CN103787909A - High performance liquid chromatography resolution method for metalaxyl racemes - Google Patents
High performance liquid chromatography resolution method for metalaxyl racemes Download PDFInfo
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- CN103787909A CN103787909A CN201210423165.0A CN201210423165A CN103787909A CN 103787909 A CN103787909 A CN 103787909A CN 201210423165 A CN201210423165 A CN 201210423165A CN 103787909 A CN103787909 A CN 103787909A
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- performance liquid
- liquid chromatography
- high performance
- metalaxyl
- metaxanin
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Abstract
The invention discloses a high performance liquid chromatography resolution method for metalaxyl racemes. The method is characterized in that a high performance liquid chromatography system is used; cellulose-tris(3,5-dimethylphenylcarbamate) is used as a filler and methanol and water are used as a mobile phase, to resolve high-pure R-(+)-metalaxyl and S-(-)-metalaxyl from racemes of metalaxyl. The method is high in automatic degree and high in production efficiency.
Description
Technical field
The invention belongs to biological medicine technology field, be specifically related to a kind of method for splitting of metaxanin enantiomorph.
Background technology
Metaxanin (Metalaxy1), chemical name is N-(2-methoxy methyl ethanoyl)-N-(2,6-3,5-dimethylphenyl)-DL-Amino Acid methyl esters.Metaxanin is new and effective systemic fungicide, can interior inspiration enter in plant, the general sterilant of water-soluble ratio is much higher, can penetrate the cytolemma of the oomycetes that new fat is little, play germicidal action, downy mildew in Oomycete and phytophthora are had to selectivity special efficacy, for example, the late blight of potato, downy mildew of garpe, hop downy mildew, beet epidemic disease, white rust of colza, black shank etc. are had to good prevention effect.Can be used for the oidium such as melon, vegetables, grape, tobacco, the late blight of potato, tobacco apple scab etc., the lasting period is long.Also can be used for cotton samping off, the downy mildew of millet, prevention effect is also very good.Metaxanin is racemic modification, its levo form (R body) has the more bactericidal properties of Gao Gengqiang, levo form (R body) is applied to phytopathogen, killing pathogenic bacteria is more thorough, and duration of efficacy is longer more for a long time, so just reduce spraying times. increase spraying cycle, improved drug effect, saved cost, reduced the pollution to environment.Although metaxanin just starts to enter Chinese market from the eighties mid-term, to the research of its fractionation at present also in the analysis phase.Thereby the method for setting up fractionation metaxanin racemic modification has very large economic and social benefits.
Summary of the invention
The object of this invention is to provide a kind of method for splitting of highly effective liquid phase chromatographic system of metaxanin enantiomorph.
The technical scheme that the present invention adopts is for achieving the above object as follows: a kind of method for splitting of high performance liquid chromatography of metaxanin enantiomorph, it is characterized in that with Mierocrystalline cellulose-tri-(3,5-3,5-dimethylphenyl carbamate) be stationary phase, with the mixture of first alcohol and water be moving phase, from metaxanin racemoid, split out highly purified R-metaxanin and S-metaxanin with highly effective liquid phase chromatographic system, comprise step:
(1) metaxanin racemic modification is dissolved in moving phase, concentration is: 0～100mg/ml;
(2) split metaxanin racemic modification with highly effective liquid phase chromatographic system;
(3) concentrate and obtain highly purified two kinds of metaxanin enantiomorphs.
The present invention has following technique effect: the present invention adopts highly effective liquid phase chromatographic system, splits out the metaxanin enantiomorph with optical purity from the racemic modification of metaxanin, and technique is simple, constant product quality, solvent adopts methyl alcohol, recoverable, pollution-free, realize cleaner production.
Embodiment
1, chromatographic column filler and moving phase (solvent) are selected
Filler fibre element-tri-(3,5-3,5-dimethylphenyl carbamate) application type chiral stationary phase, adopt known method (Okamoto Y, Kawashima M, Hatada K J. Chromatomgr .1986,363:173 ~ 186) preparation, filler granularity is 1 ~ 150um, particulate is less, and size distribution is narrower, is more conducive to separate; But more mini system pressure is larger for particle diameter, and optimum particle size range is 10 ~ 30um.
Moving phase (solvent) is the mixture of first alcohol and water.
2, separating step
Sample dissolves by moving phase, concentration is 0 ~ 100mg/ml, adopt Semipreparative chromatography instrument to carry out separation and purification, Mierocrystalline cellulose-tri-(3,5. 3,5-dimethylphenyl carbamate) filler is Hanbon Sci. & Tech. Co., Ltd.'s product, and particle diameter is 10um, and moving phase is first alcohol and water, isocratic elution.The detection wavelength of the New UV Spectrophotometric detector adopting is 330nm, collects metaxanin, through HPLC purity assay >=98.0%.
