CN109870520B - Method for determining benzotriazole ultraviolet stabilizer by ultra-high performance phase-combination chromatography - Google Patents
Method for determining benzotriazole ultraviolet stabilizer by ultra-high performance phase-combination chromatography Download PDFInfo
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Abstract
The invention discloses a method for determining benzotriazole ultraviolet stabilizer by ultra-efficient phase-combination chromatography, which comprises the following steps: (1) dissolving a sample to be detected in a solvent to prepare a sample solution; (2) carrying out ultra-high performance synthesis chromatography on the sample solution to obtain chromatographic analysis data, wherein the chromatographic conditions are as follows: a nonpolar chromatographic column with a system backpressure of 1900-2And isopropanol, the sample injection amount is 0.5-10 mu L, the flow rate is 0.6mL/min, and the PDA detection wavelength is 340 nm; (3) and (3) comparing the chromatographic analysis data obtained in the step (2) with the standard data of the preset benzotriazole ultraviolet stabilizer to obtain the content of the benzotriazole ultraviolet stabilizer. The method mainly uses nontoxic supercritical CO2As a mobile phase, the use amount of an organic solvent is reduced, the method is environment-friendly, and the benzotriazole ultraviolet stabilizer can be quickly and efficiently separated, so that the analysis time is saved, and the working efficiency is improved.
Description
Technical Field
The invention relates to a method for determining benzotriazole ultraviolet stabilizers, in particular to a method for determining benzotriazole ultraviolet stabilizers by ultra-high performance synthesis phase chromatography.
Background
Benzotriazole ultraviolet stabilizers (BuVSs) can absorb high-energy ultraviolet rays and convert the ultraviolet rays into low energy, play a role in protecting high polymer materials and human skin, and are widely applied to the fields of cosmetics, textiles, food contact materials, buildings and the like. However, studies have shown that some of the uv stabilizers, BUVSs, have persistence, bioaccumulation and toxicity, may destroy the endocrine system of an organism, adversely affect the reproduction and development of an organism, and may have carcinogenic effects on humans. Thus, the japanese government has placed UV-320 as the first level monitoring chemical in the "chemical control act" of 2006, products that are prohibited from ingesting UV-320; since UV-327 has a similar bioaccumulation effect as UV-320, it is also set by the Japanese government as a subject of class 1 chemical contaminant detection; the european chemical administration (ECHA) placed UV-320, UV-328 on the twelfth SVHC list in 12 months 2014 and classified it as a persistent bioaccumulation toxic.
At present, the determination methods of benzotriazole ultraviolet stabilizers mainly include ultra-High Performance Liquid Chromatography (HPLC), ultra-high performance liquid chromatography-tandem mass spectrometry (UPLC-MS/MS), gas chromatography-tandem mass spectrometry (GC-MS/MS), and the like. However, in practice, the ultra-high performance liquid chromatography and the ultra-high performance liquid chromatography-tandem mass spectrometry have long analysis time and low working efficiency, and a large amount of organic solvent is generally used as a mobile phase, which brings harm to the environment and the health of experimenters.
Disclosure of Invention
The invention aims to provide a method for determining benzotriazole ultraviolet stabilizers by ultra-high performance phase-combination chromatography. The method mainly uses nontoxic supercritical CO2As a mobile phase, the use amount of an organic solvent is reduced, the method is environment-friendly, and the benzotriazole ultraviolet can be separated quickly and efficientlyThe stabilizer saves the analysis time and improves the working efficiency.
The purpose of the invention is realized by the following technical scheme: a method for determining benzotriazole ultraviolet stabilizer by ultra-high performance synthesis chromatography comprises the following steps:
(1) dissolving a sample to be detected in a solvent to prepare a sample solution;
(2) carrying out ultra-high performance synthesis chromatography on the sample solution to obtain chromatographic analysis data, wherein the chromatographic conditions are as follows: a nonpolar chromatographic column with a system backpressure of 1900-2And isopropanol, the sample injection amount is 0.5-10 mu L, the flow rate is 0.6mL/min, and the PDA detection wavelength is 340 nm;
(3) and (3) comparing the chromatographic analysis data obtained in the step (2) with the standard data of the preset benzotriazole ultraviolet stabilizer to obtain the content of the benzotriazole ultraviolet stabilizer.
