CN104991021A - Hindered amine light stabilizer mass control and/or identification detection method - Google Patents
Hindered amine light stabilizer mass control and/or identification detection method Download PDFInfo
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- CN104991021A CN104991021A CN201510388138.8A CN201510388138A CN104991021A CN 104991021 A CN104991021 A CN 104991021A CN 201510388138 A CN201510388138 A CN 201510388138A CN 104991021 A CN104991021 A CN 104991021A
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Abstract
The invention discloses a separation and analysis method based on non-aqueous reverse-phase gradient liquid chromatography. Methanol, dichloromethane and triethylamine are taken as mobile phases, a gradient elution mode is adopted, circular and linear oligomers and homologs thereof of a Chimassorb 944 product are separated for the first time, and the molecular weight of the Chimassorb 944 product is identified through MALDI-TOF; by combining with the synthetic route of the Chimassorb 944 product, it is determined that chromatographic peaks of a liquid chromatogram stand for different types of the oligomers with the molecular weights with one constitutional unit deviation and the homologs thereof, attribution is conducted on the peaks, and an effective detection method for the mass control of the Chimassorb 944 product is provided. According to the hindered amine light stabilizer mass control and/or identification detection method, instruments used in the method adopt an ordinary reverse-phase chromatographic system, the operability is strong, and important economic value is achieved by applying the method to the measurement and the product mass control of the Chimassorb 944 product.
Description
Technical field
The present invention relates to a kind of light stabilizer method of quality control, be specifically related to a kind of Testing and appraisal method of hindered amine type light stabilizer Chimassorb 944 production quality control.
Background technology
Light stabilizer be a kind of can suppress or slow down plastic products to cause because of illumination variable color or the auxiliary agent of degraded.Effectively can improve light fastness and the antioxygenic property of plastic products, extend its serviceable life.Chimassorb 944 product is that a class is obstructed the light stabilizer of amine type, have volatility low, thermal stability is high, the advantage good with resin compatibility, be not easy to again simultaneously migration, anti-extracting good, use nonirritant, plastics easy-formation, be the light stabilizer of a class superior performance.
At present, document is disclosed to be mainly contained the detection method of Chimassorb 944 product: volume exclusion liquid phase chromatography that the people such as Gharfeh propose [see: J.Chromatogr.389 (1987) 211-218], by the molecular weight detecting polymkeric substance, quality control is carried out to it, and reversed phase liquid chromatography [see: J.Chromatogr.450 (1988) 430-432].The subject matter of these two kinds of methods is that resolution is low, and the potpourri of multiple oligomer by co-elute, cannot tell single oligomer composition with broad peak.The people such as Troues are filled capillary pipe technology separation Chimassorb 944 product that heats up of service routine first, obtains about 40 kinds of single oligomer composition [see J.Chromatogr.A 874 (2000) 65-71].Although his method has potential using value, be limited by the restriction of instrument condition, cannot promote the use of in plastic products enterprise.The people such as nearest Reisinger [see: Anal.Chim.Acta 803 (2013) 181-187 reports a kind of method adopting traditional reverse-phase chromatography modal cutoff Chimassorb 944 product, but its chromatographic condition but cannot realize detecting to the oligomer more than 3 repetitives.
Therefore, need to seek more efficiently method, quality control is carried out to hindered amine type light stabilizer 944.
Summary of the invention
For overcoming defect of the prior art, the invention provides a kind of method for separating and analyzing based on non-water reverse phase gradient liquid chromatography, with methyl alcohol, methylene chloride, triethylamine is mobile phase, adopt the pattern of gradient elution, ring-type in Chimassorb 944 product is separated with linear oligomers and homolog thereof, and identify its molecular weight by MALDI-TOF, in conjunction with the synthetic route of Chimassorb 944 product, the chromatographic peak determined in liquid chromatogram is dissimilar oligomer and the homolog thereof of a mass difference structural unit, each peak is belonged to, production quality control for Chimassorb 944 provides effective detection method.
Thus, the invention provides the separation method of ring-type and linear oligomers and homolog thereof in a kind of Chimassorb 944 product, comprise and adopt non-water reverse phase gradient liquid chromatography to be separated with linear oligomers and homolog thereof the ring-type in Chimassorb 944 product, and with mass spectrum, separation component is identified.
