CN1039182C - Producing method for high content water soluble triacontanol melissane solid preparation - Google Patents
Producing method for high content water soluble triacontanol melissane solid preparation Download PDFInfo
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- CN1039182C CN1039182C CN93102086A CN93102086A CN1039182C CN 1039182 C CN1039182 C CN 1039182C CN 93102086 A CN93102086 A CN 93102086A CN 93102086 A CN93102086 A CN 93102086A CN 1039182 C CN1039182 C CN 1039182C
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- triacontanol
- emulsifier
- ammonium
- weight ratio
- cyclodextrin
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Abstract
The present invention relates to a triacontanol preparation. The triacontanol preparation is prepared by the method that an emulsifier and low-grade monohydric alcohol solutions of C1 to C3 are added in triacontanol raw powder for emulsifying by heating, cyclodextrin is added for clathration, and then a mixture of more than one kind of (containing one kind of) fertilizer is used as filling materials. The weight ratio of the triacontanol to the emulsifier to the cyclodextrin to the fertilizer filling materials to the alcohol is 1: (10 to 30): (5 to 15): (50 to 65): (25 to 40). The triacontanol solid preparation with high content and water solubility has the advantages of easy use, no deterioration for long-term storage, high drug effect and stable increase effect in yield.
Description
The present invention relates to a kind of triacontanol preparation.
N-triacontanol (n-triacontanol, CH
3(CH
2)
28CH
2OH is hereinafter to be referred as TA) be a kind of new plant growth regulator that the state college professor Ries.S.K. of Michigan, United States found in 1975.(0.1～0.5ppm) just can play the growth regulating effect to multiple kinds of crops to TA, thereby causes volume increase and improve quality under extremely low concentration.Show according to domestic and international land for growing field crops application data during the last ten years: TA can make wheat, corn, cotton, peanut, oily Lay, tealeaves, celery, tomato, bottle gourd, Jasmine, citrus, sea-tangle and laver etc. increase production significantly, application prospect is very wide, more and more is subjected to various countries scientific worker's attention and peasant's popular welcome.
(25 ℃ the time, TA solvability in water is 9 * 10 because TA is at room temperature water-soluble hardly
-14G/l), therefore under the prerequisite that guarantees the former opaque amount of TA, the practical formulation of TA just becomes the most critical technology that its agricultural is used.The various countries scientific worker uses for the agricultural of quickening TA, has competitively developed the various experiment formulations of TA, as emulsifier formulation and the colloid dispersion formulation of Ries.S.K., the acetone formulation of Welebir.A.J.; Domestic mixing and emulsifying formulation emulsion, the missible oil that Xiamen University is arranged, Jiangxi engineering college missible oil (containing chloroform), emulsifiable paste and other formulations.
Above formulation is divided into two classes substantially: a class is aqua formulation (being emulsion), promptly use a certain amount of emulsifier (mainly being non-ionic surface active agent) TA emulsification in the presence of a small amount of organic solvent (as ethanol, acetone, chloroform etc.), make 0.05%～0.1% (i.e. the aqua of 500～1000PPM) following concentration, thus TA is dispersed in the water; One class is a TA missible oil formulation, promptly uses a large amount of polar organic solvent (as acetone, ethanol etc.), in the presence of emulsifier missible oil is made in TA emulsification.The common drawback of above-mentioned formulation is: be difficult to make the TA preparation of high concentration, poor stability can not long preservation, the drug effect instability; Freight volume is big, and packing, transportation difficulty are greatly.
The present invention aims to provide a kind of high-load, only needs when using just can be diluted to working concentration with the hot water dissolving, and long term storage is never degenerated the manufacture method of the efficient TA solid pharmaceutical preparation that is easy to transport.
Detailed description of the invention
The raw material of high level of water soluble TA solid pharmaceutical preparation of the present invention is TA (N-triacontanol content 〉=85%), emulsifier, cyclodextrin (hereinafter to be referred as CD), chemical fertilizer filler and C
1～C
3Lower alcohol, their proportioning (weight ratio) is 1: (10～30): (5～15): (50～65): (25～40).
