CN101294935A - Method for measuring SIPE content in modified polyester by reversed phase high efficiency liquid chromatography - Google Patents
Method for measuring SIPE content in modified polyester by reversed phase high efficiency liquid chromatography Download PDFInfo
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- CN101294935A CN101294935A CNA2007100089373A CN200710008937A CN101294935A CN 101294935 A CN101294935 A CN 101294935A CN A2007100089373 A CNA2007100089373 A CN A2007100089373A CN 200710008937 A CN200710008937 A CN 200710008937A CN 101294935 A CN101294935 A CN 101294935A
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Abstract
The invention discloses a method for measuring SIPE content of modified polyester by using a reversed phase high performance liquid chromatography method; the method adopts the reversed phase high performance liquid chromatography method to measure and the chromatographic condition is that: (1) a chromatographic column selects Shim-Pack VP-ODS C18 column; the specification is 250mm multiplied by 4.6mm; the grain size of the stuffing is 5Mum; (2) methanol and 0.1percent to 0.2 percent of phosphoric acid solution of which the volume ratio of is 10:90 to 90:10 are used as a chromatographic mobile phase; the flow rate of the mobile phase is 0.5 to 2ml/min; gradient elution is carried out; (3) the column temperature is 40 DEG C; the detection wavelength of the used ultraviolet detector is 220nm; the sampling volume is 5 to 20 MumL; the invention finds the chromatography analyzing method which is suitable for the content of the isophthalic acid diethylene glycol dilaurate-5-sulfonate (SIPE) by using a great deal of experiments and theories as analyzing base, and has the advantages of good representation of components, high resolution, simple and fast operation and precise measurement.
Description
Technical field
The present invention relates to a kind of method of utilizing m-phthalic acid binaryglycol ester in the liquid chromatography for measuring modified poly ester-5-sulfonate (SIPE).
Background technology
As the m-phthalic acid binaryglycol ester-5-sulfonate (SIPE) of estrodur dyeing modifier and the 3rd monomer is one of at present the most frequently used the 3rd monomer modified dose.Polyester industrial had obtained development rapidly in China in recent years, each enterprise is all carrying out the differential exploitation of polyester, the research that can be used as the m-phthalic acid binaryglycol ester-5-sulfonate (SIPE) of estrodur dyeing modifier and the 3rd monomer is also carried out in a large number, m-phthalic acid binaryglycol ester-5-sulfonate (SIPE) is applicable to the 3rd monomer of large-scale PTA process route production cation-dyeable type polyester, can give the CDP dacron dye of positive ion is had good soft performance, make after the CDP stock-dye bright in colour, chromatogram is complete, the degree of staining jail, and has good antistatic behaviour, hydroscopicity and gas penetration potential play the effect that reduces the dyeing cost and improve environmental protection simultaneously.Because the content size of m-phthalic acid binaryglycol ester-5-sulfonate (SIPE) can directly influence the performance of back converted products in the modified poly ester section, and what and cost of m-phthalic acid binaryglycol ester-5-sulfonate (SIPE) addition have direct correlation, so the content of m-phthalic acid binaryglycol ester-5-sulfonate (SIPE) should be as such as important quality control index in cationic polyester and the water-soluble polyester production.
Summary of the invention
The objective of the invention is to overcome the deficiency of prior art, the method of SIPE content in a kind of rp-hplc determination modified poly ester is provided, be to utilize reversed-phased high performace liquid chromatographic to measure, it is good to have presenting property of component peaks, the resolution height, simple to operate, quick, measure advantage accurately.
