2) preparation of sample solution
Take by weighing 0.5g sample (being accurate to 0.1mg), it is cut into the following fragment of 5mm * 5mm, place 50mL tool plug triangular flask, accurately pipette 10mL extraction solvent water, ultrasonic extraction 20min gets an amount of extract centrifugal 5min in centrifuge tube, gets supernatant liquor, behind 0.45 μ m water membrane filtration, obtain sample solution.
(3) efficient liquid phase chromatographic analysis
The working stamndard solution of extracting sample solution, mark-on sample solution, 5 variable concentrations carries out liquid chromatography respectively, the chromatogram of standard operation solution as shown in Figure 1, the chromatogram of sample solution as shown in Figure 2, the chromatogram of mark-on sample is as shown in Figure 3.Chromatographiccondition is: chromatographic column is the C18 chromatographic column, and specification is 150mm(length) * the 4.6mm(internal diameter) * 5.0 μ m(filler granularities); Column temperature is 30 ℃; Flow velocity is 1.0mL/min; Sample size is 10 μ L; Mobile phase A is methyl alcohol, and Mobile phase B is that concentration is the tetrabutyl ammonium hydrogen phosphate solution of 10mmol/L, adopts isocratic elution, and wherein volume ratio V/V is 50%/50%; The detection wavelength of DAD detecting device is 246nm; Be about 10min analysis time.
(4) typical curve is drawn and result's calculating
At first the concentration with solvent in the standard operation solution green 7 is horizontal ordinate, peak area with solvent in the chromatogram green 7 is ordinate, carry out regretional analysis, obtain typical curve, get the standard operation solution of least concentration, doing 10 parallel detection analyses, calculate its standard deviation, is detection limit with the concentration of 3 times standard deviation correspondences.Data such as the regression equation corresponding with standard working curve, related coefficient are specially:
The regression equation Y=18.446X-0.7952 that green 7 standard working curves of solvent are corresponding, related coefficient 0.99999, the range of linearity 0.2～10mg/L, detection limit 0.96 mg/kg.
Then with the chromatographic peak area of solvent in the sample solution that records under the same terms green 7, the substitution working curve is tried to achieve the content of solvent green 7 in the sample, and computing formula is as follows:
In the formula: X is the content of solvent green 7 in the sample, mg/kg; C is the concentration by solvent in the sample solution that reads on the standard working curve green 7, mg/L; C
0Be the concentration by solvent in the blank solution that reads on the standard working curve green 7, mg/L; 524 is the molecular weight of solvent green 7; V is the volume of extraction system, mL; M is the quality of sample, g; 1181 is the molecular weight of green 7 ion-pair compounds of solvent.
(5) sample determination
Adopt said method, 30 dry food wrapping paper samples choosing (comprise fast food wrapping paper, candy with paper, face edible paper etc.) are detected, all do not detect solvent green 7.In addition, be determination object (measured value is not for detecting) with a candy paper, adding concentration to it is the standard specimen of 80.0 mg/kg, and the fructufy measured value is 78.93mg/kg, and relative deviation is 0.67%, and the accuracy of visible measurement result is better.
Qualitative confirmation method to object solvent green 7 must meet following two conditions: 1. the retention time with the standard model chromatogram contrasts, and the retention time of sample chromatogram figure is ± 2.5% permissible error; 2. the spectrogram with standard model contrasts (following is its spectrogram, as can be seen from Figure 4, at wavelength 246nm place stronger uv absorption is arranged, and is 246nm admittedly select analytical wavelengths for use), and the spectrogram of sample must be consistent.
The detection of embodiment 3 precision and the recovery
Present embodiment is as follows to the detection method of precision of the present invention and recovery of standard addition:
The detection of precision: be object (measured value is not for detecting) with the pattern product with a candy, the content of (the mark-on level is 80mg/kg) solvent green 7 in its mark-on sample of 6 replicate determinations, calculate relative standard deviation, the precision of investigation method, the result is as shown in table 1.The good reproducibility of this method has been described.
The precision of table 1 method (n=6)
| Sequence number | Measured value (mg/kg) |
| 1 | 82.64 |
| 2 | 82.92 |
| 3 | 83.08 |
| 4 | 82.31 |
| 5 | 82.51 |
| 6 | 82.08 |
| Relative standard deviation (%) | 2.96 |
Choose 2 kinds of representational samples (fast food wrapping paper and candy paper) as the mark-on sample substrate, mark-on samples low, high 3 concentration levels of neutralization have been made respectively, the result is as shown in table 2, the recovery of fast food wrapping paper is 85.06～106.25%, candy is 83.90～101.75% with the recovery of paper, and the recovery height of this method has been described.
The recovery of standard addition of table 2 solvent green 7
Mark liquid and standard solution were that example describes with one of them concentration only in present embodiment was used, interior mark liquid and standard solution that other concentration value disposes are same as the previously described embodiments through typical curve and regression equation that chromatograph mass spectrum analysis obtains, are not enumerating one by one at this.Illustrated embodiment is method for a better understanding of the present invention just, does not have any restriction, and namely said method or the method that is equal to above-mentioned situation all are included in the protection domain of technical scheme of the present invention.