The preparation steps of high-load aqueous fusion solid pharmaceutical preparation of the present invention is as follows:
The TA of metering and emulsifier are added in the container, after placing 85～93 ℃ hot bath heated and stirred fusing, 65～80 ℃ the hot low-alcohol solution that adds metering, stirring and emulsifying is to even phase, add CD again and stir inclusion, add the chemical fertilizer mixture filler of more than one (containing a kind of) then and stir into an even transparency liquid.After removing water-bath, under room temperature, be stirred to a pastel,, promptly get high level of water soluble TA 70～75 ℃ of vacuum dryings 5～8 hours.
Emulsifier of the present invention with non-ionic surface active agent for well, the blended emulsifier formed of paregal O and paregal O and other non-ionic surface active agents preferably, as paregal O and sapn, paregal O and tween, paregal O and polyoxyethylene nonylphenol ether etc.Blended emulsifier of the present invention also comprises the blended emulsifier that paregal O and anion surfactant (as tridecyl sodium sulfonate, lauryl sodium sulfate, neopelex etc.) are formed.
What can be used as chemical fertilizer filler of the present invention has ammonium chloride, ammonium nitrate, ammonium sulfate, urea, a potassium sulphate, and potassium chloride, potassium nitrate, potassium dihydrogen phosphate, potassium hydrogen phosphate ammonium etc. are best with urea.
The present invention also can add the trace compound filler, and said trace compound is ammonium molybdate, Boratex, zinc sulphate, zinc chloride etc., with the weight ratio of TA be (0～15): 1.
Low-alcohol solution of the present invention comprises methyl alcohol, ethanol, propyl alcohol, isopropyl alcohol, is best with ethanol.The concentration (concentration expressed in percentage by volume) of alcohol is 50%～80%, and wherein 65%～75% is best.
The preparation steps of TA solid pharmaceutical preparation of the present invention also can adopt the method for emulsification behind the first inclusion, and its preparation steps is as follows:
The TA of metering and low-alcohol solution are added in the container, in the extremely even phase of 85～95 ℃ hot bath heated and stirred, after adding CD stirs inclusion, add emulsifier emulsification again, add filler at last and stir into an even liquid, remove hot bath, under room temperature, be stirred to a pastel, be poured into porcelain dish, in 70～75 ℃ of vacuum drying 5-8 hours, porphyrize slightly, cross 100 mesh sieves, promptly get high levels of water-soluble TA pulvis,, then can make tablet as compression molding.
TA solid pharmaceutical preparation of the present invention is easy to use, and long term storage is never degenerated, the drug effect height, and effect of increasing production is stable.As being mixed with 0.5PPM with prepared TA pulvis, soak the sea-tangle seedling and put in a suitable place to breed after 12 hours, on average to increase production about 40%, the volume increase reason is that sea-tangle length, width, thickness are all compared increase in the same old way, the rate of drying also improves, and has improved quality.On Jasmine, use TA, find that also TA pulvis effect of increasing production of the present invention is better than emulsion (seeing the following form)
| Handle | Cell production (kg) | Summation (kg) | On average (kg) | Folding per mu yield (kg) | Comparison is according to volume increase |
| I II | Kg/ mu % | ||||
| Milk powder (1PPM) emulsion (1PPM) contrast | 4.614 4.464 4.601 4.246 3.668 3.451 | 9.077 8.847 7.119 | 4.534 4.424 3.559 | 303.60 294.93 237.37 | 66.23 27.5 57.56 24.2 / / |
Annotate: the age of tree 3 years, 0.015 mu of sub-district area.Also fine at application effects such as other crop such as peanut, celery Lay, rape, Lai Ye, citrus, corns.
Below further specify the present invention with embodiment.
