CN104730170B - A kind of method of liquid chromatography detection Sodium Dimethyl Isophthalate-5-sulfonate purity - Google Patents
A kind of method of liquid chromatography detection Sodium Dimethyl Isophthalate-5-sulfonate purity Download PDFInfo
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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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- 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
- G01N30/89—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
- G01N30/96—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 using ion-exchange
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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
- G01N2030/022—Column chromatography characterised by the kind of separation mechanism
- G01N2030/027—Liquid chromatography
Abstract
The invention discloses the method for a kind of liquid chromatography detection DMIP 5 sodium sulfonate purity, use FL2200 liquid chromatograph, 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 is less than 10 minutes；Analysis precision is up to 0.01ng；Favorable reproducibility, relative error is 0.2%；Operation is simple, analyze all automations；Reach the purpose controling effectively the quality of DMIP 5 sodium sulfonate.
Description
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, interpolation SIPM 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)
Determined because terylene molecular structure determined conventional polyester hygroscopicity difference, dyeing difficulty, easily produce electrostatic, too high fiber
Intensity makes the easy balling-up of fabric, its style and comfortable features of clothing there is very many defects such as big gap with natural fiber.
Introduce SIPM and can produce Cationic Dyeable Pet long filament in polyester slice, although its outward appearance and ordinary polyester long filament
There is no too big difference, but cation-modified owing to have employed, not only substantially improve the suction look 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, normal temperature
Normal pressure and Mao Gongran.In the products such as cation dyeable polyester (CDP), low price, chromatogram 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 more 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 current Sodium Dimethyl Isophthalate-5-sulfonate, typically by surveying acid number and saponification
The conventional chemistry titration method 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.
Content of the invention
It is an object of the invention to overcome the deficiency of prior art, a kind of liquid chromatography detection M-phthalic acid two is provided
The method of methyl esters-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
Rate is high, analysis precision is high, favorable reproducibility, operates easy advantage, reaches the quality to Sodium Dimethyl Isophthalate-5-sulfonate
The purpose controling effectively.
For solving above-mentioned technical problem, by the following technical solutions:
A kind of method of liquid chromatography detection Sodium Dimethyl Isophthalate-5-sulfonate purity, including apparatus selection, inspection
The setting of survey condition, sample treatment, detection；
Using detection method of the present invention, detecting Sodium Dimethyl Isophthalate-5-sulfonate purity, the detection time is little
In 10 minutes；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, tetrabutylammonium chloride containing 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；Post
Temperature: 30 DEG C；
Described apparatus selection, uses FL2200 liquid chromatograph, N2000 chromatographic work station, chromatographic column Kromstar
The specification of C18 is 4.6 × 150mm 5 μm.
Use above technical scheme, have the advantages that
(1) analysis time is short: prior art uses titrimetric method, detects DMIP-5-sulfonic acid
The purity of sodium, project, the index that need to measure are many, time-consumingly long, especially the detection of one of which important indicator-saponification number, need nearly 2
The time of hour；Application the method for the invention detects, from sample pre-treatments to completing interpretation of result, it is only necessary to 30 points
Clock.
(2) component peaks good separating effect: the present invention uses new and effective particulate fixed phase stuffing so that liquid chromatogram 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 ratio is high: by selecting fixing species and proportioning with flowing phase mutually, 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 all automations, from detecting that calculating is all completed by instrument, no matter has or not chemical examination base
Plinth, it is only necessary to shirtsleeve operation training, can operate.
(7) purpose controling effectively the quality of Sodium Dimethyl Isophthalate-5-sulfonate is reached: traditional chemistry
Titration assay method cannot directly react the purity of Sodium Dimethyl Isophthalate-5-sulfonate and internal impurity content, its conversion
Rate also cannot directly obtain, and analysis time is long, therefore the lacking of property and ageing when producing control；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
The purpose of control quality.
Brief description:
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
It in the description and interpretation present invention, is not intended to limit the present invention.
Embodiment 1
A kind of method of liquid chromatography detection Sodium Dimethyl Isophthalate-5-sulfonate purity:
1st, instrument:
(1) FL2200 liquid chromatograph, 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
2nd, testing conditions:
(1) flow phase:
A. water (tetrabutylammonium chloride containing volume fraction 0.05%)；
B. methyl alcohol；
Proportion of mobile phase Va:Vb=40:60
(2) wavelength: 220nm is detected
(3) flow velocity: 0.8mL/min
(4) sampling volume: 20 μ L
(5) column temperature: 30 DEG C
3rd, sample treatment:
Accurately weigh 0.01g Sodium Dimethyl Isophthalate-5-sulfonate, with distilled water low-grade fever dissolve, after cooling constant volume in
In 100mL volumetric flask, deaerate after water system membrane filtration standby.
