CN105181849B - Method for measuring content of aminocaproic acid in caprolactam with high-performance liquid chromatography - Google Patents
Method for measuring content of aminocaproic acid in caprolactam with high-performance liquid chromatography Download PDFInfo
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- CN105181849B CN105181849B CN201510645276.XA CN201510645276A CN105181849B CN 105181849 B CN105181849 B CN 105181849B CN 201510645276 A CN201510645276 A CN 201510645276A CN 105181849 B CN105181849 B CN 105181849B
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Abstract
The invention discloses a method for measuring the content of aminocaproic acid in caprolactam with high-performance liquid chromatography. The method is an analysis method for quantitatively analyzing the content of aminocaproic acid with an external standard method with the adoption of a mobile phase acetonitrile-buffer salt mixed solution system commonly used in reversion phase chromatography. Chromatographic conditions of the method are as follows: a chromatographic column is CAPCELL CORE PC S2.7 (2.1mml.d*150 mm); a mobile phase is prepared from a mixed solution and 10 mmol/L buffer salt through isocratic elution, and a volume ratio of the mixed solution to the 10 mmol/L buffer salt is 98:2; the flow velocity is 0.4 mL/min; the detection wavelength is 200 nm; the column temperature is 40 DEG C; the injection volume is 20 mu L. The method fills the technological blank of the aminocaproic acid measuring method in the field of caprolactam and has the advantages of simple sample processing and analyzing process, high accuracy of an analysis result, good reproducibility and the like.
Description
Technical field
The invention belongs to analysis technical field, is related to a kind of method of measure aminocaproic acid content, it is specially a kind of to adopt
The analysis method of high performance liquid chromatography aminocaproic acid content in amide oil in caprolactam production process.
Background technology
Aminocaproic acid (C6H13NO2), in preparing process of caprolactam, mainly in acid or alkaline medium, in water
In the presence of caprolactam hydrolysis and obtain.
In neutralization reactor, two strands of materials, respectively rearrangement solution (containing concentrated sulphuric acid) and gas ammonia are had, if both are mixed
Close uneven, local overacidification certainly will be caused or alkali is crossed, and N-process generates certain water, make the condition that caprolactam is hydrolyzed into
It is ripe, produce a certain amount of by-product aminocaproic acid.
The density of aminocaproic acid when content is sufficiently high, often causes organic faciess between caprolactam and ammonium sulfate
Layering with inorganic phase is difficult, obvious emulsion occurs, not only increases the consumption of caprolactam and thiamine, after also increasing
The load of continuous extract and separate, and then affect the quality of finished product caprolactam.Thus aminocaproic acid during caprolactam technology
Measure is just particularly important.
At present the measure of aminocaproic acid concentrates on biological medicine aspect, and in the application of caprolactam industry, there is not been reported；
And at present the assay method of aminocaproic acid mostly is before post or after post-column derivation, then it is measured, method is complex.
The content of the invention
The purpose of the present invention is for problem above, there is provided using amino in high effective liquid chromatography for measuring caprolactam oneself
The method of acid content.
To solve above-mentioned technical problem, the technical solution adopted in the present invention is：It is a kind of to be surveyed using high performance liquid chromatography
The method for determining aminocaproic acid content in caprolactam, it is characterised in that comprise the following steps：
1) prepared by standard liquid：Aminocaproic acid standard substance is accurately weighed, is dissolved with pure water, after constant volume, then be with volumetric concentration
80% acetonitrile is configured to the standard liquid of variable concentrations for diluent；
2) standard curve is set up：Chromatograph of liquid zero point is calibrated with sample blank liquid, with determination sample identical liquid phase color
Spectral condition determination step 1) in standard liquid, instrument draws standard curve automatically；
3) prepared by sample solution：Sample 2.5g ± 0.0001g are weighed, with pure water 25mL is settled to, obtain A liquid, then from A
5mL is taken in liquid, with the acetonitrile that volumetric concentration is 80% 25mL is settled to, obtain B liquid；
4) sample determination：After the baseline stability of liquid chromatograph instrument, standard liquid and B liquid are determined, first inject standard liquid, noted twice
After entering the area change of standard liquid less than 1%, B liquid measure is carried out, the injection B liquid in the middle of the injection of standard liquid twice；
5) write down step 4 respectively) in per pin standard liquid, the area of B liquid, calculate the content of aminocaproic acid in B liquid with external standard method,
And aminocaproic acid content in sample is calculated according to extension rate.
