CN103235051B - 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 a kind of method of measuring colorant solvent green 7 in dry food wrapping paper (mainly comprising fast food wrapping paper, candy paper using, wheaten food paper using etc.).
Background technology
The green 7(Solvent Green 7 of solvent), claim again 8-hydroxyl-1,3,6-pyrene trisulfonic acid trisodium, is a kind of artificial synthetic sulphonic acids dyestuff, is mainly used in the painted of paint, plastic products etc., 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, some colorants can cause the organ irritation such as eyes, oral cavity, the colorant also having can see through skin and be absorbed by the body, there is obvious mutagenesis, use for a long time this series products even can bring out cancer.Based on above-mentioned reason, the legislation as numerous and confused in the U.S., Japan and European Union etc. of many countries is limited the consumption of colorant in the world.China's " hygienic standards for cosmetics " is also by green solvent 7 scopes of listing temporary colorant in.The molecular structural formula of solvent green 7 is as follows.
Dry food wrapping paper is important component part indispensable in 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.Very likely can serve as raw materials for production in view of solvent green 7, in the production run of paper, be used to as colorant.Therefore the detection method of exploring a kind of solvent fast and accurately green 7, control effectively to the colorant in dry food wrapping paper, ensures the safety in utilization of dry food wrapping paper, is very urgent and necessary.
About the analysis and research report of solvent green 7, mainly concentrate on cosmetics aspect.The analytical approach adopting is liquid phase chromatography.The people such as Sun little Ying, Li Ying uses respectively C18 reverse-phase chromatographic column, taking acetonitrile-potassium dihydrogen phosphate buffer solution as mobile phase, with DAD detecting device scanning detection, 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 cosmetics green 7.But actual effect checking shows, in the method, object appearance time is short, and when actual detection, has very serious overlapping phenomenon with other material in sample, and separating effect is poor.In fact, the chromatogram column length that the method adopts is 250mm, and the appearance time of solvent green 7 is more at 2min, can infer solvent green 7 and substantially not retain in chromatographic column.Therefore, the method be not suitable for solvent green 7 to detect analysis.
Summary of the invention
Goal of the invention: for the deficiencies in the prior art, the object of this invention is to provide a kind of method of measuring colorant solvent green 7 in dry food wrapping paper, the method adopts reversed phase ion to measure colorant solvent green 7 in dry food wrapping paper to high performance liquid chromatography (use diode array detector), can fast, accurately detect the content of colorant solvent green 7 in dry food wrapping paper, there is the features such as result is accurate, interference is few.
Technical scheme: in order to realize foregoing invention object, the technical solution used in the present invention is as follows:
A method of measuring colorant solvent green 7 in dry food wrapping paper, comprises the following steps:
(1) preparation of standard operation solution: taking solvent green 7 as standard items, use water as solvent, be configured to standard operation solution through stepwise dilution;
(2) preparation of sample solution: accurately take a certain amount of dry food wrapping paper sample, shred, with a certain amount of solvent supersonic extraction, extract is crossed to water filter membrane, obtain sample solution;
(3) efficient liquid phase chromatographic analysis: use with diode array detector high performance liquid chromatograph (HPLC) standard operation solution and sample solution are detected to analysis;
(4) Specification Curve of Increasing and result are calculated.
In step (1), 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 0.1～0.3g reference material solvent green 7, first use 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 respectively 10 μ L, 25 μ L, 50 μ L, 250 μ L and 500 μ L standard reserving solutions, water is cooked in the volumetric flask that solvent is settled to 100mL again.
In step (2), the preparation of described sample solution, specifically comprise the following steps: take 0.5g sample (being accurate to 0.1 mg), be cut into the fragment below 5mm × 5mm, be placed in 50mL tool plug triangular flask, accurately pipette 10mL extraction solvent water, ultrasonic extraction 20min, gets appropriate extract centrifugal 5min in centrifuge tube, gets supernatant liquor, after 0.45 μ m water membrane filtration, obtain sample solution.
In step (3), liquid-phase chromatographic analysis condition is: chromatographic column is C18 chromatographic column, and specification is 150mm(length) × 4.6mm(internal diameter) × 5.0 μ m(filler granularities); Column temperature is 30 DEG C; 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 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 step (4), described Specification Curve of Increasing and result are calculated as follows: taking the concentration of solvent in working solution green 7 as horizontal ordinate, taking the peak area of green 7 ion-pair compounds of solvent in chromatogram as ordinate, carry out regretional analysis, obtain typical curve; By the chromatographic peak area of green 7 ion-pair compounds of solvent in the sample solution recording under the same terms, substitution working curve, converts and tries to achieve the content of solvent green 7 in sample.