The solvent in the step (1) is acetonitrile.
Preferably, in step (2) of the present invention, the nonpolar chromatographic column is ACQUITYUPC2HSS C18SB chromatographic column, 100mm × 3.0mm,1.8 μm; system backpressure 2000 psi; the temperature of the chromatographic column is 50 ℃; the sample size was 5. mu.L.
Preferably, in step (2) of the present invention, supercritical CO is used in the mobile phase2The volume percentage of the isopropyl alcohol is 99-99.5%, and the volume percentage of the isopropyl alcohol is 0.5-1%.
The preset standard data of the benzotriazole ultraviolet stabilizer are series standard solutions of the benzotriazole ultraviolet stabilizer and are measured under the same set ultra-performance convergence chromatography condition.
The benzotriazole ultraviolet stabilizer is one or the combination of more than two of UV-327, UV-320 and UV-328.
Compared with the prior art, the invention has the beneficial effects that:
1. the method does not need to use a large amount of organic solvents, is environment-friendly, can quickly and efficiently separate the benzotriazole ultraviolet stabilizers within 3 minutes, saves analysis time and improves working efficiency.
2. Book (I)Mobile phase of invention with supercritical CO2Mainly, isopropanol is taken as a cosolvent, so that the separation efficiency of the benzotriazole ultraviolet stabilizer is effectively improved, and particularly, the three benzotriazole ultraviolet stabilizers UV-327, UV-320 and UV-328 can be effectively separated when the three benzotriazole ultraviolet stabilizers UV-327, UV-320 and UV-328 are detected simultaneously.
3. The method optimizes chromatographic conditions such as the chromatographic column, system back pressure, the chromatographic column temperature, the cosolvent, the detection wavelength and the like, greatly improves the effect of separating the three benzotriazole ultraviolet stabilizers UV-327, UV-320 and UV-328, greatly improves the efficiency of simultaneously detecting the UV-327, UV-320 and UV-328, and improves the detection efficiency.
Drawings
FIG. 1 is a chromatogram of a mixed standard solution;
1.UV-327，2.UV-320，3.UV-328；
FIG. 2 is a spectrum of UV-327, UV-320 and UV-328;
FIG. 3 is an ACQUITY UPC2Separation effect of HSS C18SB chromatographic column on ultraviolet stabilizer;
FIG. 4 is an ACQUITY UPC2The separation effect of the BEH chromatographic column on the ultraviolet stabilizer;
FIG. 5 is an ACQUITY UPC2Separation effect of CSH Fluoro-Phenyl chromatographic column on ultraviolet stabilizer;
FIG. 6 is the separation effect of column temperature 40 ℃ on UV stabilizer;
FIG. 7 is a graph of the separation effect of column temperature at 50 ℃ on UV stabilizers;
FIG. 8 is the separation effect of column temperature of 60 ℃ on UV stabilizers;
FIG. 9 is a graph of the separation effect of system back pressure 1600psi on UV stabilizer;
FIG. 10 is a graph of the separation effect of system back pressure 2000psi on UV stabilizer;
FIG. 11 is the separation effect of 0.2% isopropanol on UV stabilizer;
FIG. 12 is the separation effect of 0.5% isopropanol on UV stabilizer;
FIG. 13 is a graph of the separation effect of 1% isopropanol on UV stabilizer;
FIG. 14 is the separation effect of 0.5% methanol on UV stabilizers;
FIG. 15 is a graph of the separation effect of 1% methanol on UV stabilizers;
FIG. 16 is the separation effect of 0.5% acetonitrile on UV stabilizers;
FIG. 17 shows the effect of 1% acetonitrile on the separation of UV stabilizers.
Detailed Description
1. Reagent and apparatus
Reagent: isopropanol and acetonitrile
The instrument comprises the following steps: ultra-efficient phase-combination chromatograph: ACQUITY UPC2System, with ACQUITY UPC2PDA detector (Waters corporation of America)
2. Selection of detection wavelength
Respectively preparing benzotriazole ultraviolet stabilizers UV-327, UV-320 and UV-328 into solutions.