In Chimassorb 944 product of the present invention, ring-type and linear oligomers and homolog thereof are selected from A
nseries oligomer, B
nseries oligomer, C
nseries oligomer, D
none or more combination in series oligomer.Wherein, n value is repetitive structure unit number.Preferably, n is the integer of 1-26, and n can be 1,2,3,4,5,6,7,8,9,10,11,12,13,14,15,16,17,18,19,20,21,22,23,24,25,26.
A of the present invention
nseries oligomer has following structure:
B of the present invention
nseries oligomer has following structure:
C of the present invention
nseries oligomer has following structure:
D of the present invention
nseries oligomer has following structure:
In a specific embodiment of the present invention, in described Chimassorb 944 product, ring-type and linear oligomers and homolog thereof comprise A
nseries oligomer, C
nseries oligomer and D
nseries oligomer.In another preferred embodiment of the present invention, in described Chimassorb 944 product, ring-type and linear oligomers and homolog thereof comprise A
nseries oligomer, B
nseries oligomer, C
nseries oligomer and D
nseries oligomer.
Highly preferred, A in the present invention
nseries oligomer comprises A
1, A
2, A
3, A
4, A
5, A
6, A
7, A
8, A
9, A
10, A
11, A
12, A
13, A
14, A
15, A
16, A
17, A
18, A
19, A
20, A
21, A
22, A
23, A
24, A
25and/or A
26; C
nseries oligomer comprises C
1, C
2, C
3, C
4and/or C
5; D
nseries oligomer comprises D
1, D
2, D
3, D
4, D
5and/or D
6.
In a specific embodiment of the present invention, the chromatographic column of described liquid chromatography is carbon octadecyl silane filler chromatographic column.
In a specific embodiment of the present invention, the mobile phase of described liquid chromatography is methyl alcohol and methylene chloride.Preferably, also containing triethylamine in the mobile phase of liquid chromatography of the present invention.Preferably, it is 0.1%-2% that described triethylamine addition accounts for methylene chloride total volume percent, preferred, and it is 1% that described triethylamine addition accounts for methylene chloride total volume percent.
In a specific embodiment of the present invention, described liquid chromatography adopts the mode of gradient elution.Preferred, described mobile phase is A methyl alcohol, and B methylene chloride and 1% triethylamine, and described gradient is: during 0-60min B by volume number percent be 10%-40%; During 60-70min B by volume number percent be 40%; During 70-75min B by volume number percent be 40%-10% wash-out.
In a specific embodiment of the present invention, the column temperature of described liquid chromatography is 25-60 DEG C, is preferably 30-40 DEG C, is more preferably 30 DEG C.
In a specific embodiment of the present invention, the flow velocity of described liquid chromatography is 1.0mL/min.
In a specific embodiment of the present invention, the detecting device of described liquid chromatography is UV-detector.
In a specific embodiment of the present invention, the determined wavelength of described liquid chromatography is 240-250nm, is preferably 245nm.
In a specific embodiment of the present invention, described liquid chromatography and MALDI-TOF mass spectrometry.
In a specific embodiment of the present invention, described sample is configured to solution, comprising: get after Chimassorb 944 product methylene chloride dissolves and cross 0.45m filter membrane.
The present invention provides a kind of hindered amine type light stabilizer Chimassorb 944 product quality control method, detection method and/or authentication method on the other hand, comprising:
(1) non-water reverse phase gradient liquid chromatography is adopted to be separated with linear oligomers and homolog thereof the ring-type in Chimassorb 944 product;
(2) product after step (1) being separated detects, and detects Chimassorb 944 product and/or identifies.
In described step (1), in Chimassorb 944 product, ring-type and linear oligomers and homolog thereof are selected from A
nseries oligomer, B
nseries oligomer, C
nseries oligomer, D
none or more combination in series oligomer.Wherein n value is repetitive structure unit number.Preferably, n is the integer of 1-26, and n can be 1,2,3,4,5,6,7,8,9,10,11,12,13,14,15,16,17,18,19,20,21,22,23,24,25,26.
