CN105675783A - HPLC (high-performance liquid chromatography) analysis method of 3-aminobutanol chiral purity - Google Patents

HPLC (high-performance liquid chromatography) analysis method of 3-aminobutanol chiral purity Download PDF

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CN105675783A
CN105675783A CN201610043274.8A CN201610043274A CN105675783A CN 105675783 A CN105675783 A CN 105675783A CN 201610043274 A CN201610043274 A CN 201610043274A CN 105675783 A CN105675783 A CN 105675783A
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amino butanol
chiral purity
methyl
analytical procedure
alpha
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CN105675783B (en
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孙凤霞
孔琳
王美玲
韩珊
张琛
白少玲
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Hebei University of Science and Technology
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Hebei University of Science and Technology
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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
    • G01N30/88—Integrated analysis systems specially adapted therefor, not covered by a single one of the groups G01N30/04 - G01N30/86
    • 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
    • G01N30/88—Integrated analysis systems specially adapted therefor, not covered by a single one of the groups G01N30/04 - G01N30/86
    • G01N2030/8809—Integrated analysis systems specially adapted therefor, not covered by a single one of the groups G01N30/04 - G01N30/86 analysis specially adapted for the sample
    • G01N2030/884—Integrated analysis systems specially adapted therefor, not covered by a single one of the groups G01N30/04 - G01N30/86 analysis specially adapted for the sample organic compounds

Abstract

The invention belongs to the technical field of pharmaceutical analysis and particularly relates to an HPLC (high-performance liquid chromatography) analysis method of 3-aminobutanol chiral purity.The HPLC analysis method of the 3-aminobutanol chiral purity includes enabling a (R)-alpha-methyl-2-naphthyl acetyl chloride derivatization reagent and 3-aminobutanol to undergo rapid double-derivatization reaction, and determining the chiral purity by high-performance liquid chromatography and ultraviolet combination.The HPLC analysis method of the 3-aminobutanol chiral purity has the advantages of mild reaction conditions, rapidity, high detection sensitivity, good repeatability, easiness in standardized operation and capability of being used for detecting the 3-aminobutanol chiral purity effectively, thereby being promising in actual popularization application prospect.

Description

The HPLC analytical procedure of a kind of 3-amino butanol chiral purity
Technical field
The invention belongs to pharmaceutical analysis technical field, it is specifically related to the HPLC analytical procedure of a kind of 3-amino butanol chiral purity.
Background technology
HPLC detection method has detection sensitivity height, tolerance range height, and detection required time is few, and detected result repeatability advantages of higher is detection means conventional in present analysis chemistry.
(R)-3-amino butanol is the important intermediate of synthesis Du Lutewei. Du Lutewei is anti-AIDS (HIV) new drug under Britain pharmacy giant Ge Lan element SmithKline (GSK), Food and Drug Administration of the U.S. on August 12 (FDA) in 2013. Preclinical study result display degree Lu Tewei has stronger anti-HIV-1 virus activity, and security and tolerance are good.
Wu Shengwen etc. (CN201410488279.2) use Carbobenzoxy Chloride and 3-amino butanol derivatize to generate N-Cbc-3-amino butanol, Liquid Detection under 210nm. Chromatographic column AD-H; Moving phase normal hexane: Virahol (9:1); Retention time S-isomer 11.1 minutes, R-isomer 12.2 minutes, uses expensive normal phase column in process. 3-amino butanol is carried out derivatize with o-phthalaldehyde(OPA)-thiol derivatives by R.H.BUCK etc. (Journalofchromatography), chromatographic condition: KnauerHypersilODS pillar, moving phase 0.05% sodium phosphate buffer salts solution/methyl alcohol (volume ratio 35/65), pH7.0, fluoroscopic examination. And by carrying out two derivatize fast with the chiral reagent of band uv-absorbing, obtain the derivative that existing uv-absorbing has again three chiral radicals, it is possible in reversed phase high efficiency liquid phase and ultraviolet coupling, directly carry out the analysis of isomer.