The technical solution adopted for the present invention to solve the technical problems is: the method for SIPE content in a kind of rp-hplc determination modified poly ester comprises:
M-phthalic acid in modified poly ester binaryglycol ester-5-sulfonate (SIPE) is decomposed the pre-treatment step of coming out;
The testing procedure that adopts reversed-phased high performace liquid chromatographic to test;
Wherein, the reversed-phase high-performance liquid chromatography test comprises following chromatographic condition:
A. chromatographic column is selected Shim-Pack VP-ODS C18 post for use, specification 250mm * 4.6mm, filler granularity 5 μ m;
B. with the volume ratio of methyl alcohol and 0.1～0.2% phosphate aqueous solution be 10: 90～90: 10 as chromatogram flow phase; Flow rate of mobile phase is 0.5～2ml/min; Carry out gradient elution;
C. column temperature is 40 ℃, and it is 220nm that used UV-detector detects wavelength, and sampling volume is 5～20 μ L.
The chromatographic condition of described reversed-phase high-performance liquid chromatography test is further preferably:
A. chromatographic column is selected Shim-Pack VP-ODS C18 post for use, specification 250mm * 4.6mm, filler granularity 5 μ m;
B. with the volume ratio of methyl alcohol and 0.15% phosphate aqueous solution be 50: 50 as chromatogram flow phase; Flow rate of mobile phase is 1ml/min; Carry out gradient elution;
C. column temperature is 40 ℃, and it is 220nm that used UV-detector detects wavelength, and sampling volume is 10 μ L.
The described pre-treatment process of coming out that the binaryglycol ester of m-phthalic acid in the modified poly ester-5-sulfonate (SIPE) is decomposed is the alcoholysis of employing ethylene glycol (EG).
The invention has the beneficial effects as follows, owing to adopted reversed-phased high performace liquid chromatographic to come SIPE content in the modified poly ester is measured, and the chromatographic condition of reversed-phase high-performance liquid chromatography test is: a. chromatographic column is selected Shim-PackVP-ODS C18 post for use, specification 250mm * 4.6mm, filler granularity 5 μ m; B. with the volume ratio of methyl alcohol and 0.1～0.2% phosphate aqueous solution be 10: 90～90: 10 as chromatogram flow phase; Flow rate of mobile phase is 0.5～2ml/min; Carry out gradient elution; C. column temperature is 40 ℃, and it is 220nm that used UV-detector detects wavelength, and sampling volume is 5～20 μ L; It is good that this method of testing has presenting property of component peaks, and the resolution height is simple to operate, quick, measures advantage accurately.
Below in conjunction with drawings and Examples the present invention is described in further detail; But the method for SIPE content is not limited to embodiment in a kind of rp-hplc determination modified poly ester of the present invention.
Description of drawings
Fig. 1 is a SIPE canonical plotting of the present invention;
Fig. 2 is a standard SIPE chromatogram of the present invention;
Fig. 3 is the present invention's half delustring section chromatogram;
Fig. 4 is the water-soluble section chromatogram of the present invention;
Fig. 5 is a kation section chromatogram of the present invention.
Embodiment
Embodiment one, the method of SIPE content in a kind of rp-hplc determination modified poly ester of the present invention, the instrument that is adopted comprises that high performance liquid chromatograph joins UV-detector, quaternary gradient pump, common heating cover, supercentrifuge, ultrapure water preparation facilities etc.The reagent that is adopted comprises chromatogram methyl alcohol, chromatogram phosphoric acid, ultrapure water, ethylene glycol, acetate etc.
The chromatographic condition of the reversed-phased high performace liquid chromatographic that is adopted is:
A. chromatographic column is selected Shim-Pack VP-ODS C18 post for use, specification 250mm * 4.6mm, filler granularity 5 μ m;
B. with the volume ratio of methyl alcohol and 0.15% phosphate aqueous solution be 50: 50 as chromatogram flow phase; Flow rate of mobile phase is 1ml/min; Carry out gradient elution;
C. column temperature is 40 ℃, and it is 220nm that used UV-detector detects wavelength, and sampling volume is 10 μ L.
In the pre-treatment process:
Take by weighing 3 grams, half delustring section sample, in the ground conical flask of the 250ml that packs into, add 30ml ethylene glycol (EG) liquid then, add a spot of acetate simultaneously as catalyzer, be warming up to 200 ℃ and carry out back flow reaction on heating jacket, the reaction time is 2 hours, and the cooling of reaction back is left standstill.Carry out centrifugally then on SIGMA 2-16 hydro-extractor, centrifugal speed is 6000rpm/min, and it is to be tested to get supernatant liquor (half delustring section) after centrifugal 15 minutes.
