CN105259294A - Method for detecting residual quantity of melamine and cyanuric acid in melamine cyanurate - Google Patents
Method for detecting residual quantity of melamine and cyanuric acid in melamine cyanurate Download PDFInfo
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- CN105259294A CN105259294A CN201510786928.1A CN201510786928A CN105259294A CN 105259294 A CN105259294 A CN 105259294A CN 201510786928 A CN201510786928 A CN 201510786928A CN 105259294 A CN105259294 A CN 105259294A
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Abstract
The invention provides a method for detecting the residual quantity of melamine and cyanuric acid in melamine cyanurate. According to the adopted technical scheme, the method includes the steps that melamine and cyanuric acid are extracted from the melamine cyanurate product by means of solubility difference among melamine cyanurate, melamine and cyanuric acid in solvent to obtain a melamine and cyanuric acid test solution, and then liquid chromatogram is used for detecting the residual quantity of melamine and cyanuric acid in the sample. The detection method is convenient and rapid, and results are accurate.
Description
Technical field
The present invention relates to the detection method that a kind of liquid phase chromatography detects melamine and cyanuric acid residual quantity in melamine cyanurate.
Background technology
Melamine cyanurate is the salt synthesized by melamine and cyanuric acid, belongs to nitrogenated flame retardant, has Powdered and graininess two kinds of forms.Wherein melamine and cyanuric acid residual quantity are two important indicators that melamine cyanurate compares concern, both a large amount of existence can use the processing of product, production and material mechanical performance to cause larger impact on downstream, the domestic method not having melamine and cyanuric acid residual quantity in the detection melamine cyanurate of clear stipulaties at present.
The patent of invention that application number 201310014881.8 1 kinds detects the method for melamine discloses a kind of method detecting trimerization ammonia amine, the method is the detection for one matter melamine in dairy products or milk powder, but the method is unsuitable for detecting the melamine in melamine cyanurate, this is because a kind of starting material that melamine is melamine cyanurate need to carry out trace extraction, and require that detection limit is lower, lower than 100ppm.This patented method is not suitable for the melamine detected in melamine cyanurate.
Summary of the invention
The present invention aims to provide a kind of method detecting melamine and cyanuric acid residual quantity in melamine cyanurate.Fast and easy, result are accurate.
The technical solution used in the present invention is, a kind of method detecting melamine and cyanuric acid residual quantity in melamine cyanurate, the difference of melamine cyanurate, melamine and cyanuric acid solubleness is in a solvent utilized melamine, cyanuric acid to be extracted from melamine cyanurate product, obtain the test solution of melamine and cyanuric acid, then utilize liquid chromatography to detect melamine and cyanuric acid residual quantity in sample respectively.
Concrete scheme is, a kind of method detecting melamine and cyanuric acid residual quantity in melamine cyanurate, and step is as follows:
(1) prepare melamine and cyanuric acid standard solution respectively, with liquid chromatograph, it is detected, obtain retention time, generate the typical curve that peak area is corresponding with between concentration;
Wherein, ion-pairing agent buffer solution+second eyeball (v+v)=83+17 that the mobile phase that during detection melamine, liquid chromatography uses is; The preparation of ion-pairing agent buffer solution used: take 2.10g citric acid and 2.16g perfluorooctane sulfonate, use water-soluble solution, the 980mL that adds water is adjusted to pH ≈ 3, is settled to 1000mL.Mobile phase process 30 ~ 40min ultrasonic after 0.45 μm of organic membrane filtration.Liquid phase chromatogram condition: flow velocity (0.8 ~ 1.0) mL/min; Determined wavelength: 240nm; Column temperature: room temperature; Sample size 20uL.
Ion-pairing agent buffer solution+second eyeball (v+v)=92+8 that the mobile phase that during detection cyanuric acid, liquid chromatography uses is; The preparation of ion-pairing agent buffer solution used: take 1.61g tetrabutyl ammonium bromide and 1.79g sodium hydrogen phosphate, use water-soluble solution, the 980mL that adds water is adjusted to pH ≈ 7.5, is settled to 1000mL.Mobile phase is ultrasonic process 30 ~ 40min after 0.45 μm of organic membrane filtration.Liquid phase chromatogram condition: flow velocity (0.8 ~ 1.0) mL/min; Determined wavelength: 220nm; Column temperature: room temperature; Sample size 20uL.