Described liquid phase chromatogram condition is：
Chromatographic column：CAPCELL CORE PC S2.7；
Mobile phase：The buffer salt solution of mixed solution and 10mmol/L by volume 98：2 prepare, isocratic elution；
Flow velocity：0.4mL/min；
Detection wavelength：200nm；
Column temperature：40℃；
Sample size：20μL.
Further, described mixed solution adopt volumetric concentration for 95% acetonitrile solution and 10mmol/L buffer salt
Solution by volume 85：15 are formulated；The 10mmol/L buffer salt solutions are using potassium dihydrogen phosphate and phosphoric acid hydrogen two
Sodium solution by volume 1:1 mixed preparing is formed.
The specification of the CAPCELL CORE PC S2.7 posts is：2.1mml.d×150mm.
Step 1) described in variable concentrations be respectively 200.32mg/L, 100.16mg/L, 40.064mg/L, 20.032mg/
L、10.016mg/L。
The sample is crude amide oil intermediate products in caprolactam production.
The present invention has the principle of absorption using aminocaproic acid at ultraviolet region wavelength 200nm, with UV-detector
Hplc determination caprolactam production in crude amide oil in aminocaproic acid content.Using the stream commonly used in reversed phase chromatography
Dynamic phase acetonitrile-buffer salt mixed solution system, quantified by external standard method analysis aminocaproic acid content, the method has filled up caprolactam neck
The technological gap of domain aminocaproic acid assay method, simple with sample treatment and analysis process, analysis result accuracy is high, reappears
The advantages of property is good.
Description of the drawings
Fig. 1 is the chromatogram spectrogram of standard liquid, and 10.449min appearances are aminocaproic acid peak in figure.
Fig. 2 is the chromatogram spectrogram of sample preparation gained B liquid, and 10.334min appearances are aminocaproic acid peak in figure.
Specific embodiment
With reference to embodiment and attached Fig. 1 and 2, the present invention is further elucidated.
Embodiment 1：
The method of aminocaproic acid content, concretely comprises the following steps in a kind of employing high effective liquid chromatography for measuring caprolactam：
The analysis method of liquid chromatography for measuring aminocaproic acid content
1st, mobile phase is selected and Detection wavelength is selected：
1) the choice experiment result of mobile phase shows：Buffer salt content increase, mixed sample appearance time quickly, but nothing
Method is separated；Ethane nitrile content increases, and mixed sample appearance time is slow, but peak shape is poor, takes into account separating effect and analysis time, adopt with
Lower elution requirement：Mixed solution：10mmol/L buffer salt=98：2(V/V)；Wherein mixed solution adopts volumetric concentration for 95%
Acetonitrile solution and 10mmol/L buffer salt by volume 85：15 are formulated；10mmol/L buffer salts adopt biphosphate
Potassium solution and disodium phosphate soln by volume 1:1 mixed preparing is formed.
2) selection of Detection wavelength
Continuously scanned in 190-800nm with ultraviolet-uisible spectrophotometer, aminocaproic acid has feature to inhale at 200nm
Receive, therefore determine that Detection wavelength is 200nm.
2nd, the preparation of standard solution
2.0032g aminocaproic acid standard substance are accurately weighed, in being placed in 1000mL volumetric flasks, is dissolved with pure water, and constant volume, shake
It is even, obtain the standard reserving solution that concentration is 2003.2mg/L；
Standard reserving solution 10mL is taken, with 80% acetonitrile 100mL is settled to, obtain concentration for 200.32mg/L standard specimen 1#；
Standard reserving solution 5mL is taken, with 80% acetonitrile 100mL is settled to, obtain concentration for 100.16mg/L standard specimen 2#；
Standard reserving solution 2mL is taken, with 80% acetonitrile 100mL is settled to, obtain concentration for 40.064mg/L standard specimen 3#；
Standard reserving solution 1mL is taken, with 80% acetonitrile 100mL is settled to, obtain concentration for 20.032mg/L standard specimen 4#；
Mark 1# standard liquids 5mL are taken, with 80% acetonitrile 100mL is settled to, obtain concentration for 10.016mg/L standard specimen 5#.
3rd, calibration trace is set up
Chromatograph of liquid zero point is calibrated with sample blank liquid, standard specimen is determined with determination sample identical liquid phase chromatogram condition
1#, 2#, 3#, 4#, 5# solution, instrument draws calibration trace automatically.
4th, prepared by sample solution
Amide oil 2.5g is taken, is dissolved with pure water, and be settled to 25mL, shaken up, obtain solution A；5mL is pipetted from solution A, is used
80% acetonitrile is settled to 25mL, shakes up, and obtains sample solution B liquid.