Take by weighing the water-soluble section sample of 3 grams, in the ground conical flask of the 250ml that packs into, add 30ml ethylene glycol (EG) liquid then, add a spot of acetate simultaneously as catalyzer, be warming up to 200 ℃ and carry out back flow reaction on heating jacket, the reaction time is 2 hours, and the cooling of reaction back is left standstill.Carry out centrifugally then on SIGMA 2-16 hydro-extractor, centrifugal speed is 6000rpm/min, and it is to be tested to get supernatant liquor (water-soluble section) after centrifugal 15 minutes.
Take by weighing 3 gram kation section samples, in the ground conical flask of the 250ml that packs into, add 30ml ethylene glycol (EG) liquid then, add a spot of acetate simultaneously as catalyzer, be warming up to 200 ℃ and carry out back flow reaction on heating jacket, the reaction time is 2 hours, and the cooling of reaction back is left standstill.Carry out centrifugally then on SIGMA 2-16 hydro-extractor, centrifugal speed is 6000rpm/min, and it is to be tested to get supernatant liquor (kation section) after centrifugal 15 minutes.
Above-mentioned pre-treatment process is actually the pre-treating method that adopts the EG alcoholysis binaryglycol ester of the m-phthalic acid in the modified poly ester-5-sulfonate (SIPE) is decomposed to come out.
In the process of utilizing reversed-phased high performace liquid chromatographic to test, comprise test and typical curve drafting and double delustring section sample, water-soluble section sample, the chromatogram test of kation section sample and the actual content that external standard method is obtained SIPE to the SIPE standard specimen.
In test and typical curve drawing process to the SIPE standard specimen:
At first, the preparation standard specimen takes by weighing 1g m-phthalic acid binaryglycol ester-5-sulfonate (SIPE) as standard specimen, and SIPE is the solution that contains 80% EG, the 1g standard specimen is positioned in the volumetric flask of 100ml, adds water to scale, shakes up the back and places, and this liquid is A liquid; Get above-mentioned A liquid 10ml in the volumetric flask of another 100ml, add water to scale, shake up the back and place, this liquid is B liquid, set aside for use.
Then; get standard SIPE (being above-mentioned B liquid) and prepare 19.400%, 13.156%, 10.278%, 7.973% standard solution respectively, utilize the HPLC liquid chromatography to test, obtain chromatogram; wherein, the chromatogram of 19.400% standard solution is seen shown in Figure 2;
Then, be horizontal ordinate with the solution concentration, with the peak area ordinate, carry out linear regression analysis, gained typical curve coefficient R
2=0.997694.The SIPE typical curve of being drawn as shown in Figure 1.
Obtain in the actual content process of SIPE in chromatogram test and external standard method sample:
Take by weighing half delustring section sample that 1g handles well through aforementioned pre-treatment process in the volumetric flask of 100ml, add water to scale, shake up the back and place, get above-mentioned solution 10m in the volumetric flask of another 100ml, add water to scale, shake up the back and place set aside for use.Then draw a certain amount of liquid to be measured with syringe, filter through the water filtrator of 0.45 μ m, squeeze into then in the sample bottle of 1.5ml and carry out the liquid chromatography test, the volume in the sample bottle remains on about 1.0ml.Through chromatogram test, obtain half delustring section chromatogram as shown in Figure 3, by chromatogram with reference to described SIPE canonical plotting and adopt external standard method can obtain the actual content of SIPE in the half delustring section sample.