The test process comprises the following steps: accurately weighing 25mg to 25mL brown volumetric flasks of the UV-327, UV-320 and UV-328 standard samples respectively, and fixing the volume of acetonitrile. Then acetonitrile is used for diluting to 100mg/mL respectively, and single standard solution of 3 ultraviolet stabilizers is used for testing by an ultra-high performance phase-combination chromatograph alone. The spectrogram of the maximum absorption peak of each substance in the scanning range of 210-400 nm by using a PDA detector is shown in figure 2. The detection wavelength was 340nm, in view of the maximum absorption wavelengths of the three compounds.
3. Selection of chromatography columns
Preparing a mixed solution of benzotriazole ultraviolet stabilizers UV-327, UV-320 and UV-328.
Chromatographic conditions
And (3) system backpressure: 2000 psi; temperature of the column: 50 ℃; sample introduction amount: 5 mu L of the solution; mobile phase: supercritical CO2(100%); flow rate: 0.6 mL/min; PDA detection wavelength: 340 nm; the analysis time was 4 min.
Procedure of the test
Accurately weighing 25mg to 25mL brown volumetric flasks of the UV-327, UV-320 and UV-328 standard samples respectively, and carrying out constant volume on acetonitrile to prepare single-standard solutions of the UV-327, UV-320 and UV-328. Then transferring each single standard solution into a brown volumetric flask with 1-10 mL respectively, and adding BNitrile is diluted to constant volume to obtain a mixed standard solution. The ultra-high performance combined chromatograph selects chromatographic columns with three different stationary phases and strongly polar ACQUITY UPC2BEH column, moderately polar ACQUITY UPC2CSH Fluoro-Phenyl chromatography column and non-polar ACQUITY UPC2HSS C18SB column. And taking the mixed standard solution to perform on-machine test respectively.
From a comparison of FIGS. 3-5, it can be seen that ACQUITY UPC is obtained under the same conditions2The separation effect of HSS C18SB chromatographic column is better than that of ACQUITY UPC2BEH column and ACQUITY UPC2CSH Fluoro-Phenyl column, therefore ACQUITY UPC is used2The HSS C18SB column was subjected to further optimisation separation.
4. Optimization of chromatographic column temperature and system backpressure
Preparing a mixed solution of benzotriazole ultraviolet stabilizers UV-327, UV-320 and UV-328.
Chromatographic conditions
ACQUITY UPC2HSS C18SB column (100 mm. times.3.0 mm,1.8 μm); sample introduction amount: 5 mu L of the solution; mobile phase: supercritical CO2(100%); flow rate: 0.6 mL/min; PDA detection wavelength: 340 nm; the analysis time was 4 min.
Procedure of the test
Accurately weighing 25mg to 25mL brown volumetric flasks of UV-327, UV-320 and UV-328 standard substances respectively, and carrying out constant volume on acetonitrile to prepare single-standard solutions of UV-327, UV-320 and UV-328. And transferring 1mL to 10mL brown volumetric flasks of each single standard solution, and diluting with acetonitrile to a constant volume to obtain a mixed standard solution. The temperature parameters of the column were varied under the above chromatographic conditions with a system back pressure of 2000 psi. The mixed standard solution is taken out at the chromatographic column temperature of 40 ℃, 50 ℃ and 60 ℃ for on-machine test respectively.
The influence of the column temperature at 40 ℃, 50 ℃ and 60 ℃ on the separation effect of the three compounds was examined. In an ultra-high performance phase chromatography system, changes in column temperature can affect the density of the supercritical fluid, thereby changing its separation capacity. The temperature of the chromatographic column is increased, the density of the supercritical fluid is reduced, the solvating power is weakened, and the retention time of the target is increased; the temperature of the chromatographic column is reduced, the density of the supercritical fluid is increased, the solvating power is enhanced, and the retention time of the target is reduced. As can be seen from fig. 6-8, the retention time of the three uv stabilizers is prolonged with increasing temperature, but the latter two compounds are not separated effectively. Similarly, the density of the fluid is also affected by the change of the back pressure of the system, and the density of the supercritical fluid is increased by the increase of the back pressure of the system, so that the separation effect of the target object is affected. As can be seen from fig. 9-10, under 1600psi of system back pressure, the retention time of the target is prolonged, and the time of the target completely peaking reaches about 9 minutes, whereas under 2000psi of system back pressure, the target can completely peak in only 4 minutes, but the change of system back pressure still can not separate the target effectively. Comprehensively considering, the conditions of 50 ℃ chromatographic column temperature and 2000psi system backpressure are selected to further optimize other parameter conditions.