In described step (1), in described Chimassorb 944 product, ring-type and linear oligomers and homolog thereof comprise A
nseries oligomer, C
nseries oligomer and D
nseries oligomer.In another preferred embodiment of the present invention, in described Chimassorb 944 product, ring-type and linear oligomers and homolog thereof comprise A
nseries oligomer, B
nseries oligomer, C
nseries oligomer and D
nseries oligomer.Highly preferred, A
nseries oligomer comprises A
1, A
2, A
3, A
4, A
5, A
6, A
7, A
8, A
9, A
10, A
11, A
12, A
13, A
14, A
15, A
16, A
17, A
18, A
19, A
20, A
21, A
22, A
23, A
24, A
25and/or A
26; C
nseries oligomer comprises C
1, C
2, C
3, C
4and/or C
5; D
nseries oligomer comprises D
1, D
2, D
3, D
4, D
5and/or D
6.
In described step (1), the chromatographic column of described liquid chromatography is carbon octadecyl silane filler chromatographic column.
In described step (1), the mobile phase of described liquid chromatography is methyl alcohol and methylene chloride.Preferably, also containing triethylamine in the mobile phase of liquid chromatography of the present invention.Preferably, it is 0.1%-2% that described triethylamine addition accounts for methylene chloride total volume percent, preferred, and it is 1% that described triethylamine addition accounts for methylene chloride total volume percent.
In described step (1), described liquid chromatography adopts the mode of gradient elution.Preferred, described mobile phase is A methyl alcohol, and B methylene chloride and 1% triethylamine, and described gradient is: during 0-60min B by volume number percent be 10%-40%; During 60-70min B by volume number percent be 40%; During 70-75min B by volume number percent be 40%-10% wash-out.
In described step (1), the column temperature of described liquid chromatography is 25-60 DEG C, is preferably 30-40 DEG C, is more preferably 30 DEG C.
In described step (1), the flow velocity of described liquid chromatography is 1.0mL/min.
In described step (1), described sample is configured to solution, comprising: get after Chimassorb 944 product methylene chloride dissolves and cross 0.45m filter membrane.
In described step (2), described detection adopts UV-detector.Preferably, described determined wavelength is 240-250nm, is preferably 245nm.
In described step (2), described detection also comprises the Structural Identification adopting MALDI-TOF to carry out product.
In described step (2), also comprise the step of testing result and reference substance being compared.Preferably, described comparison comprises qualitative and/or quantitative comparison.
The collocation method of described reference substance comprises: take Chimassorb 944 product reference substance appropriate, in a certain amount of solvent, powerful jolting off and on, observes the dissolving situation in 5 minutes, as without visual visible particles of solute, is namely considered as dissolving completely.Preferably, the collocation method of described reference substance comprises: get 1.0g Chimassorb 944 product reference substance and be placed in 10mL volumetric flask, use dissolution with solvents constant volume, obtain the sample solution of 100mg/mL, crosses 0.45m, and filtering membrane uses.Described solvent is selected from water, methyl alcohol, ethanol, acetone, one or more the combination in methylene chloride, and preferably, described solvent is selected from methylene chloride.
In a specific embodiment of the present invention, described hindered amine type light stabilizer Chimassorb 944 product quality control method, detection method and/or authentication method, comprise
Get appropriate Chimassorb 944 product and be placed in 10mL volumetric flask, with certain dissolution with solvents constant volume, obtain the sample solution of 100mg/mL, cross 0.45m filter membrane and use.
Use high performance liquid chromatograph, UV-detector, high performance liquid chromatography and MALDI-TOF mass spectrometry, chromatographic work station, each step adopts following chromatographic condition:
Chromatographic column: carbon octadecyl silane filler chromatographic column;
Column temperature: 30-50 DEG C;
Mobile phase: A methyl alcohol, and B methylene chloride and 1% triethylamine, during 0-60min B by volume number percent be 10%-40%; During 60-70min B by volume number percent be 40%; During 70-75min B by volume number percent be 40%-10% wash-out;
Flow velocity: 1.0mL/min;
Determined wavelength: 240-250nm;
Chimassorb 944 product of the present invention is formed by dichloro diazine and own piperidines diamines, and the oligomer in its product can be divided into A, B, C, D tetra-kinds by structure and composition, and its structure and molecular weight general formula are as shown in Figure 1.A series is linear diamine structures, and B series is linear dichloro structure, and C series is ring texture, and D series is the linear structure obtained by B Series of Water solution.The structural unit that molecular weight is 598.96 is differed between the homolog of various oligomer.
