CN106198830A - A kind of method of liquid chromatographic detection three monomer - Google Patents
A kind of method of liquid chromatographic detection three monomer Download PDFInfo
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- CN106198830A CN106198830A CN201610556742.1A CN201610556742A CN106198830A CN 106198830 A CN106198830 A CN 106198830A CN 201610556742 A CN201610556742 A CN 201610556742A CN 106198830 A CN106198830 A CN 106198830A
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- G01N—INVESTIGATING OR ANALYSING MATERIALS BY DETERMINING THEIR CHEMICAL OR PHYSICAL PROPERTIES
- G01N30/00—Investigating or analysing materials by separation into components using adsorption, absorption or similar phenomena or using ion-exchange, e.g. chromatography or field flow fractionation
- G01N30/89—Inverse chromatography
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- G—PHYSICS
- G01—MEASURING; TESTING
- G01N—INVESTIGATING OR ANALYSING MATERIALS BY DETERMINING THEIR CHEMICAL OR PHYSICAL PROPERTIES
- G01N30/00—Investigating or analysing materials by separation into components using adsorption, absorption or similar phenomena or using ion-exchange, e.g. chromatography or field flow fractionation
- G01N30/02—Column chromatography
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Abstract
The present invention provides a kind of method of liquid chromatographic detection three monomer, uses FL2200 chromatograph of liquid, and N2000 chromatographic work station, the specification of chromatographic column Kromstar C18 is 4.6 × 150mm 5 μm；Flowing phase a is 80 90:10 20 with the volume ratio of flowing phase b；Detection wavelength: 220nm；Flow velocity: 0.8mL/min；Sampling volume: 20 μ L；Column temperature: 30 DEG C；Using the detection method of the present invention, the detection time was less than 10 minutes；Analysis precision is up to 0.01ng；Favorable reproducibility, relative error is 0.2%；Operation is simple, analyze whole automatization；Reach the purpose that the quality of dimethyl isophthalate 5 sodium sulfonate is control effectively.
Description
The present invention is application number 201510163946.4, the applying date: on April 9th, 2015, denomination of invention: " a kind of liquid phase color
Spectrometry detection Sodium Dimethyl Isophthalate-5-sulfonate purity method " divisional application.
Technical field
The present invention relates to a kind of method utilizing liquid chromatography detection Sodium Dimethyl Isophthalate-5-sulfonate purity,
Belong to Instrumental Analysis field.
Background technology
Sodium Dimethyl Isophthalate-5-sulfonate (popular name three monomer, SIPM write a Chinese character in simplified form in English) is the new of a kind of function admirable
Type anion surfactant, has important work at terylene (polyethylene terephthalate, i.e. PET) dyeing, modifying aspect
With, in PET production process, add SIPM and can produce the polyester fiber (CDP) of cationic dye capable of dyeing as Third monomer.Make
For producing a kind of serious difference modifying agent of modified poly ester product (CDP/ECDP etc.), solve after adding in section (PET)
The conventional polyester hygroscopicity determined because of terylene molecular structure of having determined is poor, dyeing is difficult, easily produce electrostatic, too high fiber
Intensity makes the easy balling-up of fabric, its style and comfortable features of clothing there is many defects such as the biggest gap with natural fiber.