Du Lutewei molecular structure has two chiral centres, introduce by chiral source (R)-3-amino butanol, the relative content of Du Lutewei two diastereomers only depends on the relative energy height producing their transition states, owing to generating (4R, 12aS) transition state energy relatively (4R, 12aR) isomer is low, therefore reacts the product finally generating and being configured as master with (4R, 12aS). Another isomer in (R)-3-amino butanol that low optical is pure, four chipal compounds can be generated in the reaction, reducing the chiral purity of Du Lutewei, therefore the optical purity of (R)-3-amino butanol directly determines that the optical purity of Du Lutewei, impurity is how many and anti-AIDS effect. Although this kind of new drug listing time is very short, but cause the heavy demand to this kind of new drug due to its efficient anti-AIDS effect, thus cause the heavy demand to Du Lutewei chiral source (R)-3-amino butanol.Owing to 3-amino butanol molecular structure of compounds is containing a primary amine and a hydroxyl, without uv-absorbing, set up efficiently, optical purity analysis method difficulty very big accurately and reliably, therefore (R)-3-amino butanol is detected analysis accurately, significant for synthesis new drug Du Lutewei.
Summary of the invention
It is an object of the invention to overcome the defect of prior art, it is provided that the HPLC analytical procedure of a kind of 3-amino butanol chiral purity, it is possible to fast realize qualitative, quantitative and enantiomeric excess rate analysis accurately.
In order to realize above-mentioned purpose, the technical scheme that the present invention takes is as follows:
A HPLC analytical procedure for 3-amino butanol chiral purity, specifically comprises following steps:
Step one, derivatize
3-amino butanol is dissolved in organic solvent, under certain temperature condition, taking (R)-alpha-methyl-2-naphthalene Acetyl Chloride 98Min. as derivatization reagent, the mol ratio of control 3-amino butanol and (R)-alpha-methyl-2-naphthalene Acetyl Chloride 98Min., carry out derivative reaction, obtaining the 3-amino butanol after derivatize, reaction formula is shown in formula I;
Formula I
Step 2, separation detection
Adopt reversed phase high efficiency liquid phase chromatogram-UV-detector that the 3-amino butanol after derivatize carries out qualitative, quantitative and enantiomeric excess rate mensuration.
One or more the combination that described organic solvent is selected from toluene, dimethylbenzene, sherwood oil, methylene dichloride, 1,2-ethylene dichloride, tetrahydrofuran (THF), chloroform and tetracol phenixin.
The volume ratio of described organic solvent and 3-amino butanol is 0.1 ~ 300:1, it is preferable to 1 ~ 20:1.
Described certain temperature refers to from-10 DEG C to reflux temperature, it is preferable to 15 ~ 35 DEG C.
The concrete numerical value of the reflux temperature of the present invention is relevant with the selection of organic solvent, and those skilled in the art can clearly determine the scope of reflux temperature according to the selection of solvent.
The mol ratio of described 3-amino butanol and (R)-alpha-methyl-2-naphthalene Acetyl Chloride 98Min. is 1:2 ~ 20.
The determined wavelength of described UV-detector is 210 ~ 300nm, it is preferable that 220 ~ 260nm.
The chromatographic column that described reversed phase high efficiency liquid phase chromatogram uses is common reversed-phase column. Preferably, chromatographic column is anti-phase C18 post, it is most preferred that be the anti-phase C18 post of enlightening horse (250 × 4.6mm, 5 μm, pH scope 2.0 ~ 8.0).
The moving phase of described reversed phase high efficiency liquid phase chromatogram is made up of buffer salt solution and organic solvent, organic solvent be selected from methyl alcohol, ethanol, Virahol and acetonitrile one or both; It is 20% ~ 80% that organic solvent accounts for the volume ratio scope of moving phase, it is preferable that scope is 40% ~ 60%.