4th, by the flowing for preparing mutually first through 0.45 μm of membrane filtration, then after ultrasonic degassing 15 minutes, chromatograph flowing is poured into
In phase liquid storage 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 obtaining 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, between 5 are
Rutgers.
Sample detection result:
By above testing result it can be seen that under the conditions of this baseline be not very stable, go out peak less, partial impurities peak does not has
Detection, has certain impact to testing result.
Embodiment 2
A kind of method of liquid chromatography detection Sodium Dimethyl Isophthalate-5-sulfonate purity:
1st, instrument:
(1) FL2200 liquid chromatograph, 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
2nd, testing conditions:
(1) flow phase: a. water (tetrabutylammonium chloride containing volume fraction 0.05%)；B. acetonitrile；Proportion of mobile phase Va:Vb=
80:20
(2) wavelength: 220nm is detected
(3) flow velocity: 0.8mL/min
(4) sampling volume: 20 μ L
(5) column temperature: 30 DEG C
3rd, sample treatment:
Accurately weigh 0.01g Sodium Dimethyl Isophthalate-5-sulfonate, with distilled water low-grade fever dissolve, after cooling constant volume in
In 100mL volumetric flask, deaerate after water system membrane filtration standby.
4th, by the flowing for preparing mutually first through 0.45 μm of membrane filtration, then after ultrasonic degassing 15 minutes, chromatograph flowing is poured into
In phase liquid storage 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 obtaining is shown in accompanying drawing 2, in accompanying drawing 2:
1 be solvent peak, the 2nd, the 3rd, the 4th, 6 be impurity peaks, 5 be M-phthalic acid, 7 be Sodium Dimethyl Isophthalate-5-sulfonate,
8 is DMIP.
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 and impurity peaks separating effect are not very
Preferable.
Embodiment 3
A kind of method of liquid chromatography detection Sodium Dimethyl Isophthalate-5-sulfonate purity:
1st, instrument:
(1) FL2200 liquid chromatograph, 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
2nd, testing conditions:
(1) flow phase: a. 50mmol/L sodium dihydrogen phosphate (tetrabutylammonium chloride containing volume fraction 0.05%)；b.
Methyl alcohol (chromatographically pure)；Proportion of mobile phase Va:Vb=40:60
(2) wavelength: 220nm is detected
(3) flow velocity: 0.8mL/min
(4) sampling volume: 20 μ L
(5) column temperature: 30 DEG C
3rd, sample treatment:
Accurately weigh 0.01g Sodium Dimethyl Isophthalate-5-sulfonate, with flowing phase a low-grade fever dissolve, after cooling constant volume in
In 100mL volumetric flask, deaerate after water system membrane filtration standby.
4th, by the flowing for preparing mutually first through 0.45 μm of membrane filtration, then after ultrasonic degassing 15 minutes, chromatograph flowing is poured into
In phase liquid storage 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 obtaining is shown in accompanying drawing 3, in accompanying drawing 3:
1 be solvent peak, the 2nd, the 3rd, the 4th, 6 be impurity peaks, 5 be M-phthalic acid, 7 be Sodium Dimethyl Isophthalate-5-sulfonate,
8 is DMIP.
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 each 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:
1st, instrument:
(1) FL2200 liquid chromatograph, 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
2nd, testing conditions:
(1) flow phase:
A, 50mmol/L sodium dihydrogen phosphate (tetrabutylammonium chloride containing volume fraction 0.05%, the i.e. 50mmol/ of 100ml
Tetrabutylammonium chloride containing 0.05g in L sodium dihydrogen phosphate)；
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) wavelength is detected: 220nm(PDAD determines)
(3) flow velocity: 0.8mL/min
(4) sampling volume: 20 μ L
(5) column temperature: 30 DEG C
3rd, sample treatment:
Accurately weigh 0.01g Sodium Dimethyl Isophthalate-5-sulfonate, with flowing phase a low-grade fever dissolve, after cooling constant volume in
In 100mL volumetric flask, deaerate after water system membrane filtration standby.
4th, detect:
By the flowing for preparing mutually first through 0.45 μm of membrane filtration, then after ultrasonic degassing 15 minutes, pour chromatograph flowing phase into
In liquid storage bottle, start preheating, after system stability, extract testing sample 20 μ L sample detection, after going out peak and terminating, returned by area
One method calculates percentage composition；Analyzing sample by above-mentioned chromatographic condition, the chromatogram obtaining is shown in accompanying drawing 4, in accompanying drawing 4:
1 be solvent peak, the 2nd, the 4th, the 5th, 6 be impurity peaks, 3 be M-phthalic acid, 7 be Sodium Dimethyl Isophthalate-5-sulfonate,
8 is DMIP.