(2) get melamine cyanurate sample and carry out pre-service, obtain analyze test solution, liquid chromatograph with step (1) the same terms under test solution is detected, obtain the testing result of described sample;
Wherein, the pre-service of sample: take sample and be placed in 500mL conical flask, accurately measure 250mL ultrapure water and add and fill in the conical flask of testing sample, be heated to 50 DEG C, 0.45 μm of inorganic filter membrane after cooling filters, and collects its filtrate.
(3) the characteristic peak peak area recorded in step (2) is brought into typical curve in step (1), try to achieve the concentration of melamine and cyanuric acid residual quantity in test solution to be measured, then melamine and cyanuric acid residual quantity in melamine cyanurate sample are determined in calculating.
The method that the present invention detects melamine and cyanuric acid residual quantity in melamine cyanurate is applicable to melamine and the analysis of cyanuric acid residues detection in melamine cyanurate.
The present invention has following beneficial effect:
(1) the invention solves the problem that in melamine cyanurate (MCA), melamine and cyanuric acid residual quantity can not quantitatively detect, achieve the monitoring to two kinds of raw material residual quantity indexs.Because the content of the residual melamine in melamine cyanurate (MCA) and cyanuric acid is lower, original detection method just surveys main content by surveying total nitrogen content in product, there is certain error.The invention solves the problem that melamine and cyanuric acid two kinds of raw material residual quantities guarantee to extract completely, develop the pre-treating method of product; Have selected suitable mobile phase, make the peak energy of two kinds of residuals enough complete separately, the interference at inclusion-free peak.Testing result of the present invention is accurate, and detection limit is lower, reaches below 100ppm.
(2) the present invention is while realization is monitored melamine cyanurate quality, serves critical quantitative synergism to production run and technique cost declining.
(3) the present invention is simple to operate, easy to operate, greatly shortens detection time compared with gravimetric method, is more suitable for detecting for process.
(4) the present invention effectively avoids impurity effect.Adopt above-mentioned mobile phase and pre-treating method, detect melamine characteristic peak and cyanuric acid characteristic peak in melamine cyanurate can separate completely, can not occur overlapping because of impurity peaks and melamine peak and affect and detect, be conducive to carrying out qualitative and quantitative analysis.
Accompanying drawing explanation
Fig. 1 is melamine standard items chromatograms;
Fig. 2 is melamine working curve;
Fig. 3 is melamine residual amount chromatogram in melamine cyanurate;
Fig. 1-3 chromatographic condition: chromatographic column Kromasil, C18,5um, 250*4.6mm; Flow velocity 1.0mL/min; Determined wavelength: 240nm; Column temperature: room temperature; Sample size 20uL.
Fig. 4 is cyanuric acid standard items chromatograms;
Fig. 5 is cyanuric acid working curve;
Fig. 6 is cyanuric acid residual quantity chromatogram in melamine cyanurate;
Fig. 4-6 chromatographic condition: chromatographic column Kromasil, C18,5um, 250*4.6mm; Flow velocity 1.0mL/min; Determined wavelength: 220nm; Column temperature: room temperature; Sample size 20uL
Embodiment
Further illustrate the present invention below by embodiment, following examples are the concrete embodiment of the present invention, but embodiments of the present invention are by the restriction of following embodiment.
1, instrument and equipment
Glassware etc. commonly used by liquid chromatograph with UV-detector, ultrasound wave, electronic balance (being accurate to 0.1mg), filtrator, organic filter membrane, inorganic filter membrane, disposable filtering head, injector, laboratory
2, reagent
Acetonitrile (chromatographically pure), methyl alcohol (chromatographically pure), perfluorooctane sulfonate (chromatographically pure), tetrabutyl ammonium bromide (chromatographically pure), ultrapure water, all the other are pure for analyzing
3, chromatographic condition
Chromatographic column: Kromasil, C18,5um, 250*4.6mm;
Flow velocity: 1.0mL/min;
Column temperature: room temperature;
Sample size: 20uL;
Melamine residual amount determined wavelength: 240nm;
Cyanuric acid residues detection wavelength: 220nm.