Beneficial effect: compared with prior art, the method of colorant solvent green 7 in mensuration dry food wrapping paper of the present invention, first from dry food wrapping paper, extraction obtains colorant 7, recycle itself and ion-pairing agent and form ion-pair compound, thereby can utilize DAD detecting device that it is carried out qualitative confirmation and is quantitatively detected.The method has proposed first employing reversed phase ion colorant solvent green 7 in high-performance liquid chromatogram determination dry food wrapping paper has been measured, there is the features such as quick, accurate, sensitivity is high, and can evade the interference that matrix is brought, be particularly suitable for measuring the content of colorant solvent green 7 in dry food wrapping paper.
Brief description of the 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 further described.
Embodiment 1
A method of measuring colorant solvent green 7 in dry food wrapping paper, detailed process is as follows:
(1) preparation of standard operation solution
Accurately take 0.2g reference material solvent green 7, first use a small amount of aqueous dispersion, dissolving, then water is settled in the volumetric flask of 100mL, obtain the standard reserving solution that concentration is 2000mg/L.Accurately pipette respectively 10 μ L, 25 μ L, 50 μ L, 250 μ L and 500 μ L standard reserving solutions, water is settled in the volumetric flask of 100mL again.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 0.5g sample (being accurate to 0.1mg), be cut into the fragment below 5mm × 5mm, be placed in 50mL tool plug triangular flask, accurately pipette 10mL extraction solvent water, ultrasonic extraction 20min, gets appropriate extract centrifugal 5min in centrifuge tube, gets supernatant liquor, after 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 respectively liquid chromatography, and as shown in Figure 1, as shown in Figure 2, the chromatogram of mark-on sample as shown in Figure 3 for the chromatogram of sample solution for the chromatogram of standard operation solution.Chromatographiccondition is: chromatographic column is C18 chromatographic column, and specification is 150mm(length) × 4.6mm(internal diameter) × 5.0 μ m(filler granularities); Column temperature is 30 DEG C; 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) Specification Curve of Increasing and result are calculated
First taking the concentration of solvent in standard operation solution green 7 as horizontal ordinate, taking the peak area of solvent in chromatogram green 7 as ordinate, carry out regretional analysis, obtain typical curve, get the standard operation solution of least concentration, do 10 Parallel testing analyses, calculate its standard deviation, taking concentration corresponding to the standard deviations of 3 times as detection limit.The data such as regression equation, related coefficient corresponding with standard working curve 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 by the chromatographic peak area of solvent in the sample solution recording under the same terms green 7, substitution working curve, tries to achieve the content of solvent green 7 in sample, and computing formula is as follows:
In formula: X is the content of solvent green 7 in sample, mg/kg; C is the concentration by solvent in the sample solution reading on standard working curve green 7, mg/L; C
0for the concentration of solvent in the blank solution by reading on 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, choose 30 dry food wrapping paper samples (comprising fast food wrapping paper, candy paper using, wheaten food paper using etc.) are detected, all do not detect solvent green 7.In addition, taking a candy paper using as determination object (measured value is not for detecting), adding concentration to it is the standard specimen of 80.0 mg/kg, and fructufy measured value is 78.93mg/kg, and relative deviation is 0.67%, and the accuracy of visible measurement result is better.
Embodiment 2 solvents green 7 qualitative
Must meet following two conditions to the qualitative confirmation method of object solvent green 7: 1. contrast the permissible error that the retention time of sample chromatogram figure is ± 2.5% with the retention time of standard model chromatogram; 2. contrast (be its spectrogram below, as can be seen from Figure 4, have stronger uv absorption at wavelength 246nm place, Gu Analysis about Selection wavelength is 246nm) with the spectrogram of standard model, the spectrogram of sample must be consistent.
The detection of embodiment 3 precision and the recovery
The present embodiment is as follows to the detection method of precision of the present invention and recovery of standard addition:
The detection of precision: taking a candy paper using sample as object (measured value is not for detecting), the content of (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, result is as shown in table 1.The reproducible of this method has been described.