The buffering salt of described moving phase be selected from Sodium phosphate dibasic, SODIUM PHOSPHATE, MONOBASIC, dipotassium hydrogen phosphate, potassium primary phosphate one or both, the quality volumetric concentration of buffered saline solution is 0.01% ~ 5%, it is preferable to 0.1% ~ 1%.
The pH value of described buffered saline solution is 2.0 ~ 7.0, it is preferable that pH value is 4.0 ~ 6.0.
Described flow rate of mobile phase is at 0.2 ~ 3.0mL/min, it is preferable that flow velocity is 1.0mL/min.
In the present invention, rp-hplc analysis condition is preferably:
Enlightening horse C18 chromatographic column, moving phase is 40% acetonitrile-60% buffered saline solution, buffered saline solution to be quality volumetric concentration be 0.1% biphosphate sodium water solution, pH value is 4.5; Ultraviolet detection wavelength is 254nm, and flow velocity is 1.0mL/min, and post temperature is 30 DEG C, sampling volume 20 μ L.
Compared with prior art, useful effect acquired by the present invention is as follows:
The present invention gives the derivatization method of 3-amino butanol, by control reaction conditions, generate the derivative of (R)-alpha-methyl-2-naphthalene Acetyl Chloride 98Min. and 3-amino butanol fast, and establish the HPLC (high performance liquid chromatography) to the qualitative, quantitative of the 3-amino butanol after (R)-alpha-methyl-2-naphthalene Acetyl Chloride 98Min. derivatize and enantiomerism body measurement.The method is simple to operate, favorable reproducibility, highly sensitive, accuracy are strong, is convenient to normalizing operation. By the 3-amino butanol after (R)-alpha-methyl-2-naphthalene Acetyl Chloride 98Min. derivatize carries out qualitative, quantitative and enantiomeric excess rate analysis, thus realize the qualitative, quantitative of 3-amino butanol and enantiomeric excess rate (chirality e.e. value) being analyzed.
Accompanying drawing explanation
Fig. 1: color atlas after (R)-alpha-methyl-2-naphthalene Acetyl Chloride 98Min. and (RS)-3-amino butanol derivatize;
In the accompanying drawings: 1 is the derivative of (R)-alpha-methyl-2-naphthalene Acetyl Chloride 98Min. with (R)-3-amino butanol; 2 derivatives spread out for (R)-alpha-methyl-2-naphthalene Acetyl Chloride 98Min. and (S)-3-amino butanol.
Embodiment
Below in conjunction with accompanying drawing, the present invention carried out detailed further describing.
Embodiment 1:(R) liquid-phase chromatographic analysis of derivative of-alpha-methyl-2-naphthalene Acetyl Chloride 98Min. and (RS)-3-amino butanol
Get (RS)-3-amino butanol 3.09g (0.03mol), it is dissolved in 60mL methylene dichloride, stir at 30 DEG C, slowly add (R)-alpha-methyl-2-naphthalene Acetyl Chloride 98Min. 26.23g (0.12mol). TLC monitors reaction, and reaction is steamed after terminating and done to obtain (R)-alpha-methyl-2-naphthalene Acetyl Chloride 98Min. and (RS)-3-amino butanol derivative.
Adopt high performance liquid chromatography to carry out detection after (R)-alpha-methyl-2-naphthalene Acetyl Chloride 98Min. and (RS)-3-amino butanol derivative moving phase being dissolved to analyze. Liquid phase chromatogram condition: enlightening horse C18 chromatographic column, moving phase is 40% acetonitrile-60% buffered saline solution, buffered saline solution to be quality volumetric concentration be 0.1% biphosphate sodium water solution, pH value is 4.5. Ultraviolet detection wavelength is 254nm, and flow velocity is 1.0mL/min, and post temperature is 30 DEG C, and sampling volume 20 μ L, retention time and chiral purity analysis in table 1, Fig. 1 is shown in by its collection of illustrative plates.