4, detecting step
1) melamine Specification Curve of Increasing
Take melamine standard items 0.1000g, be settled in 100mL volumetric flask with methyl alcohol+water (v+v)=60+40, as standard reserving solution (1mg/mL).Be 0 μ g/mL by mobile phase stepwise dilution concentration, 0.2 μ g/mL, 0.4 μ g/mL, 0.8 μ g/mL, 1.0 μ g/mL, 2.0 μ g/mL, 5.0 μ g/mL, 10.0 μ g/mL, the standard solution of 20.0 μ g/mL.Can adjust accordingly according to reagent situation.
Wherein, mobile phase ion-pairing agent buffer solution+second eyeball (v+v)=83+17 of being; The preparation of ion-pairing agent buffer solution used: take 2.10g citric acid and 2.16g perfluorooctane sulfonate, use water-soluble solution, the 980mL that adds water is adjusted to pH ≈ 3, is settled to 1000mL.Mobile phase process 30 ~ 40min ultrasonic after 0.45 μm of organic membrane filtration.
Melamine standard solution, by flow velocity 1.0mL/min; Determined wavelength: 240nm; Column temperature: room temperature; Sample size 20uL chromatographic condition detects.By standard solution successively sample introduction, record peak area respectively.Test result in table 1, Fig. 1, Fig. 2.
Table 1 concentration of standard solution, peak area and retention time
Drawing standard curve: take peak area as ordinate, concentration is horizontal ordinate, and drawing standard curve obtains typical curve equation.
Typical curve equation y=8188.8543x+329.0712
Y: peak area; X: melamine concentration;
Correlativity R
2=0.9998
2) cyanuric acid Specification Curve of Increasing
Take cyanuric acid standard items 0.1000g, be settled in 100mL volumetric flask with methyl alcohol+water (v+v)=60+40, as standard reserving solution (1mg/mL).Be 0 μ g/mL by mobile phase stepwise dilution concentration, 2.0 μ g/mL, 5.0 μ g/mL, 10.0 μ g/mL, 20.0 μ g/mL, 40.0 μ g/mL, 50.0 μ g/mL, 60.0 μ g/mL, the standard solution of 80.0 μ g/mL.Can adjust accordingly according to reagent situation.
Wherein, mobile phase ion-pairing agent buffer solution+second eyeball (v+v)=92+8 of being; The preparation of ion-pairing agent buffer solution used: take 1.61g tetrabutyl ammonium bromide and 1.79g sodium hydrogen phosphate, use water-soluble solution, the 980mL that adds water is adjusted to pH ≈ 7.5, is settled to 1000mL.Mobile phase is ultrasonic process 30 ~ 40min after 0.45 μm of organic membrane filtration.
Above-mentioned cyanuric acid standard solution, by liquid phase chromatogram condition: flow velocity 1.0mL/min; Determined wavelength: 220nm; Column temperature: room temperature; Sample size 20uL.By standard solution successively sample introduction, record peak area respectively.Test result in table 2, Fig. 4, Fig. 5.
Table 2 concentration of standard solution, peak area and retention time
Drawing standard curve: take peak area as ordinate, concentration is horizontal ordinate, and drawing standard curve obtains typical curve equation.
Typical curve equation y=3887.7444x+3154.4373
Y: peak area; X: cyanuric acid concentration;
Correlativity R
2=0.9996
3) testing sample is detected
Take 2g melamine cyanurate sample (being accurate to 0.1mg) as in 500mL conical flask, accurately measure 250mL ultrapure water to add and fill in the conical flask of testing sample, be heated to 50 DEG C, 0.45 μm of inorganic filter membrane after cooling filters, and gets its filtrate under the chromatographic condition of above-mentioned requirements, carries out melamine and cyanuric acid residual quantity chromatographic determination respectively.
3) result calculates
A) in sample, melamine residual amount calculates acquisition by chromatographic data:
In formula: ω---melamine residual amount (%) in sample;
C---from the concentration (μ g/mL) of the melamine residual amount that typical curve obtains
M---take the quality (g) of sample.
B) in sample, cyanuric acid residual quantity calculates acquisition by chromatographic data:
In formula: ω---cyanuric acid residual quantity (%) in sample;
C---from the concentration (μ g/mL) of the cyanuric acid residual quantity that typical curve obtains
M---take the quality (g) of sample.
Hereafter specifically test acquired results to above-mentioned detecting step to be described, the case study on implementation wherein enumerated all is carrying out pre-treatment on the same day, carries out upper machine testing on the same day.