In polyester slice, introduce SIPM can produce Cationic Dyeable Pet long filament, although its outward appearance and ordinary polyester long filament
There is no the biggest difference, but cation-modified owing to have employed, not only substantially improve the suction color performance of fiber, and reduce
Degree of crystallinity, thus adapt to the Silk of polyester fiber further.By Silkization can make fabric sofetening ventilative, comfortable,
Antistatic, normal-temperature normal-pressure dyeable.By cation-modified multifunction imitated hair, fabric can be made to have soft, antistatic, room temperature
Normal pressure and Mao Gongran.In the products such as cation dyeable polyester (CDP), low price, chromatograph can be used wide, bright in colour
Cationic dyeing, simultaneously still can use disperse dyeing, its dyeability relatively conventional polyester significantly improves uses cation
The fabric that modified fibre is made into, when dyeing with the dye of positive ion, have bright, deep-cutting gorge good, exhaustion rate is high, resistance to
Day light fastness and the advantage such as color fastness is good.When combination dyeing, fastness is good.Modified polyester fiber dyeing is the most bright-coloured dense
Thickness, coloring is good, has anti pilling effect simultaneously.In high temperature dye bath, good stability, to including conventional polyester fiber
Other fibers staining little, fast to the diffusion rate of fibrous inside, non-environmental-pollution phenomenon, in dye bath, pH value changes greatly, contaminates
Material stability is high.
Accordingly, as important cationic dyeability modifier Third monomer Sodium Dimethyl Isophthalate-5-sulfonate purity
Height directly affect the quality of downstream product quality.
Owing to Sodium Dimethyl Isophthalate-5-sulfonate boiling point is high, difficult vaporization, use the conventional gas chromatography cannot be real
Now detect the purpose of its purity, and the detection of Sodium Dimethyl Isophthalate-5-sulfonate at present, typically by surveying acid number and saponification
The chemistry titration method of the routine such as value carries out quality control, but can not reflect the inherent quality of product further, to Quality advance
Do not have directive function.
Summary of the invention
It is an object of the invention to overcome the deficiency of prior art, it is provided that a kind of liquid chromatography detection M-phthalic acid two
The method of methyl ester-5-sodium sulfonate purity, it is achieved following goal of the invention:
Use reversed phase ion high performance liquid chromatography to analyze, have that analysis time is short, component peaks good separating effect, resolution
High, analysis precision height, favorable reproducibility, operate easy advantage, reach to enter the quality of Sodium Dimethyl Isophthalate-5-sulfonate
The purpose that row effectively controls.
For solving above-mentioned technical problem, by the following technical solutions:
The method of a kind of liquid chromatography detection Sodium Dimethyl Isophthalate-5-sulfonate purity, including apparatus selection, detector bar
The setting of part, sample treatment, detection；
Using detection method of the present invention, detect Sodium Dimethyl Isophthalate-5-sulfonate purity, the detection time is less than 10
Minute；Analysis precision reaches 0.01ng；
The setting of described testing conditions, flowing phase a is 80-90:10-20 with the volume ratio of flowing phase b；
Described flowing phase a is 50mmol/L sodium dihydrogen phosphate；Flowing phase b is trifluoroacetic acid aqueous solution；
Described flowing phase a, the tetrabutylammonium chloride Han 0.05g in the 50mmol/L sodium dihydrogen phosphate of 100ml；
The setting of described testing conditions, detects wavelength: 220nm；Flow velocity: 0.8mL/min；Sampling volume: 20 μ L；Column temperature: 30
℃；
Described apparatus selection, use FL2200 chromatograph of liquid, N2000 chromatographic work station, chromatographic column Kromstar C18's
Specification is 4.6 × 150mm 5 μm.
Use above technical scheme, have the advantages that
(1) analysis time is short: prior art uses titrimetric method, detection Sodium Dimethyl Isophthalate-5-sulfonate
Purity, project, the index that need to measure are many, the longest, especially the detection of one of which important indicator-saponification number, need nearly 2 hours
Time；Application the method for the invention detects, from sample pre-treatments to completing interpretation of result, it is only necessary to 30 minutes.
(2) component peaks good separating effect: the present invention uses new and effective microgranule fixed phase stuffing so that liquid chromatograph is filled
The post effect of post reaches 5 × 103―3×104Block/m theoretical cam curve, significantly larger than gas-chromatography packed column 103Block/m theoretical cam curve
Post effect；Component contained in sample, by selecting suitable testing conditions, can be kept completely separate by the present invention.
