CN105259294B - 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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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 a kind of liquid chromatography detects melamine and cyanuric acid residual quantity in melamine cyanurate
Detection method.
Background technology
Melamine cyanurate is the salt synthesized by melamine and cyanuric acid, belongs to nitrogenated flame retardant, with powder
Two kinds of forms of shape and graininess.Wherein melamine and cyanuric acid residual quantity are two that melamine cyanurate compares concern
Important indicator, both a large amount of presence can cause larger shadow to downstream using the processing of product, production and material mechanical performance
Ring, the side for not having melamine and cyanuric acid residual quantity in the detection melamine cyanurate of clear stipulaties domestic at present
Method.
A kind of patent of invention of the method for detection melamine of application number 201310014881.8 discloses a kind of detection three
The method of poly- ammonia amine, the method is for the detection of single substance melamine in dairy products or milk powder, but the method are unsuitable for
Melamine in detection melamine cyanurate, this is because a kind of former material of the melamine for melamine cyanurate
Material needs to carry out trace extraction, and requires that detection limit is relatively low, to be less than 100ppm.The patented method is not suitable for detecting trimerization
Melamine in cyanamide cyanurate.
The content of the invention
The present invention is intended to provide a kind of method for 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 that melamine and cyanuric acid are remained in one kind detection melamine cyanurate
The method of amount, using melamine cyanurate, melamine and cyanuric acid in a solvent solubility difference by melamine,
Cyanuric acid is extracted from melamine cyanurate product, the test solution of melamine and cyanuric acid is obtained, then using liquid
Melamine and cyanuric acid residual quantity in phase chromatogram difference detection sample.
Concrete scheme is that the method for melamine and cyanuric acid residual quantity, walks in a kind of detection melamine cyanurate
It is rapid as follows：
(1) melamine and cyanuric acid standard liquid are prepared respectively, it is detected with liquid chromatographs, obtain retention time,
Generate corresponding calibration curve between peak area and concentration；
Wherein, ion-pairing agent cushioning liquid+second eyeball (v+ that the mobile phase that liquid chromatogram is used when detecting melamine is
V)=83+17；The preparation of ion-pairing agent cushioning liquid used：2.10g citric acids and 2.16g perfluorooctane sulfonates are weighed, is used
Water dissolves, the 980mL that adds water is adjusted to pH ≈ 3, is settled to 1000mL.Mobile phase is with after 0.45 μm of organic membrane filtration ultrasonically treated 30
～40min.Liquid phase chromatogram condition：Flow velocity (0.8～1.0) mL/min；Detection wavelength：240nm；Column temperature：Room temperature；Sample size 20uL.
Ion-pairing agent cushioning liquid+second eyeball (v+v)=92+ that the mobile phase that liquid chromatogram is used during detection cyanuric acid is
8；The preparation of ion-pairing agent cushioning liquid used：1.61g TBABs and 1.79g disodium hydrogen phosphates are weighed, with water-soluble
Solution, the 980mL that adds water is adjusted to pH ≈ 7.5, is settled to 1000mL.Mobile phase Jing after 0.45 μm of organic membrane filtration ultrasonically treated 30～
40min.Liquid phase chromatogram condition：Flow velocity (0.8～1.0) mL/min；Detection wavelength：220nm；Column temperature：Room temperature；Sample size 20uL.
(2) take melamine cyanurate sample to be pre-processed, obtain analyze test solution, liquid chromatograph with step
(1) test solution is detected under the same terms, obtains the testing result of the sample；
Wherein, the pretreatment of sample：Weigh sample to be placed in 500mL conical flasks, accurately measure 250mL ultra-pure waters and add Sheng
In having the conical flask of testing sample, be heated to 50 DEG C, after cooling with 0.45 μm of inorganic filter membrane filtered, collect its filtrate.
(3) calibration curve for bringing the characteristic peak peak area measured in step (2) in step (1) into, tries to achieve test solution
The concentration of middle melamine and cyanuric acid residual quantity, then calculate melamine and cyanogen urine in determination melamine cyanurate sample
Sour residual quantity.