Embodiment 1
Getting melamine cyanurate sample 2.0189g, by detecting melamine and cyanuric acid residual quantity under above-mentioned requirements condition, the results are shown in Table 3, Fig. 3, table 4, Fig. 6.
In table 3 melamine cyanurate, melamine residual measures test result
| Test sequence number | Retention time (min) | Result (%) |
| 1 | 8.68 | 0.0012 |
| 2 | 8.57 | 0.0012 |
Cyanuric acid residual quantity test result in table 4 melamine cyanurate
| Test sequence number | Retention time (min) | Result (%) |
| 1 | 4.18 | 0.2401 |
| 2 | 4.21 | 0.2393 |
Embodiment 2
Get melamine cyanurate sample 2.0156g, 5.0 μ g/mL add melamine and 5.0 μ g/mL cyanuric acids in proportion, detect melamine and cyanuric acid residual quantity under above-mentioned requirements condition.Test result is in table 5, table 6.
In table 5 melamine cyanurate, melamine residual measures test result
| Retention time (min) | Add scalar (μ g/mL) | Result (μ g/mL) | The recovery (%) |
| 8.50 | 5.0 | 4.9869 | 99.74 |
Melamine cyanurate residual quantity test result in table 6 melamine cyanurate
| Retention time (min) | Add scalar (μ g/mL) | Result (%) | The recovery (%) |
| 4.25 | 5.0 | 4.9689 | 99.38 |
Embodiment 3
Get melamine cyanurate sample 2.0000g, 5.0 μ g/mL add melamine and 5.0 μ g/mL cyanuric acids in proportion, repeat preparation 3 parts, detect melamine and cyanuric acid residual quantity under above-mentioned requirements condition.Test result is in table 7, table 8.
In table 7 melamine cyanurate, melamine residual measures test result
| Test sequence number | Retention time (min) | Result (μ g/mL) | Recovery of standard addition (%) |
| 1 | 8.59 | 4.9869 | 99.74 |
| 2 | 8.62 | 4.9568 | 99.14 |
| 3 | 8.60 | 4.9298 | 98.60 |
Cyanuric acid residual quantity test result in table 8 melamine cyanurate
| Test sequence number | Retention time (min) | Result (μ g/mL) | Recovery of standard addition (%) |
| 1 | 4.25 | 4.9568 | 99.14 |
| 2 | 4.21 | 4.9859 | 99.72 |
| 3 | 4.23 | 4.9758 | 99.52 |
Embodiment 4
Get the standard solution containing 10.0 μ g/mL melamines, detect melamine residual amount under these conditions, wherein flow velocity: 0.8mL/min.Concrete detection data are in table 9.
Table 9 the inventive method detects the retention time (flow velocity: 0.8mL/min) of melamine
| Retention time (min) | Title | Add scalar (μ g/mL) |
| 10.26 | Melamine | 10.0 |
Contrast known, the retention time of melamine standard items is 10.26min, and the impurity peaks retention time of interference may be caused in melamine cyanurate to be 10.19min, and this impurity peaks is fixing impurity peaks, do not change with the change of testing environment, and it retains peak time near melamine.In the inventive method testing result, the retention time difference of impurity and melamine obviously, can separate completely, do not cause interference to test result by impurity peaks and melamine.
Embodiment 5
Get the standard solution containing 10.0 μ g/mL cyanuric acids, detect cyanuric acid residual quantity under these conditions, wherein ion-pairing agent buffer solution+second eyeball (v+v)=85+15.Concrete detection data are in table 10.
Table 10 the inventive method detects the retention time (flow velocity: 0.8mL/min) of melamine
| Retention time (min) | Title | Add scalar (μ g/mL) |
| 3.56 | Melamine | 10.0 |
Contrast known, the retention time of cyanuric acid standard items is 3.56min, and the impurity peaks retention time of interference may be caused in melamine cyanurate to be 3.49min, and this impurity peaks is fixing impurity peaks, do not change with the change of testing environment, and it retains peak time near cyanuric acid.In the inventive method testing result, the retention time difference of impurity and cyanuric acid obviously, can separate completely, do not cause interference to test result by impurity peaks and melamine.
From above method validation result, method of the present invention is convenient and simple, easy to operate, and accuracy is higher.Can be used as the detection of melamine and cyanuric acid residual quantity in melamine cyanurate.