3-amino butanol retention time after table 1 (R)-alpha-methyl-2-naphthalene Acetyl Chloride 98Min. derivatize and chirality e.e.% value
The investigation test of the derivative reaction condition of embodiment 2:3-amino butanol and (R)-alpha-methyl-2-naphthalene Acetyl Chloride 98Min.
2-1: get (RS)-3-amino butanol 3.09g (0.03mol), is dissolved in 40mL chloroform, stirs, slowly add (R)-alpha-methyl-2-naphthalene Acetyl Chloride 98Min. 13.12g (0.06mol) at 40 DEG C. TLC monitors reaction, and reaction is steamed after terminating and done to obtain (R)-alpha-methyl-2-naphthalene Acetyl Chloride 98Min. and (RS)-3-amino butanol derivative.
Adopt high performance liquid chromatography to carry out detection after (R)-alpha-methyl-2-naphthalene Acetyl Chloride 98Min. and (RS)-3-amino butanol derivative moving phase being dissolved to analyze. Liquid phase chromatogram condition: enlightening horse C18 chromatographic column, moving phase is 40% acetonitrile-60% buffered saline solution, buffered saline solution to be quality volumetric concentration be 0.1% biphosphate sodium water solution, pH value is 4.5. Ultraviolet detection wavelength is 254nm, and flow velocity is 1.0mL/min, and post temperature is 30 DEG C, and sampling volume 20 μ L, retention time and chirality e.e.% value are with embodiment 1.
: take (RS)-3-amino butanol 3.09g (0.03mol), it is dissolved in 40mL tetracol phenixin, stir at 30 DEG C, slowly drip and add (R)-alpha-methyl-2-naphthalene Acetyl Chloride 98Min. 19.67g (0.09mol). TLC monitors reaction, and reaction is steamed after terminating and done to obtain (R)-alpha-methyl-2-naphthalene Acetyl Chloride 98Min. and (RS)-3-amino butanol derivative.
Adopt high performance liquid chromatography to carry out detection after (R)-alpha-methyl-2-naphthalene Acetyl Chloride 98Min. and (RS)-3-amino butanol derivative moving phase being dissolved to analyze. Liquid phase chromatogram condition: enlightening horse C18 chromatographic column, moving phase is 40% acetonitrile-60% buffered saline solution, buffered saline solution to be quality volumetric concentration be 0.1% biphosphate sodium water solution, pH value is 4.5.Ultraviolet detection wavelength is 254nm, and flow velocity is 1.0mL/min, and post temperature is 30 DEG C, and sampling volume 20 μ L, retention time and chirality e.e.% value are with embodiment 1.
: get (RS)-3-amino butanol 3.09g (0.03mol), it is dissolved in 30mL1,2-ethylene dichloride, stir at 80 DEG C, slowly add (R)-alpha-methyl-2-naphthalene Acetyl Chloride 98Min. 15.30g (0.07mol). TLC monitors reaction, and reaction is steamed after terminating and done to obtain (R)-alpha-methyl-2-naphthalene Acetyl Chloride 98Min. and (RS)-3-amino butanol derivative.
Adopt high performance liquid chromatography to carry out detection after (R)-alpha-methyl-2-naphthalene Acetyl Chloride 98Min. and (RS)-3-amino butanol derivative moving phase being dissolved to analyze. Liquid phase chromatogram condition: enlightening horse C18 chromatographic column, moving phase is 40% acetonitrile-60% buffered saline solution, buffered saline solution to be quality volumetric concentration be 0.1% biphosphate sodium water solution, pH value is 4.5. Ultraviolet detection wavelength is 254nm, and flow velocity is 1.0mL/min, and post temperature is 30 DEG C, and sampling volume 20 μ L, retention time and chirality e.e.% value are with embodiment 1.