In separation method of the present invention, be separated the number 40 of chromatographic peak of afterproduct nearly, be preferably greater than 30, be preferredly greater than 40.Due to after elution time 55min, some less peaks are also had to occur, so be not limited to 40 by the chromatographic peak eluted.In order to carry out structural confirmation to eluting peak, MALDI-TOF is adopted to identify, in conjunction with the m/z at each peak, to A
n, B
n, C
n, D
nthe molecular weight of series oligomer carries out peak ownership.The homolog that m/z can be differed the A series oligomer of 598.96 by the method for gradient liquid chromatography that the present invention sets up is separated completely.
Because technique scheme is used, the present invention compared with prior art has following advantages:
(1) method for separating and analyzing based on non-water reverse phase gradient liquid chromatography provided by the invention, with methyl alcohol, methylene chloride, triethylamine for mobile phase, adopt the pattern of gradient elution, first the ring-type in Chimassorb944 product is separated with linear oligomers and homolog thereof, and by mass spectrum, its molecular weight is identified
(2) the present invention is in conjunction with the synthetic route of Chimassorb 944 product, the chromatographic peak determined in liquid chromatogram is dissimilar oligomer and the homolog thereof of a mass difference structural unit, belong to each peak, the production quality control for Chimassorb 944 provides more meticulous effective detection method.Fill up the vacancy of domestic and international coherent detection.
(3) instrument used in the present invention is common Reversed-phase Chromatographic System, workable, this kind of method is used for mensuration and the production quality control of Chimassorb 944 product, has important economic worth.
Accompanying drawing explanation
The structure type of oligomer and molecular weight in Fig. 1 Chimassorb 944 product.
Wherein, A series represents A
nseries oligomer, its molecular weight is Mw=394.68+598.96n; B series represents B
nseries oligomer, its molecular weight is Mw=277.19+598.96n; C series represents C
nseries oligomer, its molecular weight is Mw=598.96n; D series represents D
nseries oligomer, its molecular weight is Mw=258.75+598.96n.
The separate colors spectrogram of Fig. 2 Chimassorb 944 product.A
nrepresent A series oligomer; B
nrepresent B series oligomer; C
nrepresent C series oligomer; D
nrepresent D series oligomer.N value is repetitive structure unit number.The oblique line of below is the blank of gradient liquid phase; Inset portion is the enlarged drawing in high-quality number region.
The uv absorption chromatogram of Fig. 3 Chimassorb 944 product.
Fig. 4 mobile phase adds the chromatogram that different amount removes Chimassorb 944 product when trailing agent triethylamine.
The separate colors spectrogram of Fig. 5 Chimassorb 944 product under the column temperature of 30,60 DEG C compares.
The direct mass spectrogram of Fig. 6 Chimassorb 944 product
Fig. 7 embodiment 1Chimassorb 944 separation of products chromatogram.
Fig. 8 embodiment 2Chimassorb 944 separation of products chromatogram.
Embodiment
Below in conjunction with embodiment, the invention will be further described, but these embodiments are not to be construed as limiting the scope of the invention.
Experimental apparatus is in the examples below: Waters 600 high performance liquid chromatograph, comprises quaternary gradient pump, column oven, Waters 484 UV-detector, Rheodyne 7125 manual injector, N2000 chromatographic work station.Brooker Autoflex III MALDI-TOF mass spectrometer, is configured to binary pump; Nd:YAG laser instrument, operation wavelength 355nm; Ionogenic delay extraction.
Chromatographic condition is:
Chromatographic column: carbon octadecyl silane filler chromatographic column;
Column temperature: 30 DEG C;
Mobile phase: methyl alcohol (A)-methylene chloride+1% triethylamine (B), gradient: 0 ~ 60min, 10% ~ 40%B; 60 ~ 70min, 40%B; 70 ~ 75min, 40% ~ 10%B wash-out;
Flow velocity: 1.0mL/min;
Determined wavelength: 245nm;
Embodiment 1
The Testing and appraisal method of Chimassorb 944 production quality control:
1. the configuration of sample solution: take Chimassorb 944 product reference substance appropriate, (water in a certain amount of solvent, methyl alcohol, ethanol, acetone, methylene chloride), powerful jolting off and on, observe the dissolving situation in 5 minutes, as without visual visible particles of solute, be namely considered as dissolving completely.Experiment finds that Chimassorb 944 product solubleness in methylene chloride is best, gets 1.0g Chimassorb944 product reference substance and is placed in 10mL volumetric flask, dissolve constant volume, obtain the sample solution of 100mg/mL with methylene chloride, crosses 0.45m filter membrane and uses.