Embodiment 1
Sample dissolves by moving phase, concentration is 20mg/ml, adopt Semipreparative chromatography instrument to carry out separation and purification, column size is Φ 10 × 250mm, and Mierocrystalline cellulose-tri-(3,5. 3,5-dimethylphenyl carbamate) filler is Hanbon Sci. & Tech. Co., Ltd.'s product, particle diameter is 10um, applied sample amount 10mg, and moving phase is methyl alcohol: water=80:20, isocratic elution.The detection wavelength of the New UV Spectrophotometric detector adopting is 330nm, collects metaxanin, through HPLC purity assay >=98.0%.
Embodiment 2
Sample dissolves by moving phase, concentration is 50mg/ml, adopt Semipreparative chromatography instrument to carry out separation and purification, column size is Φ 20 × 250mm, and Mierocrystalline cellulose-tri-(3,5. 3,5-dimethylphenyl carbamate) filler is Hanbon Sci. & Tech. Co., Ltd.'s product, particle diameter is 10um, applied sample amount 80mg, and moving phase is methyl alcohol: water=85:15, isocratic elution.The detection wavelength of the New UV Spectrophotometric detector adopting is 330nm, collects metaxanin, through HPLC purity assay >=98.2%.
Embodiment 3
Sample dissolves by moving phase, concentration is 100mg/ml, adopt Semipreparative chromatography instrument to carry out separation and purification, column size is Φ 20 × 250mm, and Mierocrystalline cellulose-tri-(3,5. 3,5-dimethylphenyl carbamate) filler is Hanbon Sci. & Tech. Co., Ltd.'s product, particle diameter is 10um, applied sample amount 120mg, and moving phase is methyl alcohol: water=88:12, isocratic elution.The detection wavelength of the New UV Spectrophotometric detector adopting is 330nm, collects metaxanin, through HPLC purity assay >=98.2%.
Claims (4)
1. the high performance liquid chromatography method for splitting of a metaxanin enantiomorph, it is characterized in that: adopt high performance liquid chromatography separation system, moving phase is first alcohol and water, type of elution isocratic elution, chromatographic column filler is Mierocrystalline cellulose-tri-(3,5. 3,5-dimethylphenyl carbamate), filler granularity 10 ~ 30um, service temperature is 20 ~ 40 ℃.
2. method according to claim 1, is characterized in that: methyl alcohol is chromatographically pure.
3. method according to claim 1, is characterized in that: volume ratio (V/V) scope of mobile phase methanol and water is 7:3 ~ 9:1.
4. method according to claim 1, is characterized in that described optimum service temperature is 30 ℃.
Priority Applications (1)
| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| CN201210423165.0A CN103787909A (en) | 2012-10-30 | 2012-10-30 | High performance liquid chromatography resolution method for metalaxyl racemes |
Applications Claiming Priority (1)
| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| CN201210423165.0A CN103787909A (en) | 2012-10-30 | 2012-10-30 | High performance liquid chromatography resolution method for metalaxyl racemes |
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| CN103787909A true CN103787909A (en) | 2014-05-14 |
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Family Applications (1)
| Application Number | Title | Priority Date | Filing Date |
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| CN201210423165.0A Pending CN103787909A (en) | 2012-10-30 | 2012-10-30 | High performance liquid chromatography resolution method for metalaxyl racemes |
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Cited By (2)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN104745509A (en) * | 2015-03-25 | 2015-07-01 | 浙江工业大学 | Pseudochrobactrum asaccharolyticum WZZ003 and application thereof |
| CN108863835A (en) * | 2018-07-03 | 2018-11-23 | 浙江禾本科技有限公司 | A kind of solvent and its application method purifying Metalaxyl-M |
-
2012
- 2012-10-30 CN CN201210423165.0A patent/CN103787909A/en active Pending
Cited By (3)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN104745509A (en) * | 2015-03-25 | 2015-07-01 | 浙江工业大学 | Pseudochrobactrum asaccharolyticum WZZ003 and application thereof |
| CN104745509B (en) * | 2015-03-25 | 2017-08-25 | 浙江工业大学 | Sugar vacation anthropi WZZ003 and its application are not understood |
| CN108863835A (en) * | 2018-07-03 | 2018-11-23 | 浙江禾本科技有限公司 | A kind of solvent and its application method purifying Metalaxyl-M |
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Application publication date: 20140514 |