Claims (6)
1. a method of measuring colorant solvent green 7 in the dry food wrapping paper is characterized in that, may further comprise the steps:
(1) is standard items with solvent green 7, uses water as solvent, be configured to standard operation solution through stepwise dilution;
(2) take by weighing quantitative dry food wrapping paper sample, pulverize, the water filter membrane is crossed in the ultrasonic extraction of water, gets sample solution;
(3) with having the diode array detector high performance liquid chromatograph standard operation solution and sample solution are detected analysis;
(4) typical curve is drawn and result's calculating.
2. the method for colorant solvent green 7 in the mensuration dry food wrapping paper according to claim 1 is characterized in that in the step (1), the preparation of standard operation solution specifically may further comprise the steps:
(1) standard reserving solution: it is green 7 accurately to take by weighing 0.1～0.3g reference material solvent, and with aqueous dispersion, dissolving, water is settled in the volumetric flask of 100mL again, obtains the standard reserving solution that concentration is 1000～3000mg/L earlier;
(2) standard operation solution: accurately pipette 10 μ L, 25 μ L, 50 μ L, 250 μ L and 500 μ L standard reserving solutions respectively, be settled in the volumetric flask of 100mL as solvent with methyl alcohol.
3. the method for colorant solvent green 7 in the mensuration dry food wrapping paper according to claim 1, it is characterized in that in the step (2), concrete operations are: take by weighing the 0.5g sample, be cut into the following fragment of 5mm * 5mm, place 50mL tool plug triangular flask, accurately pipette 10mL extraction solvent water, ultrasonic extraction 20 min, get an amount of extract centrifugal 5min in centrifuge tube, get supernatant liquor, behind 0.45 μ m water membrane filtration, obtain sample solution.
4. the method for colorant solvent green 7 in the mensuration dry food wrapping paper according to claim 1, it is characterized in that in the step (3), chromatographiccondition is: chromatographic column is the C18 chromatographic column, specification is 150mm * 4.6mm * 5.0 μ m; Column temperature is 30 ℃; Flow velocity is 1.0mL/min; Sample size is 10 μ L; Mobile phase A is methyl alcohol, and Mobile phase B is ion-pairing agent solution, and V/V is 45%/55%～55%/45%, adopts isocratic elution; The detection wavelength of DAD detecting device is 246nm.
5. the method for colorant solvent green 7 in the mensuration dry food wrapping paper according to claim 4, it is characterized in that: the used ion-pairing agent of Mobile phase B is that concentration is tetrabutyl ammonium hydrogen phosphate or the TBAH aqueous solution of 5mmol/L～15 mmol/L.
6. the method for colorant solvent green 7 in the mensuration dry food wrapping paper according to claim 1, it is characterized in that, in the step (4), typical curve is drawn and the result is calculated as follows: the concentration with solvent in the working solution green 7 is horizontal ordinate, peak area with green 7 ion-pair compounds of solvent in the chromatogram is ordinate, carry out regretional analysis, obtain typical curve; With the chromatographic peak area of green 7 ion-pair compounds of solvent in the sample solution that records under the same terms, the substitution working curve, the content of solvent green 7 in the sample is tried to achieve in conversion according to following formula:
In the formula: in the formula: X is the content of solvent green 7 in the sample, mg/kg; C is the concentration by solvent in the sample solution that reads on the standard working curve green 7, mg/L; C
0Be the concentration by solvent in the blank solution that reads on the standard working curve green 7, mg/L; 524 is the molecular weight of solvent green 7; V is the volume of extraction system, mL; M is the quality of sample, g; 1181 is the molecular weight of green 7 ion-pair compounds of solvent.
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Cited By (4)
| Publication number | Priority date | Publication date | Assignee | Title |
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| CN104122362A (en) * | 2014-07-31 | 2014-10-29 | 国家烟草质量监督检验中心 | Method for determining contents of solvent green 7,2,4-dinitrophenol, propyl p-hydroxybenzoate and sodium salt thereof in paper |
| CN104251893A (en) * | 2014-04-23 | 2014-12-31 | 河北中烟工业有限责任公司 | Method for determining colorant in cigarette package material |
| CN107607651A (en) * | 2017-09-20 | 2018-01-19 | 国家烟草质量监督检验中心 | The assay method of 14 kinds of disabling colouring agents in a kind of ultra performance liquid chromatography tandem mass spectrum detection cigarette paper |
| CN110836937A (en) * | 2019-11-29 | 2020-02-25 | 江苏中烟工业有限责任公司 | Method for evaluating distribution rate of functional additives in dry food packaging paper |
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Cited By (5)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN104251893A (en) * | 2014-04-23 | 2014-12-31 | 河北中烟工业有限责任公司 | Method for determining colorant in cigarette package material |
| CN104122362A (en) * | 2014-07-31 | 2014-10-29 | 国家烟草质量监督检验中心 | Method for determining contents of solvent green 7,2,4-dinitrophenol, propyl p-hydroxybenzoate and sodium salt thereof in paper |
| CN104122362B (en) * | 2014-07-31 | 2015-11-04 | 国家烟草质量监督检验中心 | The assay method of green 7, the 2,4-DNP of solvent and propylparaben and sodium salt content thereof in paper |
| CN107607651A (en) * | 2017-09-20 | 2018-01-19 | 国家烟草质量监督检验中心 | The assay method of 14 kinds of disabling colouring agents in a kind of ultra performance liquid chromatography tandem mass spectrum detection cigarette paper |
| CN110836937A (en) * | 2019-11-29 | 2020-02-25 | 江苏中烟工业有限责任公司 | Method for evaluating distribution rate of functional additives in dry food packaging paper |
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