The optimization of 2.HPLC chromatographiccondition:
The selection of 2.1 uv absorption wavelength
As shown in Figure 3, in 200 ~ 400nm wavelength, it has absorption maximum at 233nm place to the ultraviolet spectrum data of Chimassorb 944 product product, is the typical absorption wavelength of piperidine ring in structure.Meanwhile, the mobile phase of use is methyl alcohol, the potpourri of methylene chloride and triethylamine, and the cutoff wavelength of triethylamine is less than 200nm, and its content is little, can leave out of consideration; The cutoff wavelength of methyl alcohol is 205nm, and the cutoff wavelength of methylene chloride is 235nm.Employing the gradient elution program of long period in the present invention, in order to reduce the baseline wander produced because of solvent change, selecting 240-250nm as mensuration wavelength.
2.2 investigations of going to trail agent addition
In Chimassorb 944 product structure, cause alkalescence very high due to the existence of a large amount of nitrogenous base, and in conventional silica matrix chromatogram post remaining many silicone hydroxyl, nitrogen-containing group can be combined with each other with silicone hydroxyl when flowing through chromatographic column and cause wash-out difficulty, affect degree of separation and peak shape, so when detecting alkaline matter, need in mobile phase, add hangover agent.Go hangover agent just to combine with remaining silicone hydroxyl before sample enters chromatographic column, site taken, then after basic sample solution enters chromatographic column would not disturb by the suction-operated of silicone hydroxyl.What liquid phase was conventional goes hangover agent to be triethylamine, adds in methylene chloride, the B component using mixed liquor as gradient elution mobile phase in the present invention by triethylamine.Investigated the impact that triethylamine addition is separated chromatographic peak when to account for methylene chloride total amount number percent be respectively 0.1%, 0.3%, 0.5%, 1% and 2%, the spectrogram obtained as shown in Figure 4.Can clearly carry out contrast to obtain from figure, when triethylamine addition increases to 1% from 0.1%, each chromatographic peak separation case in Chimassorb 944 product mixture is tending towards good gradually, and peak shape is symmetrical, when it increases to 2% again, separating effect change is little, this represents when going hangover agent triethylamine addition to be 1%, silanol base binding site in silica matrix chromatogram post can be taken, be equivalent to carry out end-blocking again to chromatograph packing material, now basic sample solution enters chromatographic column again and with silica matrix, too much suction-operated would not occur again.
The investigation of 2.3 column temperatures
In liquid chromatography, when the sample for macromolecular compound is analyzed, column temperature generally need higher than room temperature.In the literature, researcher's mode that service routine heats up in filled capillary pipe column liquid chromatographic replaces gradient elution, and for the analysis of Chimassrob944 product, visible column temperature can produce larger impact to the chromatographic behavior of sample.In invention, employ gradient elution mode, control column temperature constant simultaneously.The separation case of sample when being respectively 30 DEG C and ultimate value 60 DEG C by investigating column temperature, as shown in Figure 5, find high column temperature and be unfavorable for the separation of each oligomer in Chimassrob944 product, this may be because the mobile phase methanol used, methylene chloride are organic phase, and the reason that methylene chloride boiling point (40 DEG C) is lower.
The mass spectrum checking of 3.Chimassorb 944 product
In the chromatographic peak obtained in order to the gradient liquid chromatography analytical approach seeking above-mentioned foundation and Chimassorb 944 product product oligomer form between relation, the present invention adopts MALDI-TOF to carry out Structural Identification to it.Mass spectrophotometry condition: using DHB (DHB) as mixing sample matrix, is configured to the acetonitrile-aqueous solution (3: 1, v/v adds the acetic acid of 0.1%) that concentration is 12mg/mL by DHB.