Take by weighing water-soluble section sample that 1g handles well through aforementioned pre-treatment process in the volumetric flask of 100ml, add water to scale, shake up the back and place, get above-mentioned solution 10m in the volumetric flask of another 100ml, add water to scale, shake up the back and place set aside for use.Then draw a certain amount of liquid to be measured with syringe, filter through the water filtrator of 0.45 μ m, squeeze into then in the sample bottle of 1.5ml and carry out the liquid chromatography test, the volume in the sample bottle remains on about 1.0ml.Through chromatogram test, obtain water-soluble section chromatogram as shown in Figure 4, by chromatogram with reference to described SIPE canonical plotting and adopt external standard method can obtain the actual content of SIPE in the water-soluble section sample.
Take by weighing kation section sample that 1g handles well through aforementioned pre-treatment process in the volumetric flask of 100ml, add water to scale, shake up the back and place, get above-mentioned solution 10m in the volumetric flask of another 100ml, add water to scale, shake up the back and place set aside for use.Then draw a certain amount of liquid to be measured with syringe, filter through the water filtrator of 0.45 μ m, squeeze into then in the sample bottle of 1.5ml and carry out the liquid chromatography test, the volume in the sample bottle remains on about 1.0ml.Through chromatogram test, obtain kation section chromatogram as shown in Figure 5, by chromatogram with reference to described SIPE canonical plotting and adopt external standard method can obtain the actual content of SIPE in the kation section sample.
Embodiment two, and the method for SIPE content in a kind of rp-hplc determination modified poly ester of the present invention is that with the difference of embodiment one chromatographic condition of the reversed-phased high performace liquid chromatographic that is adopted is:
A. chromatographic column is selected Shim-Pack VP-ODS C18 post for use, specification 250mm * 4.6mm, filler granularity 5 μ m;
B. with the volume ratio of methyl alcohol and 0.1% phosphate aqueous solution be 40: 60 as chromatogram flow phase; Flow rate of mobile phase is 1.5ml/min; Carry out gradient elution;
C. column temperature is 40 ℃, and it is 220nm that used UV-detector detects wavelength, and sampling volume is 20 μ L.
Embodiment three, and the method for SIPE content in a kind of rp-hplc determination modified poly ester of the present invention is that with the difference of embodiment one chromatographic condition of the reversed-phased high performace liquid chromatographic that is adopted is:
A. chromatographic column is selected Shim-Pack VP-ODS C 18 posts for use, specification 250mm * 4.6mm, filler granularity 5 μ m;
B. with the volume ratio of methyl alcohol and 0.2% phosphate aqueous solution be 70: 30 as chromatogram flow phase; Flow rate of mobile phase is 0.7ml/min; Carry out gradient elution;
C. column temperature is 40 ℃, and it is 220nm that used UV-detector detects wavelength, and sampling volume is 5 μ L.
Embodiment four, and the method for SIPE content in a kind of rp-hplc determination modified poly ester of the present invention is that with the difference of embodiment one chromatographic condition of the reversed-phased high performace liquid chromatographic that is adopted is:
A. chromatographic column is selected Shim-Pack VP-ODS C18 post for use, specification 250mm * 4.6mm, filler granularity 5 μ m;
B. with the volume ratio of methyl alcohol and 0.13% phosphate aqueous solution be 10: 90 as chromatogram flow phase; Flow rate of mobile phase is 2ml/min; Carry out gradient elution;