5. Optimization of co-solvents
Preparing a mixed solution of benzotriazole ultraviolet stabilizers UV-327, UV-320 and UV-328.
The chromatographic conditions are as follows: ACQUITY UPC2HSS C18SB column (100 mm. times.3.0 mm,1.8 μm); and (3) system backpressure: 2000 psi; temperature of the column: 50 ℃; sample introduction amount: 5 mu L of the solution; flow rate: 0.6 mL/min; PDA detection wavelength: 340 nm; the analysis time was 4 min.
The test process comprises the following steps: accurately weighing 25mg to 25mL brown volumetric flasks of the UV-327, UV-320 and UV-328 standard samples respectively, and carrying out constant volume on acetonitrile to prepare single-standard solutions of the UV-327, UV-320 and UV-328. And transferring 1mL to 10mL brown volumetric flasks of each single standard solution, and diluting with acetonitrile to a constant volume to obtain a mixed standard solution. And (3) changing the types and the proportions of the cosolvents according to the chromatographic conditions, and taking the mixed standard solution to perform on-machine test respectively.
The addition of the organic solvent plays an important role in the separation effect of the target in the system. The organic solvent has different influences on the retention behavior of the target object due to different polarities and elution capacities. The organic solvent is added as a cosolvent, and the separation effect of the target substance is influenced by the different proportion of the organic solvent to the supercritical carbon dioxide. The influence of three common organic reagents with different polarities on the separation effect of the target object is examined according to the proportion conditions of 0.2 percent of isopropanol, 0.5 percent of isopropanol, 1 percent of isopropanol, 0.5 percent of methanol, 1 percent of methanol, 0.5 percent of acetonitrile and 1 percent of acetonitrile. As can be seen from FIGS. 11-17, 0.5% isopropanol as a co-solvent gave the best separation, effective in separating UV-327, UV-320 and UV-328.
6. Linear range, detection limit, recovery and precision
Respectively weighing 50mg of each of 3 ultraviolet stabilizers UV-327, UV-320 and UV-328 in a 50mL volumetric flask, dissolving with acetonitrile, fixing the volume, preparing into standard stock solution, and storing at-4 ℃ in dark place. The stock solutions were prepared into a series of standard working solutions with concentrations of 0.5, 1, 2, 5, 10, 25, 50. mu.g/mL. The concentration is plotted on the abscissa and the response value is plotted on the ordinate, and the results are shown in Table 1. The correlation coefficient of the three compounds is more than 0.995 in the range of 0.5-50 mu g/mL, and the linearity is good. The signal to noise ratio is more than or equal to 3 as the detection Limit (LOD), and the detection limit of each substance is shown in Table 1.
Chromatographic conditions
A chromatographic column: ACQUITY UPC2HSS C18SB column (100 mm. times.3.0 mm,1.8 μm);
and (3) system backpressure: 2000 psi;
temperature of the column: 50 ℃;
sample introduction amount: 5 mu L of the solution;
mobile phase: supercritical CO299.5% and isopropanol 0.5%;
flow rate: 0.6 mL/min;
PDA detection wavelength: 340 nm.
TABLE 1 Linear Range and detection limits
The samples were injected 7 times in succession with solutions of known concentration, and the results of recovery and precision are given in Table 2. As can be seen from Table 2, the method has accurate results and good precision.
TABLE 2 recovery and precision
7. Comparative example
The method is rapid, efficient, green and environment-friendly, can realize effective separation of three ultraviolet stabilizers within 3min, and avoids using a large amount of organic solvents.
Because the standard of a measuring method of the benzotriazole ultraviolet stabilizer is lacked at home at present, compared with the published measuring method of the benzotriazole ultraviolet stabilizer, the comparison result is shown in the following table (the analysis time is calculated by the latest retention time of 3 benzotriazole ultraviolet stabilizers). As can be seen from the table, supercritical CO was used2The method is a mobile phase, is friendly to the environment and human health, has extremely short analysis time and improves the working efficiency.
TABLE 34 analysis time comparison of methods
GC-MS/MS reference: wangchengyun, Shegantang, Tanglichun, et al, the content of 6 benzotriazole ultraviolet absorbers [ J ] in the textile was simultaneously determined by ultrasonic extraction gas chromatography-tandem mass spectrometry, the industrial textile, 2016,34 (8).