Embodiment 1
TA and the 4.77g paregal O of 0.23g (purity 87%) are put into the 150ml beaker, place in 95 ℃ of water-baths, heated and stirred is fused and is become to spare a grease, the 50% ethanolic solution 25ml that adds 70 ℃, stir into again and even be added to 2.5g β-CD and stir inclusion, add 12.5g urea again, be stirred to even phase.Remove hot bath, after being stirred to pastel under the room temperature, be poured into porcelain dish, 70 ℃ of vacuum dryings 6 hours.Porphyrize is crossed 100 mesh sieves slightly, promptly gets 1% (10000PPM) TA milk powder.
Get said milk powder 1g and add 95 ℃ of hot water 99g (99ml), stirred 2-3 minute, milk powder all dissolves, and solution is transparent, and TA concentration is 100PPM.
Embodiment 2
Operating procedure such as embodiment 1 only change emulsifier into paregal O 3.22g, Tween-80 1.5g, and other components are constant, can make the 1%TA solid pharmaceutical preparation with blended emulsifier emulsification.
Embodiment 3
TA and the 6g paregal O of 0.46g (purity 87%) are put into the 150ml beaker, after heat fused in 90 ℃ of water-baths becomes an even grease, add 70 ℃ of hot ethanol solution and the 1g lauryl sodium sulfate of 25ml 60%, stir into even phase, add 2.5g β-CD again and stir and comprise, add 10.4g urea at last, stir into even phase, take out beaker, vigorous stirring to a pastel under room temperature, be poured on the porcelain dish, 70 ℃ of vacuum dryings 7 hours.Porphyrize is crossed 100 mesh sieves, promptly gets 2%TA milk powder, and compression molding then gets the 2%TA tablet.
Embodiment 4
Operating procedure such as embodiment 1 change filler into urea 9.5g, ammonium molybdate 3g, and other components are constant, promptly get the TA solid pharmaceutical preparation that contains trace element molybdenum.
Embodiment 5
TA 0.23g (purity 87%) is put into the 150ml beaker, add 70% ethanolic solution 30ml, heated and stirred becomes even phase in 95 ℃ of hot baths, add β-CD 2g and stir inclusion, add 3.22g paregal O and disk-80 2g again, heated and stirred is emulsified into even phase, add urea 12.5g then and be stirred to even phase again, from hot bath, take out beaker, after being stirred to pastel under the room temperature, be poured on the porcelain dish, in 70 ℃ of vacuum dryings 5 hours, porphyrize is crossed 100 mesh sieves, promptly gets 1%TA milk powder, and compressing tablet gets the 1%TA tablet.
Embodiment 6
Operating procedure such as embodiment 1 change filler into the 6g dipotassium hydrogen phosphate, 6.5g urea, and other components are constant, can make the 1%TA pulvis of nitrogenous, phosphorus, potassium.
Embodiment 7
Add 0.92gTA (content 87%) and 7.5g paregal O in the beaker of 200ml, heat fused in 95 ℃ of water-baths stirs into even phase, add 70 ℃ of 50% ethanol water 40ml and 0.6g dodecyl sodium sulfate, continue to be stirred to homogeneous phase, add 4g β-CD and 6.98g urea, stir into homogeneous phase after, remove water-bath, under room temperature, be stirred to pastel, be poured on the porcelain dish, 70 ℃ of vacuum dryings 6 hours, porphyrize is crossed 100 mesh sieves, promptly gets 4%TA milk powder.
Embodiment 8
Operating procedure such as embodiment 1 change filler into 6.5g urea and 6g ammonium chloride, and other components are constant, can make 1%TA milk powder.