The method of melamine and cyanuric acid residual quantity is applied to melamine in present invention detection melamine cyanurate
Melamine and cyanuric acid residues detection are analyzed in amine cyanurate.
The present invention has the advantages that：
(1) present invention solves in melamine cyanurate (MCA) that melamine and cyanuric acid residual quantity can not be quantitative
The problem of detection, realizes the monitoring that two kinds of raw materials are remained with figureofmerit.Due to the residual in melamine cyanurate (MCA)
The content of melamine and cyanuric acid is relatively low, and original detection method is surveyed master and contained simply by nitrogen content total in product is surveyed
, there is certain error in amount.The present invention solves two kinds of raw material residual quantities of melamine and cyanuric acid and guarantees to extract completely
Problem, develop the pre-treating method of product；Have selected suitable mobile phase so that the peak energy of two kinds of residuals is enough completed
Separate, the interference at free from admixture peak.Testing result of the present invention is accurate, and detection limit is relatively low, reaches below 100ppm.
(2) it is of the invention while realizing being monitored melamine cyanurate quality, to production process and technique
Cost declining serves critical quantitative synergism.
(3) present invention is simple to operate, easy to operate, and detection time is greatly shortened compared with gravimetric method, is particularly suited for process
Detection.
(4) present invention is prevented effectively from impurity effect.Using above-mentioned mobile phase and pre-treating method, melamine cyanurea is detected
Melamine characteristic peak and cyanuric acid characteristic peak can be completely isolated in hydrochlorate, will not go out with melamine peak because of impurity peaks
Now overlap and affect detection, be conducive to carrying out qualitative and quantitative analysis.
Description of the drawings
Fig. 1 is melamine standard items chromatogram；
Fig. 2 is melamine working curve；
Fig. 3 is melamine residual amount chromatogram in melamine cyanurate；
Fig. 1-3 chromatographic conditions：Chromatographic column Kromasil, C18,5um, 250*4.6mm；Flow velocity 1.0mL/min；Detection ripple
It is long：240nm；Column temperature：Room temperature；Sample size 20uL.
Fig. 4 is cyanuric acid standard items chromatogram；
Fig. 5 is cyanuric acid working curve；
Fig. 6 is cyanuric acid residual quantity chromatogram in melamine cyanurate；
Fig. 4-6 chromatographic conditions：Chromatographic column Kromasil, C18,5um, 250*4.6mm；Flow velocity 1.0mL/min；Detection ripple
It is long：220nm；Column temperature：Room temperature；Sample size 20uL
Specific embodiment
The present invention is further illustrated below by specific embodiment, following examples are the specific embodiment party of the present invention
Formula, but embodiments of the present invention are not limited by following embodiments.
1st, instrument and equipment
Liquid chromatograph with UV-detector, ultrasonic wave, electronic balance (being accurate to 0.1mg), filter, there is machine filter
Film, inorganic filter membrane, disposable filtering head, injector, the conventional glassware in laboratory etc.
2nd, reagent
It is acetonitrile (chromatographically pure), methyl alcohol (chromatographically pure), perfluorooctane sulfonate (chromatographically pure), TBAB (chromatographically pure), super
Pure water, remaining is pure for analysis
3rd, 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 Detection wavelength：240nm；
Cyanuric acid residues detection wavelength：220nm.
4th, detecting step
1) melamine Specification Curve of Increasing
Melamine standard items 0.1000g is weighed, is settled in 100mL volumetric flasks with methyl alcohol+water (v+v)=60+40, made
For standard reserving solution (1mg/mL).With mobile phase stepwise dilution concentration be 0 μ g/mL, 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 liquid of 20.0 μ g/mL.Can be done accordingly according to reagent situation
Adjustment.
Wherein, the ion-pairing agent cushioning liquid that mobile phase is+second eyeball (v+v)=83+17；Ion-pairing agent used delays
Rush the preparation of solution：2.10g citric acids and 2.16g perfluorooctane sulfonates are weighed, with water dissolves, the 980mL that adds water is adjusted to pH ≈ 3, it is fixed
Hold to 1000mL.Mobile phase ultrasonically treated 30～40min after 0.45 μm of organic membrane filtration.