(3) resolution is high: by selecting fixing phase and the kind of flowing phase and proportioning, can reach optimal separation effect
Really.
(4) analysis precision is high: precision is up to 0.01ng.
(5) favorable reproducibility: same sample repeatedly analyzes detection, analysis result is stable, and error is little, and relative error is 0.2%.
(6) operation is simple, analyze whole automatization, from detecting that calculating is all completed by instrument, no matter with or without chemical examination base
Plinth, it is only necessary to shirtsleeve operation training, can operate.
(7) purpose that the quality of Sodium Dimethyl Isophthalate-5-sulfonate is control effectively is reached: traditional chemistry
Titration assay method cannot the purity of direct reaction Sodium Dimethyl Isophthalate-5-sulfonate and internal impurity content, it converts
Rate also cannot directly obtain, and analysis time is long, therefore produce control time lacking of property and ageing；Use the present invention's
Detection method can analyze the purity of Sodium Dimethyl Isophthalate-5-sulfonate and the content of other impurity at short notice,
By impurity generational verctor is analyzed, targetedly production can be adjusted, improve its conversion ratio, thus reach
Control the purpose of quality.
Accompanying drawing illustrates:
Accompanying drawing 1: use the Technical Analysis sample gained chromatogram of embodiment 1；
Accompanying drawing 2: use the Technical Analysis sample gained chromatogram of embodiment 2；
Accompanying drawing 3: use the Technical Analysis sample gained chromatogram of embodiment 3；
Accompanying drawing 4: use the Technical Analysis sample gained chromatogram of embodiment 4.
Detailed description of the invention
Hereinafter the preferred embodiments of the present invention are illustrated, it will be appreciated that preferred embodiment described herein is only used
In the description and interpretation present invention, it is not intended to limit the present invention.
Embodiment 1
A kind of method of liquid chromatography detection Sodium Dimethyl Isophthalate-5-sulfonate purity:
1, instrument:
(1) FL2200 chromatograph of liquid, joins UV-detector, N2000 chromatographic work station
(2) chromatographic column Kromstar C18 4.6 × 150mm 5 μm
(3) thermocolumn case: day Puli RPL-C2000
(4) ultrasonic degasser
2, testing conditions:
(1) flowing phase:
A. water (containing volume fraction 0.05% tetrabutylammonium chloride)；
B. methanol；
Proportion of mobile phase Va:Vb=40:60
(2) detection wavelength: 220nm
(3) flow velocity: 0.8mL/min
(4) sampling volume: 20 μ L
(5) column temperature: 30 DEG C
3, sample treatment:
Accurately weighing 0.01g Sodium Dimethyl Isophthalate-5-sulfonate, dissolve by distilled water slight fever, after cooling, constant volume is in 100mL
In volumetric flask, deaerate after water system membrane filtration standby.
4, by the flowing for preparing mutually first through 0.45 μm membrane filtration, after the most ultrasonic degassing 15 minutes, chromatograph flowing is poured into
In phase liquid containing bottle, start preheating, after system stability, extract testing sample 20 μ L sample detection, after going out peak and terminating, use area
Normalization method calculates percentage composition.
Analyzing sample by above-mentioned chromatographic condition, the chromatogram obtained is shown in accompanying drawing 1, in accompanying drawing 1:
1 is solvent peak, and 2 is impurity peaks, and 3 is M-phthalic acid, and 4 is Sodium Dimethyl Isophthalate-5-sulfonate, and 5 is isophthalic two
Formic acid dimethyl ester.
Sample detection result:
By above testing result it can be seen that under the conditions of this baseline be not the most stable, go out peak less, partial impurities peak is not examined
Go out, testing result is had certain impact.