: take (RS)-3-amino butanol 3.09g (0.03mol), it is dissolved in 60mL sherwood oil, stir at 0 DEG C, slowly add (R)-alpha-methyl-2-naphthalene Acetyl Chloride 98Min. 21.86g (0.1mol). TLC monitors reaction, and reaction is steamed after terminating and done to obtain (R)-alpha-methyl-2-naphthalene Acetyl Chloride 98Min. and (RS)-3-amino butanol derivative.
Adopt high performance liquid chromatography to carry out detection after (R)-alpha-methyl-2-naphthalene Acetyl Chloride 98Min. and (RS)-3-amino butanol derivative moving phase being dissolved to analyze. Liquid phase chromatogram condition: enlightening horse C18 chromatographic column, moving phase is 40% acetonitrile-60% buffered saline solution, buffered saline solution to be quality volumetric concentration be 0.1% biphosphate sodium water solution, pH value is 4.5. Ultraviolet detection wavelength is 254nm, and flow velocity is 1.0mL/min, and post temperature is 30 DEG C, and sampling volume 20 μ L, retention time and chirality e.e.% value are with embodiment 1.
: get (RS)-3-amino butanol 3.09g (0.03mol), it is dissolved in 500mL(methylene dichloride: chloroform 1:1) in, stir at 20 DEG C, slowly add (R)-alpha-methyl-2-naphthalene Acetyl Chloride 98Min. 131.16g (0.6mol). TLC monitors reaction, and reaction is steamed after terminating and done to obtain (R)-alpha-methyl-2-naphthalene Acetyl Chloride 98Min. and (RS)-3-amino butanol derivative.
Adopt high performance liquid chromatography to carry out detection after (R)-alpha-methyl-2-naphthalene Acetyl Chloride 98Min. and (RS)-3-amino butanol derivative moving phase being dissolved to analyze. Liquid phase chromatogram condition: enlightening horse C18 chromatographic column, moving phase is 40% acetonitrile-60% buffered saline solution, buffered saline solution to be quality volumetric concentration be 0.1% biphosphate sodium water solution, pH value is 4.5. Ultraviolet detection wavelength is 254nm, and flow velocity is 1.0mL/min, and post temperature is 30 DEG C, and sampling volume 20 μ L, retention time and chirality e.e.% value are with embodiment 1.
Embodiment 3: chromatographic condition investigates test
(1) derivatize
Get (RS)-3-amino butanol 3.09g (0.03mol), it is dissolved in 60mL methylene dichloride, stir at 30 DEG C, slowly add (R)-alpha-methyl-2-naphthalene Acetyl Chloride 98Min. 13.12g (0.06mol). TLC monitors reaction, and reaction is steamed after terminating and done to obtain (R)-alpha-methyl-2-naphthalene Acetyl Chloride 98Min. and (RS)-3-amino butanol derivative.
(2) following different chromatographic condition is adopted to carry out separation detection in (R)-alpha-methyl-2-naphthalene Acetyl Chloride 98Min. and (RS)-3-amino butanol derivative
A. adopt high performance liquid chromatography to carry out detection after (R)-alpha-methyl-2-naphthalene Acetyl Chloride 98Min. and (RS)-3-amino butanol derivative moving phase being dissolved to analyze.Liquid phase chromatogram condition: liquid phase chromatogram condition: enlightening horse C18 chromatographic column, moving phase is 20% acetonitrile-80% buffered saline solution, and buffered saline solution is quality volumetric concentration is the aqueous solution of 5% SODIUM PHOSPHATE, MONOBASIC, and pH value is 3. Ultraviolet detection wavelength is 254nm, and flow velocity is 1.0mL/min, and post temperature is 30 DEG C, and sampling volume 20 μ L, chirality e.e.% value is with embodiment 1.