5th, chromatograph of liquid condition setting：
Instrument is Agilent liquid chromatograph 1260,
Mobile phase is mixed solution：10mmol buffer salt=98：2, isocratic elution；
Flow velocity：0.4mL/min；
Detection wavelength：200nm；
Detector：Ultraviolet-visible detector；
Column temperature：40℃；
Sample size：20μL；
CAPCELL CORE PC S2.7,2.1mml.d × 150mm.
6th, sample determination：After the baseline stability of instrument, standard liquid and B liquid are determined, first inject standard liquid, standard liquid is injected twice
After area change is less than 1%, B liquid measure is carried out, the injection B liquid in the middle of the injection of standard liquid twice.
The chromatogram of wherein standard specimen is shown in Fig. 1, and the chromatogram of B liquid is shown in Fig. 2, and according to external standard method aminocaproic acid in B liquid is calculated
Content is 42.63mg/L, and it is 0.1060wt% to calculate aminocaproic acid content in sample according to extension rate.
7th, standard recovery test is shown in Table 1
Table 1
Conclusion：The conclusion of mark-on reclaims:The response rate is 92% -106%, meets analysis demand.
8th, precision test
To with portion sample METHOD FOR CONTINUOUS DETERMINATION 10 times with optimal conditions, relative standard deviation is 3.45%.
The embodiment is interpreted as being merely to illustrate the present invention rather than for limiting the scope of the invention.Reading
After the content of record of the present invention, those skilled in the art can make various changes or modifications to the present invention, these equivalent changes
Change and modification equally falls into claims of the present invention limited range.
Claims (4)
1. in a kind of employing high effective liquid chromatography for measuring caprolactam aminocaproic acid content method, it is characterised in that include
Following steps：
1）It is prepared by standard liquid：Aminocaproic acid standard substance is accurately weighed, is dissolved with pure water, after constant volume, then be 80% with volumetric concentration
Acetonitrile is configured to the standard liquid of variable concentrations for diluent；
2）Set up standard curve：Chromatograph of liquid zero point is calibrated with sample blank liquid, with determination sample identical liquid chromatograph bar
Part determination step 1）In standard liquid, instrument draws standard curve automatically；
3）It is prepared by sample solution：2.5 g of sample ± 0.0001g are weighed, with pure water 25mL is settled to, obtain A liquid, then from A liquid
In take 5mL, be settled to 25mL with the acetonitrile that volumetric concentration is 80%, obtain B liquid；
4）Sample determination：After the baseline stability of liquid chromatograph instrument, standard liquid and B liquid are determined, first inject standard liquid, twice injection mark
After the area change of liquid is less than 1%, B liquid measure is carried out, the injection B liquid in the middle of the injection of standard liquid twice；
5）Step 4 is write down respectively）In per pin standard liquid, the area of B liquid, calculate the content of aminocaproic acid in B liquid, and root with external standard method
Aminocaproic acid content in sample is calculated according to extension rate；
Described liquid phase chromatogram condition is：
Chromatographic column：CAPCELL CORE PC S2.7；
Mobile phase：The buffer salt of mixed solution and 10mmol/L by volume 98：2 prepare, isocratic elution；
Flow velocity：0.4mL/min；
Detection wavelength：200nm；
Column temperature：40℃；
Sample size：20μL；
Mixed solution in described mobile phase adopt volumetric concentration for 95% acetonitrile solution and 10mmol/L buffer salt by body
Product compares 85：15 are formulated；The 10mmol/L buffer salts press volume using potassium dihydrogen phosphate and disodium phosphate soln
Than 1:1 mixed preparing is formed.
2. method according to claim 1, it is characterised in that：The specification of the CAPCELL CORE PC S2.7 posts is：
2.1mml.d×150mm。
3. method according to claim 1, it is characterised in that：Step 1）Described in variable concentrations be respectively 200.32mg/
L、100.16mg/L、40.064mg/L、20.032mg/L、10.016mg/L。
4. the method according to claim 1-3 any one, it is characterised in that：The sample is caprolactam production
Middle crude amide oil intermediate products.
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| CN111122720B (en) * | 2019-12-11 | 2022-09-02 | 湖北三宁碳磷基新材料产业技术研究院有限公司 | Method for analyzing caprolactam, 6-aminocaproamide and 6-aminocapronitrile |
| CN114166982B (en) * | 2021-11-15 | 2023-11-10 | 北京百奥药业有限责任公司 | Method for simultaneously determining dimer, trimer and caprolactam in aminocaproic acid injection |
| CN117092254B (en) * | 2023-10-18 | 2024-01-26 | 吉林四环制药有限公司 | Method for detecting impurities in aminocaproic acid or preparation thereof |
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