CN103880902A - Preparation method of natamycin acicular crystal - Google Patents
Preparation method of natamycin acicular crystal Download PDFInfo
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- CN103880902A CN103880902A CN201410094966.6A CN201410094966A CN103880902A CN 103880902 A CN103880902 A CN 103880902A CN 201410094966 A CN201410094966 A CN 201410094966A CN 103880902 A CN103880902 A CN 103880902A
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- tennecetin
- suspension
- natamycin
- needle crystal
- water
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Abstract
The invention provides a preparation method of a natamycin acicular crystal, which comprises the following steps: adding natamycin in water, regulating the pH value to 1-3 or 11-13, stirring until the natamycin is completely dissolved, slowly regulating the pH value to 4-10 within 5-120 minutes (being too fast or too slow is not beneficial to formation of the acicular crystal), continuing stirring for 20-40 minutes to obtain a natamycin acicular crystal suspension, and drying the suspension to obtain the natamycin acicular crystal. The obtained sample has high suspension stability in water or 75% ethanol, does not precipitate for a long time, thus, is convenient to use, and has favorable market application prospects in corrosion resistance of food.
Description
(1) technical field
The present invention relates to a kind of preparation method of tennecetin needle crystal.
(2) background technology
Tennecetin (Natamycin) has another name called natamycin, pimaricin or (horse) mycin (Pimaricin), it is a kind of microbiotic through fermentative production by Streptomyces natalensis, belong to polyene macrolides material, the narrow spectrum inhibition yeast of energy and mould, stop the formation of filamentous fungus aflatoxin.Tennecetin is amphiprotic substance, has a basic group and an acidic-group in molecule, and iso-electric point is 6.5.In water and in polar organic solvent, solubleness is very low, is insoluble to non-polar solvent, and the solubleness under room temperature in water is 30～50mg/L, and in the time of pH>9 or <3, solubleness increases.Solubleness just because of tennecetin is low, and available its surface on food processes to increase effective period of food quality does not but affect local flavor and the mouthfeel of food.At present, tennecetin has been approved in the production and preservation of the numerous food products such as some milk-product, meat, beverage, fruit as a kind of natural biological antiseptic agent.
The formulation being applied at present in food antiseptic is pre-mixture, suspension, its main drawback is that tennecetin solubleness in water or ethanol is extremely low, thereby generation sedimentation, cause tennecetin can not be evenly distributed in water or ethanolic soln, and tennecetin dosage is very low in the time of application, be generally 0.03%～0.05%, so even if vigorous stirring can not make tennecetin be evenly distributed in solution, thereby the result of use of having influence on.More seriously, while taking suspension spray, tennecetin solid also can also usually can stop up shower nozzle, causes using inconvenient.Therefore, problem demanding prompt solution is how to make tennecetin be distributed in equably in solution at present.Although add the assistant agents such as tensio-active agent can increase the homogeneity of tennecetin in solution, need increase cost.
(3) summary of the invention
Plate crystal for existing tennecetin crystallization, in solution, suspension is bad, thereby cause the inconvenience on using, the object of the invention is to change the crystal form of tennecetin, make tennecetin crystallization become the needle crystal of 0.2～20nm from macrobead plate crystal, increase the suspension of tennecetin in solution, so easy to use.
The technical solution used in the present invention is:
A kind of preparation method of tennecetin needle crystal, described method is as follows: tennecetin (plate crystal) is added in the aqueous solution, adjust pH is 1～3 or 11～13, after stirring is dissolved it completely, in 5min～120min, slowly (too soon or too slow all formation of unfavorable needle crystal) adjusts pH to 4～10 again, continue to stir 20～40min, obtain the suspension of tennecetin needle crystal, suspension drying obtains tennecetin needle crystal.The crystallization obtaining is needle-like or cylindric, and mean size is 0.2～20nm, or also the crystal of acquisition can be suspended in to (gained crystal has good suspension in 75% ethanol or water) use in 75% ethanol or water.Regulate pH value, can adopt acid or the alkali of this area routine, common acid has HCl, H
2sO
4, HNO
3, H
3pO
4deng, common alkali has NaOH, KOH, NH
4oH, Na
3pO
4deng, be preferably HCl and NaOH, also can be with other common bronsted lowry acids and bases bronsted lowries.