B. adopt high performance liquid chromatography to carry out detection after (R)-alpha-methyl-2-naphthalene Acetyl Chloride 98Min. and (RS)-3-amino butanol derivative moving phase being dissolved to analyze. Liquid phase chromatogram condition: enlightening horse C18 chromatographic column, moving phase is 20% acetonitrile-80% buffered saline solution, and buffered saline solution is quality volumetric concentration is the potassium dihydrogen phosphate aqueous solution of 5%, and pH value is 5.0. Ultraviolet detection wavelength is 254nm, and flow velocity is 1.0mL/min, and post temperature is 30 DEG C, and sampling volume 20 μ L, chirality e.e.% value is with embodiment 1.
C. adopt high performance liquid chromatography to carry out detection after (R)-alpha-methyl-2-naphthalene Acetyl Chloride 98Min.-and (RS)-3-amino butanol moving phase being dissolved to analyze. Liquid phase chromatogram condition: enlightening horse C18 chromatographic column, moving phase is 80% Virahol-20% buffered saline solution, buffered saline solution to be quality volumetric concentration be 5% biphosphate sodium water solution, pH value is 2.0. Ultraviolet detection wavelength is 254nm, and flow velocity is 1.0mL/min, and post temperature is 30 DEG C, and sampling volume 20 μ L, chirality e.e.% value is with embodiment 1.
D. adopt high performance liquid chromatography to carry out detection after (R)-alpha-methyl-2-naphthalene Acetyl Chloride 98Min. and (RS)-3-amino butanol derivative moving phase being dissolved to analyze. Liquid phase chromatogram condition: enlightening horse C18 chromatographic column, moving phase is 20% methyl alcohol-80% buffered saline solution, buffered saline solution to be quality volumetric concentration be 1% the Sodium phosphate dibasic aqueous solution, pH value is 6.0. Ultraviolet detection wavelength is 254nm, and flow velocity is 1.0mL/min, and post temperature is 30 DEG C, and sampling volume 20 μ L, chirality e.e.% value is with embodiment 1.
E. adopt high performance liquid chromatography to carry out detection after (R)-alpha-methyl-2-naphthalene Acetyl Chloride 98Min. and (RS)-3-amino butanol derivative moving phase being dissolved to analyze. Liquid phase chromatogram condition: enlightening horse C18 chromatographic column, moving phase is 60% ethanol-40% buffered saline solution, and buffered saline solution is quality volumetric concentration is the aqueous dibasic potassium phosphate solution of 0.5%, and pH value is 7.0. Ultraviolet detection wavelength is 254nm, and flow velocity is 1.0mL/min, and post temperature is 30 DEG C, and sampling volume 20 μ L, chirality e.e.% value is with embodiment 1.
The above enforcement mode is only the preferred embodiments of the present invention, and and the feasible enforcement of non-invention exhaustive. For persons skilled in the art, to any apparent change done by it under the prerequisite not deviating from the principle of the invention and spirit, all should be contemplated as falling with within the claims of the present invention.

Claims (10)

1. the HPLC analytical procedure of a 3-amino butanol chiral purity, it is characterised in that, specifically comprise following steps:
Step one, derivatize
3-amino butanol is dissolved in organic solvent, under certain temperature condition, taking (R)-alpha-methyl-2-naphthalene Acetyl Chloride 98Min. as derivatization reagent, the mol ratio of control 3-amino butanol and (R)-alpha-methyl-2-naphthalene Acetyl Chloride 98Min., carry out derivative reaction, obtaining the 3-amino butanol after derivatize, reaction formula is shown in formula I;
Formula I
Step 2, separation detection
Adopt reversed phase high efficiency liquid phase chromatogram-UV-detector that the 3-amino butanol after derivatize carries out qualitative, quantitative and enantiomeric excess rate mensuration.