Melamine standard liquid, by flow velocity 1.0mL/min；Detection wavelength：240nm；Column temperature：Room temperature；Sample size 20uL
Chromatographic condition is detected.By standard liquid successively sample introduction, peak area is recorded respectively.Test result is shown in Table 1, Fig. 1, Fig. 2.
The concentration of standard solution of table 1, peak area and retention time
Draw calibration curve：With peak area as ordinate, concentration is abscissa, draws calibration curve, obtains calibration curve
Equation.
Calibration curve equation y=8188.8543x+329.0712
Y：Peak area；x：Melamine concentration；
Correlation R2=0.9998
2) cyanuric acid Specification Curve of Increasing
Cyanuric acid standard items 0.1000g is weighed, is settled in 100mL volumetric flasks with methyl alcohol+water (v+v)=60+40, as
Standard reserving solution (1mg/mL).With mobile phase stepwise dilution concentration be 0 μ g/mL, 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 liquid of 80.0 μ g/mL.Can be done according to reagent situation
Corresponding adjustment.
Wherein, the ion-pairing agent cushioning liquid that mobile phase is+second eyeball (v+v)=92+8；Ion-pairing agent buffering used
The preparation of solution：1.61g TBABs and 1.79g disodium hydrogen phosphates are weighed, with water dissolves, the 980mL that adds water is adjusted to pH ≈
7.5, it is settled to 1000mL.Mobile phase ultrasonically treated 30～40min Jing after 0.45 μm of organic membrane filtration.
Above-mentioned cyanuric acid standard liquid, by liquid phase chromatogram condition：Flow velocity 1.0mL/min；Detection wavelength：220nm；Column temperature：
Room temperature；Sample size 20uL.By standard liquid successively sample introduction, peak area is recorded respectively.Test result is shown in Table 2, Fig. 4, Fig. 5.
The concentration of standard solution of table 2, peak area and retention time
Draw calibration curve：With peak area as ordinate, concentration is abscissa, draws calibration curve, obtains calibration curve
Equation.
Calibration curve equation y=3887.7444x+3154.4373
Y：Peak area；x：Cyanuric acid concentration；
Correlation R2=0.9996
3) testing sample is detected
During 2g melamine cyanurate samples (being accurate to 0.1mg) is weighed as 500mL conical flasks, accurately measure
250mL ultra-pure waters are added and filled in the conical flask of testing sample, are heated to 50 DEG C, after cooling with 0.45 μm of inorganic filter membrane carry out
Filter, take its filtrate carries out respectively melamine and cyanuric acid residual quantity chromatographic determination under the chromatographic condition of above-mentioned requirements.
3) result is calculated
A) melamine residual amount calculates acquisition by chromatographic data in sample：
In formula：ω --- melamine residual amount (%) in sample；
The concentration (μ g/mL) of c --- the melamine residual amount obtained from calibration curve
M --- weigh the quality (g) of sample.
B) cyanuric acid residual quantity calculates acquisition by chromatographic data in sample：
In formula：ω --- cyanuric acid residual quantity (%) in sample；
The concentration (μ g/mL) of c --- the cyanuric acid residual quantity obtained from calibration curve
M --- weigh the quality (g) of sample.
Hereafter specifically tested acquired results to above-mentioned detecting step to be described, wherein the case study on implementation enumerated exists
Pre-treatment is carried out on the same day, and machine testing is carried out on the same day.
Embodiment 1
Melamine cyanurate sample 2.0189g is taken, it is residual by detection melamine and cyanuric acid under the conditions of above-mentioned requirements
Allowance, the results are shown in Table 3, Fig. 3, table 4, Fig. 6.
Melamine residual measures test result in the melamine cyanurate of table 3
| Test sequence number | Retention time (min) | As a result (%) |
| 1 | 8.68 | 0.0012 |
| 2 | 8.57 | 0.0012 |
Cyanuric acid residual quantity test result in the melamine cyanurate of table 4
| Test sequence number | Retention time (min) | As a result (%) |
| 1 | 4.18 | 0.2401 |
| 2 | 4.21 | 0.2393 |
Embodiment 2
Melamine cyanurate sample 2.0156g is taken, in proportion 5.0 μ g/mL addition melamines and 5.0 μ g/mL cyanogen
Uric acid, detects melamine and cyanuric acid residual quantity under the conditions of above-mentioned requirements.Test result is shown in Table 5, table 6.