Embodiment 2
A kind of method of liquid chromatography detection Sodium Dimethyl Isophthalate-5-sulfonate purity:
1, instrument:
(1) FL2200 chromatograph of liquid, joins UV-detector, N2000 chromatographic work station
(2) chromatographic column Kromstar C18 4.6 × 150mm 5 μm
(3) thermocolumn case: day Puli RPL-C2000
(4) ultrasonic degasser
2, testing conditions:
(1) flowing phase: a. water (containing volume fraction 0.05% tetrabutylammonium chloride)；B. acetonitrile；Proportion of mobile phase Va:Vb=80:
20
(2) detection wavelength: 220nm
(3) flow velocity: 0.8mL/min
(4) sampling volume: 20 μ L
(5) column temperature: 30 DEG C
3, sample treatment:
Accurately weighing 0.01g Sodium Dimethyl Isophthalate-5-sulfonate, dissolve by distilled water slight fever, after cooling, constant volume is in 100mL
In volumetric flask, deaerate after water system membrane filtration standby.
4, by the flowing for preparing mutually first through 0.45 μm membrane filtration, after the most ultrasonic degassing 15 minutes, chromatograph flowing is poured into
In phase liquid containing bottle, start preheating, after system stability, extract testing sample 20 μ L sample detection, after going out peak and terminating, use area
Normalization method calculates percentage composition.
Analyzing sample by above-mentioned chromatographic condition, the chromatogram obtained is shown in accompanying drawing 2, in accompanying drawing 2:
1 is solvent peak, and 2,3,4,6 is impurity peaks, and 5 is M-phthalic acid, and 7 is Sodium Dimethyl Isophthalate-5-sulfonate, and 8 are
Dimethyl isophthalate.
Sample detection result:
By above testing result it can be seen that to go out peak under the conditions of this more, but main peak is less desirable with impurity peaks separating effect.
Embodiment 3
A kind of method of liquid chromatography detection Sodium Dimethyl Isophthalate-5-sulfonate purity:
1, instrument:
(1) FL2200 chromatograph of liquid, joins UV-detector, N2000 chromatographic work station
(2) chromatographic column Kromstar C18 4.6 × 150mm 5 μm
(3) thermocolumn case: day Puli RPL-C2000
(4) ultrasonic degasser
2, testing conditions:
(1) flowing phase: a. 50mmol/L sodium dihydrogen phosphate (containing volume fraction 0.05% tetrabutylammonium chloride)；B. methanol
(chromatographically pure)；Proportion of mobile phase Va:Vb=40:60
(2) detection wavelength: 220nm
(3) flow velocity: 0.8mL/min
(4) sampling volume: 20 μ L
(5) column temperature: 30 DEG C
3, sample treatment:
Accurately weigh 0.01g Sodium Dimethyl Isophthalate-5-sulfonate, with flowing phase a slight fever dissolve, after cooling constant volume in
In 100mL volumetric flask, deaerate after water system membrane filtration standby.
4, by the flowing for preparing mutually first through 0.45 μm membrane filtration, after the most ultrasonic degassing 15 minutes, chromatograph flowing is poured into
In phase liquid containing bottle, start preheating, after system stability, extract testing sample 20 μ L sample detection, after going out peak and terminating, use area
Normalization method calculates percentage composition.
Analyzing sample by above-mentioned chromatographic condition, the chromatogram obtained is shown in accompanying drawing 3, in accompanying drawing 3:
1 is solvent peak, and 2,3,4,6 is impurity peaks, and 5 is M-phthalic acid, and 7 is Sodium Dimethyl Isophthalate-5-sulfonate, and 8 are
Dimethyl isophthalate.
Sample detection result:
By above testing result it can be seen that to go out peak number amount under the conditions of this same as in Example 2, each peak separates also good, but respectively
Impurity peaks peak value is less, and the peak value of main peak is on the low side, has conditions of streaking.