2. the HPLC analytical procedure of a kind of 3-amino butanol chiral purity according to claim 1, it is characterized in that, one or more the combination that described organic solvent is selected from toluene, dimethylbenzene, sherwood oil, methylene dichloride, 1,2-ethylene dichloride, tetrahydrofuran (THF), chloroform and tetracol phenixin.
3. the HPLC analytical procedure of a kind of 3-amino butanol chiral purity according to claim 1, it is characterised in that, the volume ratio of described organic solvent and 3-amino butanol is 0.1 ~ 300:1, it is preferable that be 1 ~ 20:1.
4. the HPLC analytical procedure of a kind of 3-amino butanol chiral purity according to claim 1, it is characterised in that, described certain temperature refers to from-10 DEG C to reflux temperature, it is preferable to 15 ~ 35 DEG C.
5. the HPLC analytical procedure of a kind of 3-amino butanol chiral purity according to claim 1, it is characterised in that, the mol ratio of described 3-amino butanol and (R)-alpha-methyl-2-naphthalene Acetyl Chloride 98Min. is 1:2 ~ 20.
6. the HPLC analytical procedure of a kind of 3-amino butanol chiral purity according to claim 1, it is characterised in that, the determined wavelength of described UV-detector is 210 ~ 300nm, it is preferable that 220 ~ 260nm.
7. the HPLC analytical procedure of a kind of 3-amino butanol chiral purity according to claim 1, it is characterised in that, the chromatographic column that described reversed phase high efficiency liquid phase chromatogram uses is common reversed-phase column.
8. the HPLC analytical procedure of a kind of 3-amino butanol chiral purity according to claim 1, it is characterized in that, the moving phase of described reversed phase high efficiency liquid phase chromatogram is made up of buffer salt solution and organic solvent, organic solvent be selected from methyl alcohol, ethanol, Virahol and acetonitrile one or both; It is 20% ~ 80% that organic solvent accounts for the volume ratio scope of moving phase, it is preferable that be 40% ~ 60%.
9. the HPLC analytical procedure of a kind of 3-amino butanol chiral purity according to claim 8, it is characterized in that, the buffering salt of described moving phase be selected from Sodium phosphate dibasic, SODIUM PHOSPHATE, MONOBASIC, dipotassium hydrogen phosphate, potassium primary phosphate one or both, the quality volumetric concentration of buffered saline solution is 0.01% ~ 5%, it is preferable that be 0.1% ~ 1%.
10. want the HPLC analytical procedure of a kind of 3-amino butanol chiral purity described in 8 according to right, it is characterised in that, the pH value of the moving phase buffered saline solution of described reversed phase high efficiency liquid phase chromatogram is 2.0 ~ 7.0, it is preferable that pH value be 4.0 ~ 6.0.
CN201610043274.8A 2016-01-23 2016-01-23 A kind of HPLC analysis methods of 3 amino butanol chiral purity Expired - Fee Related CN105675783B (en)

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Cited By (3)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
CN107677735A (en) * 2016-08-02 2018-02-09 上海朴颐化学科技有限公司 A kind of HPLC analysis methods of (S) 2 aminopropanol
CN108845048A (en) * 2018-05-04 2018-11-20 浙江工业大学 It is a kind of for measuring the efficient liquid-phase chromatography method of amino butanol content
CN113820442A (en) * 2021-08-18 2021-12-21 上虞京新药业有限公司 Method for detecting optical purity of chiral enantiomer 2-aminobutyric acid

Cited By (3)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
CN107677735A (en) * 2016-08-02 2018-02-09 上海朴颐化学科技有限公司 A kind of HPLC analysis methods of (S) 2 aminopropanol
CN108845048A (en) * 2018-05-04 2018-11-20 浙江工业大学 It is a kind of for measuring the efficient liquid-phase chromatography method of amino butanol content
CN113820442A (en) * 2021-08-18 2021-12-21 上虞京新药业有限公司 Method for detecting optical purity of chiral enantiomer 2-aminobutyric acid

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