Claims (7)
1, a kind of manufacture method of high content water soluble triacontanol melissane solid preparation, it is to add emulsifier and a kind of low-alcohol solution heating emulsification by content 〉=former powder of 85% N-triacontanol to form, feature of the present invention is that said manufacture method also will be with cyclodextrin encapsulated, and is filler with one or more chemical fertilizer mixture; Said emulsifier is the blended emulsifier of a kind of nonionic surface active agent or two kinds of non-ionic surface active agent compositions or the blended emulsifier of a kind of non-ionic surface active agent and a kind of anion surfactant composition, and the weight ratio of TA and emulsifier is 1: (10～30); Said cyclodextrin CD comprises α-CD, β-CD, and γ CD, the weight ratio of TA and CD is 1: (5～15); The weight ratio of said chemical fertilizer and TA is (50～80): 1; Said emulsification and inclusion carry out at 85～95 ℃, and the adding filler also stirs the back temperature and reduces to room temperature, stirs into pastel again, 70～75 ℃ of following vacuum dryings 5～8 hours, gets the TA pulvis of high level of water soluble.
2,, it is characterized in that said lower alcohol is C according to the method for claim 1
1～C
3Monohydric alcohol, be best with ethanol.
3, according to the method for claim 1 and 2, the concentration expressed in percentage by volume that it is characterized in that said lower alcohol is 50%80%, preferably 65%～75%.
4,, it is characterized in that said non-ionic surface active agent is a peregal 0, tween and sapn and polyoxyethylene nonylphenol ether according to the method for claim 1; Anion surfactant is a lauryl sodium sulfate, neopelex, dodecyl sodium sulfate.
5, according to the method for claim 1, it is characterized in that said chemical fertilizer is an ammonium chloride, ammonium nitrate, ammonium sulfate, urea, potassium nitrate, potassium dihydrogen phosphate, dipotassium hydrogen phosphate, the potassium hydrogen phosphate ammonium is best with urea.
6,, it is characterized in that said cyclodextrin is β-CD according to the method for claim 1.
7,, it is characterized in that to add the trace compound filler i.e. ammonium molybdate, Boratex, zinc sulphate according to the method for claim 1; Zinc chloride, with the weight ratio of TA be (0～15): 1.
Priority Applications (1)
| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| CN93102086A CN1039182C (en) | 1993-02-20 | 1993-02-20 | Producing method for high content water soluble triacontanol melissane solid preparation |
Applications Claiming Priority (1)
| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| CN93102086A CN1039182C (en) | 1993-02-20 | 1993-02-20 | Producing method for high content water soluble triacontanol melissane solid preparation |
Publications (2)
| Publication Number | Publication Date |
|---|---|
| CN1078851A CN1078851A (en) | 1993-12-01 |
| CN1039182C true CN1039182C (en) | 1998-07-22 |
Family
ID=4983935
Family Applications (1)
| Application Number | Title | Priority Date | Filing Date |
|---|---|---|---|
| CN93102086A Expired - Fee Related CN1039182C (en) | 1993-02-20 | 1993-02-20 | Producing method for high content water soluble triacontanol melissane solid preparation |
Country Status (1)
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|---|---|
| CN (1) | CN1039182C (en) |
Families Citing this family (1)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN101913951B (en) * | 2010-08-26 | 2013-06-19 | 中国科学院遗传与发育生物学研究所 | Plant photosynthesis promoter and preparation method thereof |
Citations (1)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| GB2230700A (en) * | 1989-04-26 | 1990-10-31 | Sumitomo Chemical Co | Emulsifiable pesticidal or plant growth regulating solid compositions |
-
1993
- 1993-02-20 CN CN93102086A patent/CN1039182C/en not_active Expired - Fee Related
Patent Citations (1)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| GB2230700A (en) * | 1989-04-26 | 1990-10-31 | Sumitomo Chemical Co | Emulsifiable pesticidal or plant growth regulating solid compositions |
Non-Patent Citations (1)
| Title |
|---|
| 植物生长调节剂品种手册 1990.12.1 程暄生，叶亚辉编著;中国农药工业协会 * |
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| Publication number | Publication date |
|---|---|
| CN1078851A (en) | 1993-12-01 |
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