Get 1L above-mentioned Chimassorb 944 product solution and the above-mentioned DHB solution of 1L respectively, mixed liquor is added drop-wise on MALDI dish, air oxygen detrition.Positive ion mode, accelerating potential is 20kv, and time delay is 100ns.The sweep limit of LC-MS is 500-4250m/z, and direct mass spectrographic sweep limit expands to 11000m/z.As shown in Figure 6, visible Chimassorb 944 product forms, by a series of from A primarily of the oligomer of category-A type for gained mass spectrogram and ownership
1~ A
13the homolog composition of even longer strand, and the oligomer of visible a small amount of C and D type, the oligomer of category-B type is because content is very low, and its signal that dissociates is suppressed, does not therefore detect in direct mass spectrum.By carrying out Mass Spectrometer Method by after the efflux Fractional Collections of liquid chromatography, the existence of the category-B type oligomer of lower content still can be detected.
In this embodiment, Chimassorb 944 product is provided by Beijin Tiangang Auxiliary Co., Ltd..
3 experimental results
By Chimassorb 944 product solution sample introduction 20L, carry out liquid-phase chromatographic analysis, 70 minutes writing times, the results are shown in Figure 7.
Embodiment 2
The Testing and appraisal method of Chimassorb 944 production quality control of separate sources:
Get Chimassorb 944 product being purchased from country variant, its experimental procedure is identical with embodiment 1, the results are shown in Figure 8.From result, the composition of method to this product that the present invention sets up gives more details, can provide data more reliably, be applicable to very much being applied to the mensuration to Chimassorb 944 product and quality control in the contrast of like product.
Above-described embodiment does not limit the present invention in any way, and the technical scheme that the mode that every employing is equal to replacement or equivalent transformation obtains all drops in protection scope of the present invention.
Claims (10)
1. the separation method of ring-type and linear oligomers and homolog thereof in Chimassorb 944 product, it is characterized in that, non-water reverse phase gradient liquid chromatography is adopted to be separated with linear oligomers and homolog thereof the ring-type in Chimassorb 944 product, the chromatographic column of described liquid chromatography is carbon octadecyl silane filler chromatographic column, and the mobile phase of described liquid chromatography is methyl alcohol, methylene chloride and to account for methylene chloride total volume percent be 0.1-2% triethylamine.
2. the separation method of ring-type and linear oligomers and homolog thereof in a kind of Chimassorb 944 product according to claim 1, it is characterized in that, the mode of the employing gradient elution of described liquid chromatography, mobile phase is A methyl alcohol, and B methylene chloride and to account for methylene chloride total volume percent be 0.1-2% triethylamine, described gradient is: during 0-60min B by volume number percent be 10%-40%; During 60-70min B by volume number percent be 40%; During 70-75min B by volume number percent be 40%-10% wash-out; The column temperature of described liquid chromatography is 25-60 DEG C, is preferably 30-40 DEG C, is more preferably 30 DEG C.
3. the separation method of ring-type and linear oligomers and homolog thereof in a kind of Chimassorb 944 product according to claim 1, it is characterized in that, the flow velocity of described liquid chromatography is 1.0mL/min.
4. in a kind of Chimassorb 944 product described in claim 1-3 Arbitrary Term, the separation method of ring-type and linear oligomers and homolog thereof, is characterized in that, in described Chimassorb 944 product, ring-type and linear oligomers and homolog thereof are selected from A
nseries oligomer, B
nseries oligomer, C
nseries oligomer, D
none or more combination in series oligomer, wherein, n value is repetitive structure unit number;
Described A
nseries oligomer has following structure:
Described B
nseries oligomer has following structure:
Described C
nseries oligomer has following structure:
Described D
nseries oligomer has following structure:
5. the method for quality control of hindered amine type light stabilizer Chimassorb 944 product, detection method and/or an authentication method, is characterized in that, comprise the following steps:
(1) non-water reverse phase gradient liquid chromatography is adopted to be separated with linear oligomers and homolog thereof the ring-type in Chimassorb 944 product;
(2) product after step (1) being separated detects, and detects Chimassorb 944 product and/or identifies;
In described step (1), the chromatographic column of liquid chromatography is carbon octadecyl silane filler chromatographic column, and the mobile phase of liquid chromatography is methyl alcohol, methylene chloride and to account for methylene chloride total volume percent be 0.1-2% triethylamine.