Melamine residual measures test result in the melamine cyanurate of table 5
| Retention time (min) | Plus scalar (μ g/mL) | As a result (μ g/mL) | The rate of recovery (%) |
| 8.50 | 5.0 | 4.9869 | 99.74 |
Melamine cyanurate residual quantity test result in the melamine cyanurate of table 6
| Retention time (min) | Plus scalar (μ g/mL) | As a result (%) | The rate of recovery (%) |
| 4.25 | 5.0 | 4.9689 | 99.38 |
Embodiment 3
Melamine cyanurate sample 2.0000g is taken, in proportion 5.0 μ g/mL addition melamines and 5.0 μ g/mL cyanogen
Uric acid, repeats to prepare 3 parts, and melamine and cyanuric acid residual quantity are detected under the conditions of above-mentioned requirements.Test result is shown in Table 7, table
8。
Melamine residual measures test result in the melamine cyanurate of table 7
| Test sequence number | Retention time (min) | As a 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 the melamine cyanurate of table 8
| Test sequence number | Retention time (min) | As a 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
The standard liquid containing 10.0 μ g/mL melamines is taken, melamine residual amount is detected under these conditions, wherein flowing
Speed：0.8mL/min.Concrete detection data is shown in Table 9.
The inventive method of table 9 detects the retention time (flow velocity of melamine：0.8mL/min)
| Retention time (min) | Title | Plus scalar (μ g/mL) |
| 10.26 | Melamine | 10.0 |
Contrast understands that the retention time of melamine standard items is 10.26min, may be made in melamine cyanurate
Impurity peaks retention time into interference is 10.19min, and the impurity peaks are fixed impurity peaks, do not change with the change of detection environment
Become, and it retains peak time in the vicinity of melamine.In the inventive method testing result, during the reservation of impurity and melamine
Between difference it is obvious, impurity peaks can be completely isolated with melamine, test result is not interfered.
Embodiment 5
The standard liquid containing 10.0 μ g/mL cyanuric acids is taken, cyanuric acid residual quantity, wherein ion pair are detected under these conditions
Reagent cushioning liquid+second eyeball (v+v)=85+15.Concrete detection data is shown in Table 10.
The inventive method of table 10 detects the retention time (flow velocity of melamine：0.8mL/min)
| Retention time (min) | Title | Plus scalar (μ g/mL) |
| 3.56 | Melamine | 10.0 |
Contrast understands that the retention time of cyanuric acid standard items is 3.56min, is likely to result in melamine cyanurate dry
The impurity peaks retention time disturbed is 3.49min, and the impurity peaks are fixed impurity peaks, do not change with the change of detection environment, and
It retains peak time in the vicinity of cyanuric acid.In the inventive method testing result, the retention time difference of impurity and cyanuric acid is obvious,
Impurity peaks can be completely isolated with melamine, test result is not interfered.
From above method the result, the method for the present invention is convenient and simple, easy to operate, and the degree of accuracy is higher.Can be used as
The detection of melamine and cyanuric acid residual quantity in melamine cyanurate.