Claims (6)
1. detect a method for melamine and cyanuric acid residual quantity in melamine cyanurate, it is characterized in that, comprise the following steps:
(1) prepare melamine and cyanuric acid standard solution respectively, with liquid chromatograph, it is detected, obtain retention time, generate the typical curve that peak area is corresponding with between concentration;
(2) get melamine cyanurate sample and carry out pre-service, obtain analyze test solution, utilize liquid chromatograph with step (1) the same terms under test solution is detected, obtain the testing result of described sample;
(3) the characteristic peak peak area recorded in step (2) is brought into typical curve in step (1), try to achieve the concentration of melamine and cyanuric acid residual quantity in test solution to be measured, then melamine and cyanuric acid residual quantity in melamine cyanurate sample are determined in calculating;
Ion-pairing agent buffer solution+second eyeball (v+v)=83+17 that the mobile phase that in described step (1), during detection melamine, liquid chromatography uses is; The preparation of described ion-pairing agent buffer solution: take 2.10g citric acid and 2.16g perfluorooctane sulfonate, use water-soluble solution, the 980mL that adds water is adjusted to pH ≈ 3, is settled to 1000mL; Described mobile phase is ultrasonic process 30 ~ 40min after 0.45 μm of organic membrane filtration;
Ion-pairing agent buffer solution+second eyeball (v+v)=92+8 that the mobile phase that in described step (1), during detection cyanuric acid, liquid chromatography uses is; The preparation of described ion-pairing agent buffer solution: take 1.61g tetrabutyl ammonium bromide and 1.79g sodium hydrogen phosphate, use water-soluble solution, the 980mL that adds water is adjusted to pH ≈ 7.5, is settled to 1000mL; Described mobile phase is ultrasonic process 30 ~ 40min after 0.45 μm of organic membrane filtration;
Sample pretreatment in described step (2) comprises the following steps: take 2.0g sample and be placed in 500mL conical flask, accurately measure 250mL ultrapure water to add and fill in the conical flask of testing sample, be heated to 50 DEG C, 0.45 μm of inorganic filter membrane after cooling filters, and collects its filtrate.
2. the method for melamine and cyanuric acid residual quantity in detection melamine cyanurate according to claim 1, it is characterized in that, in described step (1), melamine standard solution compound method is: melamine standard items 0.1000g, be settled in 100mL volumetric flask with methyl alcohol+water (v+v)=60+40, as standard reserving solution (1mg/mL); Be 0 μ g/mL by mobile phase stepwise dilution concentration, 0.2 μ g/mL, 0.4 μ g/mL, 0.8 μ g/mL, 1.0 μ g/mL, 2.0 μ g/mL, 5.0 μ g/mL, 10.0 μ g/mL, the standard solution of 20.0 μ g/mL.
3. the method for melamine and cyanuric acid residual quantity in detection melamine cyanurate according to claim 1, it is characterized in that, in described step (1), cyanuric acid standard solution compound method is: take cyanuric acid standard items 0.1000g, be settled in 100mL volumetric flask with methyl alcohol+water (v+v)=60+40, as standard reserving solution (1mg/mL); Be 0 μ g/mL by mobile phase stepwise dilution concentration, 2.0 μ g/mL, 5.0 μ g/mL, 10.0 μ g/mL, 20.0 μ g/mL, 40.0 μ g/mL, 50.0 μ g/mL, 60.0 μ g/mL, the standard solution of 80.0 μ g/mL.
4. the method for melamine and cyanuric acid residual quantity in detection melamine cyanurate according to claim 1, is characterized in that, detects the liquid phase chromatogram condition of melamine: flow velocity 0.8-1.0mL/min in described step (1); Determined wavelength: 240nm; Column temperature: room temperature; Sample size 20uL.
5. the method for melamine and cyanuric acid residual quantity in detection melamine cyanurate according to claim 1, is characterized in that, detects the phase chromatographic condition of cyanuric acid liquid: flow velocity 0.8-1.0mL/min in described step (1); Determined wavelength: 220nm; Column temperature: room temperature; Sample size 20uL.
6. the application of the method detecting melamine and cyanuric acid residual quantity in melamine cyanurate described in claim 1 in melamine cyanurate in melamine and cyanuric acid qualitative and quantitative analysis.
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| CN110132958A (en) * | 2019-05-09 | 2019-08-16 | 广东环凯微生物科技有限公司 | A kind of cyanuric acid measurement reagent and its preparation method and application |
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