Preferably, in water, the addition of tennecetin is 20～100g/L water.
Preferably, described method is as follows: tennecetin is added in the aqueous solution, adjust pH is 1～3 or 11～13, after stirring is dissolved it completely, in 10min～90min, slowly adjust again pH to 6～8, continue to stir 20～40min, obtain the suspension of tennecetin needle crystal, the spray-dried acquisition tennecetin of suspension needle crystal.
Preferably, be suspended in again water or 75%(v/v after obtaining described tennecetin needle crystal) for subsequent use in ethanol.
Preferably, the present invention is with NaOH or the HCl adjust pH of 1～2M.
Beneficial effect of the present invention is mainly reflected in: adopt the inventive method, the sample obtaining is suspending stabilized good in water or 75% ethanol, do not precipitate for a long time, thus easy to use, on food antiseptic, there is good market application foreground.
(4) brief description of the drawings
Fig. 1 is that under microscope, new silver resembles tennecetin crystallization photo (10 × 40).
Fig. 2 is that new silver resembles tennecetin X-ray spectrogram.
Fig. 3 is tennecetin needle crystal photo (10 × 40) under microscope.
Fig. 4 is the X-ray spectrogram of tennecetin needle crystal.
Fig. 5 is that new silver resembles tennecetin product HPLC color atlas.
Fig. 6 is aciculiform tennecetin product HPLC color atlas.
(5) embodiment
Below in conjunction with specific embodiment, the present invention is described further, but protection scope of the present invention is not limited in this:
Embodiment 1:
Getting tennecetin product (content 93.5%) 36g being produced by Zhejiang Silver Elephant Bioengineering Co., Ltd. joins in 1000mL beaker, add again water 900mL, under normal temperature, stir, drip 2M HCl105mL simultaneously, being stirred to tennecetin dissolves completely, slowly add again the about 100mL of 2M NaOH, to pH6.5, be controlled at the interior interpolation of 80min complete.Continue to stir 30min.Obtain the suspension of needle crystal.Direct spraying is dry, obtains sample 39.5g, and tennecetin content is 82.3%.
Embodiment 2:
Getting tennecetin product (content 93.5%) 36g being produced by Zhejiang Silver Elephant Bioengineering Co., Ltd. joins in 1000mL beaker, add again water 900mL, under normal temperature, stir, drip 2M NaOH105mL simultaneously, being stirred to tennecetin dissolves completely, slowly add again the about 100mL of 2M HCl, to pH6.5, be controlled at the interior interpolation of 60min complete.Continue to stir 30min.Obtain the suspension of needle crystal.After centrifugal, add deionized water and suspend, spraying is dry, obtains sample 36.4g, and tennecetin content is 90.7%.
Embodiment 3:
The tennecetin needle crystal sample that embodiment 1 and 2 is obtained resembles tennecetin sample with new silver and carries out suspension stability test, test-results (tennecetin dosage is 1g/L, and solvent is 75% ethanol, places after stirring) as shown in table 1.Embodiment 2 tennecetin needle crystal samples are shown in respectively Fig. 1～Fig. 6 with micro-collection of illustrative plates, X-ray figure and HPLC spectrogram that new silver resembles tennecetin sample.
Table 1
From table 1, the needle crystal tennecetin that the present invention makes, suspending stabilized good in 75% ethanol, do not precipitate for a long time more convenient use compared with plate crystal.
Claims (5)
1. the preparation method of tennecetin needle crystal, described method is as follows: tennecetin is added in the aqueous solution, adjust pH is 1～3 or 11～13, after stirring is dissolved it completely, in 5min～120min, slowly adjust again pH to 4～10, continue to stir 20～40min, obtain the suspension of tennecetin needle crystal, suspension drying obtains tennecetin needle crystal.