Claims (4)
1. it is a kind of detection melamine cyanurate in melamine and cyanuric acid residual quantity method, it is characterised in that include
Following steps：
(1) melamine and cyanuric acid standard liquid are prepared respectively, it is detected with liquid chromatograph, obtain retention time, generate
Corresponding calibration curve between peak area and concentration；
(2) take melamine cyanurate sample to be pre-processed, obtain analyze test solution, using liquid chromatograph with step
(1) test solution is detected under the same terms, obtains the testing result of the sample；
(3) calibration curve for bringing the characteristic peak peak area measured in step (2) in step (1) into, tries to achieve three in test solution
The concentration of poly cyanamid and cyanuric acid residual quantity, then calculate determination melamine cyanurate sample in melamine and cyanuric acid it is residual
Allowance；
The mobile phase that liquid chromatogram is used during detection melamine in the step (1) is ion-pairing agent cushioning liquid+acetonitrile
=83+17, v+v；The preparation of described ion-pairing agent cushioning liquid：2.10g citric acids and 2.16g perfluorooctane sulfonates are weighed,
With water dissolves, the 980mL that adds water is adjusted to pH ≈ 3, is settled to 1000mL；Mobile phase ultrasound Jing after 0.45 μm of organic membrane filtration
Process 30～40min；
The mobile phase that liquid chromatogram is used during detection cyanuric acid in the step (1) be ion-pairing agent cushioning liquid+acetonitrile=
92+8, v+v；The preparation of described ion-pairing agent cushioning liquid：Weigh 1.61g TBABs and 1.79g phosphoric acid hydrogen two
Sodium, with water dissolves, the 980mL that adds water is adjusted to pH ≈ 7.5, is settled to 1000mL；0.45 μm of organic membrane filtration of mobile phase Jing
Ultrasonically treated 30～40min afterwards；
Sample pretreatment in the step (2) is comprised the following steps：Weigh 2.0g samples to be placed in 500mL conical flasks, accurately
Measure 250mL ultra-pure waters to add in the conical flask for filling testing sample, be heated to 50 DEG C, entered with 0.45 μm of inorganic filter membrane after cooling
Row is filtered, and collects its filtrate；
Melamine standard liquid compound method is in the step (1)：Melamine standard items 0.1000g, with methyl alcohol+water=
60+40, v+v, in being settled to 100mL volumetric flasks, as standard reserving solution 1mg/mL；It is 0 μ g/ with mobile phase stepwise dilution concentration
ML, 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, 20.0 μ g/mL
Standard liquid；
Cyanuric acid standard liquid compound method is in the step (1)：Weigh cyanuric acid standard items 0.1000g, with methyl alcohol+water=
60+40, v+v, in being settled to 100mL volumetric flasks, as standard reserving solution 1mg/mL；It is 0 μ g/ with mobile phase stepwise dilution concentration
ML, 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, 80.0 μ
The standard liquid of g/mL.
2. it is according to claim 1 detection melamine cyanurate in melamine and cyanuric acid residual quantity method,
Characterized in that, detecting the liquid phase chromatogram condition of melamine in the step (1)：Flow velocity 0.8-1.0mL/min；Detection ripple
It is long：240nm；Column temperature：Room temperature；The μ L of sample size 20.
3. it is according to claim 1 detection melamine cyanurate in melamine and cyanuric acid residual quantity method,
Characterized in that, detecting the liquid phase chromatogram condition of cyanuric acid in the step (1)：Flow velocity 0.8-1.0mL/min；Detection wavelength：
220nm；Column temperature：Room temperature；The μ L of sample size 20.
4. detect the method for melamine and cyanuric acid residual quantity in melamine cyanurate in trimerization as claimed in claim 1
Application in cyanamide cyanurate in melamine and cyanuric acid qualitative and quantitative analysis.
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| CN108802236B (en) * | 2018-07-10 | 2021-05-18 | 南方医科大学 | Method for determining melamine content in dairy product |
| CN110132958B (en) * | 2019-05-09 | 2021-07-27 | 广东环凯微生物科技有限公司 | Cyanuric acid determination reagent and preparation method and application thereof |
| CN114720628A (en) * | 2022-04-07 | 2022-07-08 | 山东泰星新材料股份有限公司 | Method for determining content of free melamine in melamine cyanurate |
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| CN102924395B (en) * | 2012-10-26 | 2015-08-26 | 清远市普塞呋磷化学有限公司 | A kind of microwave process for producing crystal of high-purity melamine cyanuric acid ester |
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Address after: 250204 Luxi Luye Road, Diaozhen Chemical Park, Mingshui Economic and Technological Development Zone, Zhangqiu District, Jinan City, Shandong Province Patentee after: Shandong Taixing New Materials Co., Ltd. Address before: 250204 Luye Road West, Diaozhen Chemical Park, Zhangqiu Mingshui Economic and Technological Development Zone, Jinan City, Shandong Province Patentee before: Jinan TaiXing Fine Chemical Co., Ltd. |