Embodiment 4
A kind of method of liquid chromatography detection Sodium Dimethyl Isophthalate-5-sulfonate purity:
1, instrument:
(1) FL2200 chromatograph of liquid, joins UV-detector, N2000 chromatographic work station
(2) chromatographic column Kromstar C18 4.6 × 150mm 5 μm
(3) thermocolumn case: day Puli RPL-C2000
(4) ultrasonic degasser
2, testing conditions:
(1) flowing phase:
A, 50mmol/L sodium dihydrogen phosphate is (containing volume fraction 0.05% tetrabutylammonium chloride, i.e. the 50mmol/L phosphorus of 100ml
The tetrabutylammonium chloride Han 0.05g in acid dihydride sodium solution)；
B, acetonitrile (chromatographically pure)；
C, proportion of mobile phase Va:Vb=90:10(i.e. flow phase a and the volume ratio of phase b that flows is 90:10)；
(2) detection wavelength: 220nm(diode array detector determines)
(3) flow velocity: 0.8mL/min
(4) sampling volume: 20 μ L
(5) column temperature: 30 DEG C
3, sample treatment:
Accurately weigh 0.01g Sodium Dimethyl Isophthalate-5-sulfonate, with flowing phase a slight fever dissolve, after cooling constant volume in
In 100mL volumetric flask, deaerate after water system membrane filtration standby.
4, detection:
By the flowing for preparing mutually first through 0.45 μm membrane filtration, after the most ultrasonic degassing 15 minutes, pour chromatograph flowing phase liquid storage into
In Ping, start preheating, after system stability, extract testing sample 20 μ L sample detection, after going out peak and terminating, use area normalization method
Calculate percentage composition；Analyzing sample by above-mentioned chromatographic condition, the chromatogram obtained is shown in accompanying drawing 4, in accompanying drawing 4:
1 is solvent peak, and 2,4,5,6 is impurity peaks, and 3 is M-phthalic acid, and 7 is Sodium Dimethyl Isophthalate-5-sulfonate, and 8 are
Dimethyl isophthalate.
Sample detection result:
By above testing result it can be seen that under the conditions of this, baseline balances, and in sample, all impurity peaks are all detected, and separate
Effective, peak value is normal, and the peak shape of main peak is symmetrical, and substantially without conditions of streaking, all of peak all went out in 10 minutes, during detection
Between short.
Through test, proportion of mobile phase Va:Vb=80-90:10-20, other use the technical scheme of embodiment 4, also obtain good
Good experimental result, baseline balances, and in sample, all impurity peaks are all detected, and good separating effect, and peak value is normal, the peak of main peak
Shape is symmetrical, substantially without conditions of streaking.
Employing technical solution of the present invention:
(1) use high-precision analytical tool-chromatograph of liquid that Sodium Dimethyl Isophthalate-5-sulfonate sample is directly carried out
Analyzing, the purity of sample and other impurity contents all can intuitively and accurately be presented on chromatogram, no matter to isophthalic two
Producing or applying of formic acid dimethyl ester-5-sodium sulfonate has the biggest directive function.
(2) aqueous phase in flowing mutually uses buffer salt solution.Reversed phase chromatography separation sample is based primarily upon compound to be separated
Polarity realize separate.The material retention that polarity is strong in the situation (molecular weight, space structure) that other conditions are similar
Little.For neutral species, its polarity depends on compound itself, but can be by adjusting it for ionic compound
Whether dissociate or dissociation degree is to adjust its polarity, be finally reached its retention of adjustment, separating degree and post effect (general retention
The raising that post is imitated can be brought in advance).Sodium Dimethyl Isophthalate-5-sulfonate belongs to ionic compound, with being suitable for the slow of pH value
Rush saline solution to control the dissociation degree of Sodium Dimethyl Isophthalate-5-sulfonate sample as aqueous phase, one side, adjust it
Polarity, on the other hand can control the hydrolysis of Sodium Dimethyl Isophthalate-5-sulfonate sample, improves accuracy of detection.