2. the method for claim 1, the addition that it is characterized in that tennecetin in water is 20～100g/L water.
3. method as claimed in claim 2, it is characterized in that described method is as follows: tennecetin is added in the aqueous solution, adjust pH is 1～3 or 11～13, after stirring is dissolved it completely, in 10min～90min, slowly adjust behind pH to 6～8 again, continue to stir 20～40min, obtain the suspension of tennecetin needle crystal, the spray-dried acquisition tennecetin of suspension needle crystal.
4. method as claimed in claim 3, is suspended in water or 75% ethanol after it is characterized in that obtaining described tennecetin needle crystal again.
5. method as claimed in claim 3, is characterized in that NaOH or HCl adjust pH with 1～2M.
Priority Applications (1)
| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| CN201410094966.6A CN103880902A (en) | 2014-03-14 | 2014-03-14 | Preparation method of natamycin acicular crystal |
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| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| CN201410094966.6A CN103880902A (en) | 2014-03-14 | 2014-03-14 | Preparation method of natamycin acicular crystal |
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|---|---|
| CN103880902A true CN103880902A (en) | 2014-06-25 |
Family
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Family Applications (1)
| Application Number | Title | Priority Date | Filing Date |
|---|---|---|---|
| CN201410094966.6A Pending CN103880902A (en) | 2014-03-14 | 2014-03-14 | Preparation method of natamycin acicular crystal |
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Cited By (3)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN109232689A (en) * | 2017-07-11 | 2019-01-18 | 浙江新银象生物工程有限公司 | A kind of pimaricin superfine powder and its preparation method and application |
| WO2020029168A1 (en) * | 2018-08-09 | 2020-02-13 | 浙江新银象生物工程有限公司 | Natamycin superfine powder, preparation method therefor and use thereof |
| CN112585150A (en) * | 2018-08-16 | 2021-03-30 | 帝斯曼知识产权资产管理有限公司 | Novel epolyonic amphomacrolides and process for purifying natamycin |
Citations (3)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| US5231014A (en) * | 1991-08-05 | 1993-07-27 | Bio-Technical Resources | Fermentation process for producing natamycin |
| CN1515678A (en) * | 2003-08-25 | 2004-07-28 | 天津科技大学 | Preparation method of natamycin |
| CN101048510A (en) * | 2004-10-28 | 2007-10-03 | 帝斯曼知识产权资产管理有限公司 | Stable needle-shaped crystals of natamycin |
-
2014
- 2014-03-14 CN CN201410094966.6A patent/CN103880902A/en active Pending
Patent Citations (3)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| US5231014A (en) * | 1991-08-05 | 1993-07-27 | Bio-Technical Resources | Fermentation process for producing natamycin |
| CN1515678A (en) * | 2003-08-25 | 2004-07-28 | 天津科技大学 | Preparation method of natamycin |
| CN101048510A (en) * | 2004-10-28 | 2007-10-03 | 帝斯曼知识产权资产管理有限公司 | Stable needle-shaped crystals of natamycin |
Cited By (4)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN109232689A (en) * | 2017-07-11 | 2019-01-18 | 浙江新银象生物工程有限公司 | A kind of pimaricin superfine powder and its preparation method and application |
| WO2020029168A1 (en) * | 2018-08-09 | 2020-02-13 | 浙江新银象生物工程有限公司 | Natamycin superfine powder, preparation method therefor and use thereof |
| CN112585150A (en) * | 2018-08-16 | 2021-03-30 | 帝斯曼知识产权资产管理有限公司 | Novel epolyonic amphomacrolides and process for purifying natamycin |
| CN112585150B (en) * | 2018-08-16 | 2024-03-29 | 帝斯曼知识产权资产管理有限公司 | New epoxypolyene ampholytic macrolides and process for purifying natamycin |
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Application publication date: 20140625 |