C. column temperature is 40 ℃, and it is 220nm that used UV-detector detects wavelength, and sampling volume is 16 μ L.
Embodiment five, and the method for SIPE content in a kind of rp-hplc determination modified poly ester of the present invention is that with the difference of embodiment one chromatographic condition of the reversed-phased high performace liquid chromatographic that is adopted is:
A. chromatographic column is selected Shim-Pack VP-ODS C18 post for use, specification 250mm * 4.6mm, filler granularity 5 μ m;
B. with the volume ratio of methyl alcohol and 0.18% phosphate aqueous solution be 90: 10 as chromatogram flow phase; Flow rate of mobile phase is 0.5ml/min; Carry out gradient elution;
C. column temperature is 40 ℃, and it is 220nm that used UV-detector detects wavelength, and sampling volume is 8 μ L.
The foregoing description only is used for further specifying the method for SIPE content in a kind of rp-hplc determination modified poly ester of the present invention; but the present invention is not limited to embodiment; every foundation technical spirit of the present invention all falls in the protection domain of technical solution of the present invention any simple modification, equivalent variations and modification that above embodiment did.
Claims (3)
1. the method for SIPE content in the rp-hplc determination modified poly ester is characterized in that: comprising:
M-phthalic acid in modified poly ester binaryglycol ester-5-sulfonate (SIPE) is decomposed the pre-treatment step of coming out;
The testing procedure that adopts reversed-phased high performace liquid chromatographic to test;
Wherein, the reversed-phase high-performance liquid chromatography test comprises following chromatographic condition:
A. chromatographic column is selected Shim-Pack VP-ODS C18 post for use, specification 250mm * 4.6mm, filler granularity 5 μ m;
B. with the volume ratio of methyl alcohol and 0.1～0.2% phosphate aqueous solution be 10: 90～90: 10 as chromatogram flow phase; Flow rate of mobile phase is 0.5～2ml/min; Carry out gradient elution;
C. column temperature is 40 ℃, and it is 220nm that used UV-detector detects wavelength, and sampling volume is 5～20 μ L.
2. the method for SIPE content in a kind of rp-hplc determination modified poly ester according to claim 1 is characterized in that: the chromatographic condition of described reversed-phase high-performance liquid chromatography test is:
A. chromatographic column is selected Shim-Pack VP-ODS C18 post for use, specification 250mm * 4.6mm, filler granularity 5 μ m;
B. with the volume ratio of methyl alcohol and 0.15% phosphate aqueous solution be 50: 50 as chromatogram flow phase; Flow rate of mobile phase is 1ml/min; Carry out gradient elution;
C. column temperature is 40 ℃, and it is 220nm that used UV-detector detects wavelength, and sampling volume is 10 μ L.
3. the method for SIPE content in a kind of rp-hplc determination modified poly ester according to claim 1 is characterized in that: the described pre-treatment process of coming out that the binaryglycol ester of m-phthalic acid in the modified poly ester-5-sulfonate (SIPE) is decomposed is the alcoholysis of employing ethylene glycol (EG).
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Cited By (3)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN104807772A (en) * | 2015-04-28 | 2015-07-29 | 上海大学 | Method for analyzing monosaccharide composition of secretion of bdelloid rotifer |
| CN106066371A (en) * | 2015-04-09 | 2016-11-02 | 青岛中科荣达新材料有限公司 | A kind of three monomer liquid chromatograph rapid analysis methods |
| 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 |
-
2007
- 2007-04-29 CN CNA2007100089373A patent/CN101294935A/en active Pending
Cited By (5)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN106066371A (en) * | 2015-04-09 | 2016-11-02 | 青岛中科荣达新材料有限公司 | A kind of three monomer liquid chromatograph rapid analysis methods |
| CN106198830A (en) * | 2015-04-09 | 2016-12-07 | 泰山医学院 | A kind of method of liquid chromatographic detection three monomer |
| CN106066371B (en) * | 2015-04-09 | 2018-07-06 | 青岛中科荣达新材料有限公司 | A kind of three monomer liquid chromatogram rapid analysis methods |
| CN104807772A (en) * | 2015-04-28 | 2015-07-29 | 上海大学 | Method for analyzing monosaccharide composition of secretion of bdelloid rotifer |
| 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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Open date: 20081029 |