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
Good separating effect, 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, inspection
The survey time is 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 instrument-liquid chromatograph direct to Sodium Dimethyl Isophthalate-5-sulfonate sample
Being analyzed, the purity of sample and other impurity contents all can be directly perceived and be presented on accurately on chromatogram, no matter pair between
The production of rutgers-5-sodium sulfonate or application have very big directive function.
(2) aqueous phase flowing in phase 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 similar situation (molecular weight, space structure) of other conditions
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 delaying of applicable pH value
Rush salting liquid 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 phase flowing in phase uses acetonitrile.In general, the organic phase in the flowing phase of reversed-phase HPLC is commonly used
For chromatogram methyl alcohol and acetonitrile.Methyl alcohol has the advantage of its cost performance, but methanol activity is high, may react with some sample,
And methyl alcohol has UV absorption at lower wavelengths that, the sensitivity of analysis method can be reduced；Although acetonitrile price is very high, toxicity compares first
Alcohol is big, but eluting power is stronger than methyl alcohol, seldom reacts with sample, is used as flow phase system pressure lower very than methyl alcohol
Many, and cutoff wavelength than methyl alcohol low 20nm, add the possibility detecting the impurity just having absorption at lower wavelengths that.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 methyl alcohol as organic phase, be possible under given conditions to produce reaction with it, increase detection error, and table after experiment
Bright, with acetonitrile as organic phase, 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 made under the inventive concept of the present invention any change all incite somebody to action
Fall within the scope of protection of the present invention.
Claims (1)
1. a method for liquid chromatography detection Sodium Dimethyl Isophthalate-5-sulfonate purity, including apparatus selection, detection
The setting of condition, sample treatment, 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 b is trifluoroacetic acid aqueous solution；
Described flowing phase a, tetrabutylammonium chloride containing 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 liquid chromatograph, N2000 chromatographic work station, chromatographic column Kromstar C18's
Specification is 4.6 × 150mm 5 μm；
Sample treatment: accurately weigh 0.01g Sodium Dimethyl Isophthalate-5-sulfonate, is dissolved by flowing phase a low-grade fever, after cooling
Constant volume, in 100mL volumetric flask, deaerates standby after water system membrane filtration；
Described detection, by the flowing for preparing mutually first through 0.45 μm of membrane filtration, then after ultrasonic degassing 15 minutes, pours chromatograph stream into
In dynamic phase liquid storage bottle, start preheating, after system stability, extract testing sample 20 μ L sample detection.
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| CN201610556742.1A CN106198830B (en) | 2015-04-09 | 2015-04-09 | A kind of method of the monomer of liquid chromatographic detection three |
| CN201510163946.4A CN104730170B (en) | 2015-04-09 | 2015-04-09 | A kind of method of liquid chromatography detection Sodium Dimethyl Isophthalate-5-sulfonate purity |
| CN201610556741.7A CN106066371B (en) | 2015-04-09 | 2015-04-09 | A kind of three monomer liquid chromatogram rapid analysis methods |
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| CN111103364A (en) * | 2019-05-02 | 2020-05-05 | 浙江佳人新材料有限公司 | PET content detection method |
| 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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| JPS61204564A (en) * | 1984-11-08 | 1986-09-10 | Yanagimoto Seisakusho:Kk | Method and instrument for automatic analysis of sex steroid hormone |
| DE3585505D1 (en) * | 1984-12-21 | 1992-04-09 | Procter & Gamble | BLOCK POLYESTER AND SIMILAR COMPOUNDS, USED AS A DETOIL REMOVER IN DETERGENT COMPOSITIONS. |
| US4711730A (en) * | 1986-04-15 | 1987-12-08 | The Procter & Gamble Company | Capped 1,2-propylene terephthalate-polyoxyethylene terephthalate polyesters useful as soil release agents |
| PT1581617E (en) * | 2002-02-08 | 2011-05-05 | Danisco Us Inc | Methods for producing end-products from carbon substrates |
| US7888405B2 (en) * | 2004-01-30 | 2011-02-15 | E. I. Du Pont De Nemours And Company | Aliphatic-aromatic polyesters, and articles made therefrom |
| CN101294935A (en) * | 2007-04-29 | 2008-10-29 | 厦门翔鹭化纤股份有限公司 | Method for measuring SIPE content in modified polyester by reversed phase high efficiency liquid chromatography |
| KR101003551B1 (en) * | 2008-04-30 | 2010-12-30 | 주식회사 아이바이오팜 | Method of analyzing bisphophonate compound using derivative reaction |
| CN103030187A (en) * | 2011-10-09 | 2013-04-10 | 山东科技职业学院 | Method for removing high-molecular polymer in sodiosulfoisophthalate (SIPM) waste water |
| CN102633693B (en) * | 2012-03-22 | 2013-11-13 | 潍坊沃尔特化学有限公司 | Method for synthesizing dimethyl isophthalate-5-sodium sulfonate |
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