6. the method for quality control of a kind of hindered amine type light stabilizer Chimassorb 944 product according to claim 5, detection method and/or authentication method, it is characterized in that, in described step (1), the mode of the employing gradient elution of liquid chromatography, mobile phase is A methyl alcohol, and B methylene chloride and to account for methylene chloride total volume percent be 0.1-2% triethylamine, described gradient is: during 0-60min B by volume number percent be 10%-40%; During 60-70min B by volume number percent be 40%; During 70-75min B by volume number percent be 40%-10% wash-out; The column temperature of liquid chromatography is 25-60 DEG C, and be preferably 30-40 DEG C, be more preferably 30 DEG C, the flow velocity of liquid chromatography is 1.0mL/min.
7. the method for quality control of a kind of hindered amine type light stabilizer Chimassorb 944 product according to claim 5, detection method and/or authentication method, it is characterized in that, in described Chimassorb 944 product, ring-type and linear oligomers and homolog thereof are selected from A
nseries oligomer, B
nseries oligomer, C
nseries oligomer, D
none or more combination in series oligomer, wherein, n value is repetitive structure unit number;
Described A
nseries oligomer has following structure:
Described B
nseries oligomer has following structure:
Described C
nseries oligomer has following structure:
Described D
nseries oligomer has following structure:
8. the method for quality control of a kind of hindered amine type light stabilizer Chimassorb 944 product according to claim 5, detection method and/or authentication method, is characterized in that, A
nseries oligomer comprises A
1, A
2, A
3, A
4, A
5, A
6, A
7, A
8, A
9, A
10, A
11, A
12, A
13, A
14, A
15, A
16, A
17, A
18, A
19, A
20, A
21, A
22, A
23, A
24, A
25and/or A
26; C
nseries oligomer comprises C
1, C
2, C
3, C
4and/or C
5; D
nseries oligomer comprises D
1, D
2, D
3, D
4, D
5and/or D
6.
9. the method for quality control of a kind of hindered amine type light stabilizer Chimassorb 944 product described in claim 5-8 any one, detection method and/or authentication method, it is characterized in that, in described step (2), described detection adopts UV-detector, described determined wavelength is 240-250nm, is preferably 245nm.
10. the method for quality control of a kind of hindered amine type light stabilizer Chimassorb 944 product described in claim 5-8 any one, detection method and/or authentication method, it is characterized in that, in described step (2), also comprise the step of testing result and reference substance being compared.
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Cited By (4)
| Publication number | Priority date | Publication date | Assignee | Title |
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| CN110392829A (en) * | 2017-03-16 | 2019-10-29 | 百特基公司 | Quality guiding separation |
| CN113848274A (en) * | 2021-07-30 | 2021-12-28 | 中国科学院宁波材料技术与工程研究所 | Method for measuring light stabilizer UV119 in leather material |
| CN115078595A (en) * | 2022-08-04 | 2022-09-20 | 山东京博石油化工有限公司 | Method for detecting multiple hindered amine light stabilizer components in polyolefin product |
| CN113848274B (en) * | 2021-07-30 | 2024-05-31 | 中国科学院宁波材料技术与工程研究所 | Determination method of light stabilizer UV119 in leather material |
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Cited By (5)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN110392829A (en) * | 2017-03-16 | 2019-10-29 | 百特基公司 | Quality guiding separation |
| CN113848274A (en) * | 2021-07-30 | 2021-12-28 | 中国科学院宁波材料技术与工程研究所 | Method for measuring light stabilizer UV119 in leather material |
| CN113848274B (en) * | 2021-07-30 | 2024-05-31 | 中国科学院宁波材料技术与工程研究所 | Determination method of light stabilizer UV119 in leather material |
| CN115078595A (en) * | 2022-08-04 | 2022-09-20 | 山东京博石油化工有限公司 | Method for detecting multiple hindered amine light stabilizer components in polyolefin product |
| CN115078595B (en) * | 2022-08-04 | 2024-05-31 | 山东京博石油化工有限公司 | Detection method for multiple hindered amine light stabilizer components in polyolefin product |
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