HPLC method reference: zhao ocean wave, Xuhong, Hanning, etc. ultrasonic extraction-HPLC method to determine 4 benzotriazole ultraviolet absorbers [ J ] and printing and dyeing, 2017(8): 46-51.
UPLC-MS/MS reference: the method comprises the steps of determining 4 benzotriazole ultraviolet stabilizers in the textile simultaneously by ultra-high performance liquid chromatography-tandem mass spectrometry, and the like, wherein 2016,35(4) is adopted as an analytical test report, and 414-419 is adopted.
The above examples are some embodiments of the present invention, and are not intended to limit the present invention. It will be apparent to those skilled in the art that various modifications and variations can be made without departing from the principles of the invention.
Claims (4)
1. A method for determining benzotriazole ultraviolet stabilizer by ultra-high performance synthesis chromatography is characterized by comprising the following steps:
(1) dissolving a sample to be detected in a solvent to prepare a sample solution;
(2) carrying out ultra-high performance synthesis chromatography on the sample solution to obtain chromatographic analysis data, wherein the chromatographic conditions are as follows: a nonpolar chromatographic column with a system backpressure of 1900-2And isopropanol, supercritical CO2The volume percentage of the sample is 99-99.5%, the volume percentage of the isopropanol is 0.5-1%, the sample amount is 0.5-10 mu L, the flow rate is 0.6mL/min, and the PDA detection wavelength is 340 nm; the nonpolar chromatographic column is ACQUITY UPC2HSS C18SB chromatography column;
(3) comparing the chromatographic analysis data obtained in the step (2) with the standard data of the preset benzotriazole ultraviolet stabilizer to obtain the content of the benzotriazole ultraviolet stabilizer; the benzotriazole ultraviolet stabilizer is UV-327, UV-320 or UV-328.
2. The method for determining the benzotriazole ultraviolet stabilizer by ultra-high performance phase-combination chromatography according to claim 1, wherein the solvent in the step (1) is acetonitrile.
3. The method for determining benzotriazole ultraviolet stabilizer by ultra-high performance phase-combination chromatography as claimed in claim 1, wherein in the step (2), ACQUITY UPC2HSC 18SB chromatographic column of 100mm × 3.0mm,1.8 μm; system backpressure 2000 psi; the temperature of the chromatographic column is 50 ℃; the sample size was 5. mu.L.
4. The method for determining the benzotriazole ultraviolet stabilizer by the ultra-high performance phase-combination chromatography method according to claim 1, wherein the predetermined standard data of the benzotriazole ultraviolet stabilizer is a series of standard solutions of the benzotriazole ultraviolet stabilizer, and the standard data are measured under the same set ultra-high performance phase-combination chromatography conditions.
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Citations (3)
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| JP2002372516A (en) * | 2001-06-15 | 2002-12-26 | Shimadzu Corp | Liquid chromatographic mass spectrometer |
| CN106033082A (en) * | 2015-03-12 | 2016-10-19 | 谱尼测试集团上海有限公司 | Detection method for four benzotriazole ultraviolet absorbers in plastics and related products |
| CN109212073A (en) * | 2018-09-26 | 2019-01-15 | 胡贝贞 | The extraction and measuring method of 4 kinds of benzotriazole ultra-violet stabilizer residual quantities in dyeing waste water |
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Patent Citations (3)
| Publication number | Priority date | Publication date | Assignee | Title |
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| JP2002372516A (en) * | 2001-06-15 | 2002-12-26 | Shimadzu Corp | Liquid chromatographic mass spectrometer |
| CN106033082A (en) * | 2015-03-12 | 2016-10-19 | 谱尼测试集团上海有限公司 | Detection method for four benzotriazole ultraviolet absorbers in plastics and related products |
| CN109212073A (en) * | 2018-09-26 | 2019-01-15 | 胡贝贞 | The extraction and measuring method of 4 kinds of benzotriazole ultra-violet stabilizer residual quantities in dyeing waste water |
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| Development of an achiral supercritical fluid chromatography method with ultraviolet absorbance and mass spectrometric detection for impurity profiling of drug candidates. Part II. Selection of an orthogonal set of stationary phases;Elise Lemasson 等;《Journal of Chromatography A》;20150821;第1408卷;第217-226页 * |
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