(3) organic facies in flowing mutually uses acetonitrile.In general, the organic facies in the flowing mutually of reversed-phase HPLC is commonly used
For chromatograph methanol and acetonitrile.Methanol has the advantage of its cost performance, but methanol activity is high, may react with some sample,
And methanol has uv absorption at lower wavelengths that, the sensitivity of analysis method can be reduced；Although acetonitrile price is the highest, toxicity compares first
Alcohol is big, but eluting power is stronger than methanol, seldom reacts with sample, lower very than methanol as flow phase system pressure
Many, and cutoff wavelength 20nm lower than methanol, add the probability detecting the impurity the most just having absorption.Isophthalic two
The production technology of formic acid dimethyl ester-5-sodium sulfonate determines and can contain unreacted M-phthalic acid impurity completely in product, if
Select methanol as organic facies, the most likely can produce reaction with it, increase detection error, and table after experiment
Bright, with acetonitrile as organic facies, baseline is more stable, impurity peaks separates with main peak and becomes apparent from.
(4) inherent quality of Sodium Dimethyl Isophthalate-5-sulfonate can be reacted accurately.
(5) shorten the detection time, simplify the detecting step of Sodium Dimethyl Isophthalate-5-sulfonate, improve work
Make efficiency.
In the above-described embodiments, the preferred forms of the present invention is described, it is obvious that at the invention structure of the present invention
Under think of, still can make a lot of change.Here, it should be noted that any change made under the inventive concept of the present invention is all incited somebody to action
Fall within the scope of protection of the present invention.
Claims (2)
1. the method for liquid chromatographic detection three monomer, it is characterised in that: include apparatus selection, the setting of testing conditions, sample
Product process, detection；
The setting of described testing conditions, flowing phase a is 80-90:10-20 with the volume ratio of flowing phase b；
Described flowing phase a is 50mmol/L sodium dihydrogen phosphate tetrabutylammonium chloride Han volume fraction 0.05%；
Described flowing phase b is trifluoroacetic acid aqueous solution；
Described apparatus selection, the model of thermocolumn case is day Puli RPL-C2000；The described detection time is less than 10 minutes, analyzes
Precision reaches 0.01ng.
The method of a kind of liquid chromatographic detection three monomer the most according to claim 1, it is characterised in that:
The setting of described testing conditions, detects wavelength: 220nm；Flow velocity: 0.8mL/min；Sampling volume: 20 μ L；Column temperature: 30
℃；
Described apparatus selection, use FL2200 chromatograph of liquid, N2000 chromatographic work station, chromatographic column Kromstar C18's
Specification is 4.6 × 150mm 5 μm；
Described sample treatment: accurately weigh 0.01g Sodium Dimethyl Isophthalate-5-sulfonate, dissolves by flowing phase a slight fever, cold
But after, constant volume is in 100mL volumetric flask, deaerates standby after water system membrane filtration；
Described detection, by the flowing for preparing mutually first through 0.45 μm membrane filtration, after the most ultrasonic degassing 15 minutes, pours chromatograph stream into
In dynamic phase liquid containing bottle, start preheating, after system stability, extract testing sample 20 μ L sample detection.
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| CN110907551A (en) * | 2019-11-30 | 2020-03-24 | 山东第一医科大学(山东省医学科学院) | Method for detecting purity of dimethyl isophthalate-5-sulfonic acid in esterification liquid for producing three monomers |
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| CN105181843B (en) * | 2015-09-10 | 2017-03-01 | 中华人民共和国台州出入境检验检疫局 | 3 kinds of aromatic organic acids of HPLC/MS-MS/salt Special migration method |
| CN111103364A (en) * | 2019-05-02 | 2020-05-05 | 浙江佳人新材料有限公司 | PET content detection method |
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Also Published As
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| CN104730170A (en) | 2015-06-24 |
| CN106198830B (en) | 2018-01-02 |
| CN104730170B (en) | 2016-10-05 |
| CN106066371A (en) | 2016-11-02 |
| CN106066371B (en) | 2018-07-06 |
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