The precision (n=6) of table 1 method
| 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 using) as mark-on sample substrate, make respectively low, to neutralize high 3 concentration levels mark-on sample, result is as shown in table 2, the recovery of fast food wrapping paper is 85.06～106.25%, the recovery of candy paper using is 83.90～101.75%, has illustrated that the recovery of this method is high.
The recovery of standard addition of table 2 solvent green 7
The present embodiment interior mark liquid used and standard solution only describe as an example of one of them concentration example, typical curve and regression equation that the interior mark liquid that other concentration value configures and standard solution obtain through chromatograph mass spectrum analysis are same as the previously described embodiments, are not enumerating at this.Just method for a better understanding of the present invention of illustrated embodiment, does not have any restriction, and said method or the method that is equal to above-mentioned situation are all included in the protection domain of technical scheme of the present invention.
Claims (4)
1. a method of measuring colorant solvent green 7 in dry food wrapping paper, is characterized in that, comprises the following steps:
(1) taking solvent green 7 as standard items, use water as solvent, be configured to standard operation solution through stepwise dilution;
(2) take quantitative dry food wrapping paper sample, pulverize, the ultrasonic extraction of water, crosses water filter membrane, obtains sample solution;
(3) use with diode array detector high performance liquid chromatograph standard operation solution and sample solution are detected to analysis;
(4) Specification Curve of Increasing and result are calculated;
In step (3), chromatographiccondition is: chromatographic column is C18 chromatographic column, and specification is 150mm × 4.6mm × 5.0 μ m; Column temperature is 30 DEG C; 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; Mobile phase B ion-pairing agent used is that concentration is tetrabutyl ammonium hydrogen phosphate or the TBAH aqueous solution of 5mmol/L～15mmol/L.
2. the method for colorant solvent green 7 in mensuration dry food wrapping paper according to claim 1, is characterized in that, in step (1), the preparation of standard operation solution specifically comprises the following steps:
(1) standard reserving solution: accurately take 0.1～0.3g reference material solvent green 7, first use aqueous dispersion, dissolving, then water is settled in the volumetric flask of 100mL, obtain the standard reserving solution that concentration is 1000～3000mg/L;
(2) standard operation solution: accurately pipette respectively 10 μ L, 25 μ L, 50 μ L, 250 μ L and 500 μ L standard reserving solutions, be settled in the volumetric flask of 100mL as solvent with methyl alcohol.
3. the method for colorant solvent green 7 in mensuration dry food wrapping paper according to claim 1, it is characterized in that, in step (2), concrete operations are: take 0.5g sample, be cut into the fragment below 5mm × 5mm, be placed in 50mL tool plug triangular flask, accurately pipette 10mL extraction solvent water, ultrasonic extraction 20min, get appropriate extract centrifugal 5min in centrifuge tube, get supernatant liquor, after 0.45 μ m water membrane filtration, obtain sample solution.
4. the method for colorant solvent green 7 in mensuration dry food wrapping paper according to claim 1, it is characterized in that, in step (4), Specification Curve of Increasing and result are calculated as follows: taking the concentration of solvent in working solution green 7 as horizontal ordinate, taking the peak area of green 7 ion-pair compounds of solvent in chromatogram as ordinate, carry out regretional analysis, obtain typical curve; By the chromatographic peak area of green 7 ion-pair compounds of solvent in the sample solution recording under the same terms, substitution working curve, converts and tries to achieve the content of solvent green 7 in sample according to following formula:
In formula: in formula: X is the content of solvent green 7 in sample, mg/kg; C is the concentration by solvent in the sample solution reading on standard working curve green 7, mg/L; C
0for the concentration of solvent in the blank solution by reading on 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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| 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 |
| 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 |
Citations (2)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| US5108502A (en) * | 1990-03-16 | 1992-04-28 | Hewlett-Packard Company | Boronic acid dyes |
| CN101965513A (en) * | 2008-03-12 | 2011-02-02 | 津浦罗公司 | Fluorescent dye tracer method for animal feed supplement products |
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| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| US5108502A (en) * | 1990-03-16 | 1992-04-28 | Hewlett-Packard Company | Boronic acid dyes |
| CN101965513A (en) * | 2008-03-12 | 2011-02-02 | 津浦罗公司 | Fluorescent dye tracer method for animal feed supplement products |
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