• 专利附录
  • 专利说明
  • 权利要求
  • 类似技术
  • 同族专利
  • 引用文献
  • 法律状态
  • 优先权
    • 专利摘要:
    This invention relates to formulations applied to food and medicine as a protective coating. Purpose . the invention is an improvement in the release of the β-active substance with a pH of 1.5-3.0. The composition contains a pH-sensitive vinyl-2-pyridine styrene or methyl-2-vinyl-5-pyridine styrene copolymer of 67-70% and a cellulose acetobutyrate that is not sensitive to pH changes or 30-33%. Granulated methionite is coated with a protective coating of the indicated composition, at the same time granules are characterized by a methionine content of 75.9%, and 73% in the control. The ability to extract in water is 15.4% after 16 hours, 23.7% after 48 hours. Extraction in acidic medium at pH 1.5-71% after 15 minutes; 98% after 30 min and 100% after 1 h, respectively, in the control 42, 71 and 85%. Table 1: § O)
    公开号:SU1428178A3
    申请号:SU823501204
    申请日:1982-10-06
    公开日:1988-09-30
    发明作者:Отан Пьер；Катиллье Андре；Кентен Жан-Пьер
    申请人:Аец Сосьете Де Шими Органик Э Биоложик (Фирма)；
    IPC主号:
    专利说明:

     Yu
    00
    00
     s
    This invention relates to formulations applied to products, medicines as a protective rim. .
    The purpose of the invention is improvement. the release of the active substance at a pH of 1.5-3.0.,
    This goal is achieved by the fact that, in the quality of a styrene-spinnered copolymer, the protective coating composition contains a pH-sensitive vinyl-2-pyridine styrene or methyl-2-vinyl-5-pyridine styrene copolymer and additionally insensitive to pH changes acetobutyrate polymer cellulose or ethyldellulose in the following ratio of components, (wt.%):
    Vinyl-2-pyridinestirol or methyl 2-win11L-5-pyridine-styrene67-70 Cellulose acetobutyrate or
    ethyldellulose 30-33 Example 1. A protective sheath is coated with 400 g of granulated methionine in the form of spherical particles titrated to 98% with a diameter of 0.5 0.63 mm by boiling: a layer of 872 g of a protective sheath consisting of 70 parts of a vinyl copolymer -2- pyridinestirol (70-30) and 30 h of cellulose acetobutyrate.
    Granules with the following characteristics are obtained: methionine content 75.9 D%; ability to be extracted in water 15.4% after 16 hours j 23.7% after 48 hours; resistance in the first chamber of the ruminant stomach 78.7%
    48
    extractive ability
    acid in pH 1.5 71% after 15 min, 98% after 30 min, 100% after 1 h.
    As a comparison, granules obtained from 400 g of methionine and 72 g of vinyl-2-pyridine styrene copolymer have the following properties: methionine content 73%, ability to be extracted in water 20.3% after 16 h, 31.3% after 48 h; resistance in the first chamber of the ventricle of ruminants 70% after 48 h, method-. The ability to be extracted in an acidic medium at pH 1.5 42% after 15 min, 71% after 30 min, 85% after 1 h
    Pellets coated with a protective coating containing 70% vinyl copolymer 2-pyridinestirol and 30% acetobutyrate cellulose were tested on fistula sheep, while covered with protective
    five
    0
    five
    0
    five
    0
    5 Q

    shell methionine was injected into the first chamber of the stomach through the fistula. Animals receive a dose of 6 g per day or 12 g per day for 5 days, then no pellets are administered to the animals the following week (control week). The determination of absorbed methionine is carried out by means of its content in the blood at the end of the week. The blood methionine content is expressed in 1 mg of methionine per 100 g of blood. At a dose of 6 g per day, the blood content is 6.9 mg / 100 g of blood, and at a dose of 12 g per day it is 13.4 mg / 100 g of blood, while with the introduction of free methionine, the content in the blood is is 1.32 and 1.61 mg per -100 g of blood.
    From this it follows that with a dose of 12 g per day, the content of methionine in the blood increases 8.3 times, and with a dose of 6 g per day increases 5.3 times.
    The composition of the protective sheath is obtained as follows.
    50.4 g of a vinyl-2-pyridine styrene copolymer and 22.6 g of cellulose acetobutyrate in 1200 cm of tetrahydrofuran are dispersed, then 1.5 g of dibutylphthalate and 0.07 g of dye are added.
    When completely dissolved, sufficient N-acetypethanolamine is added to ensure that the resistivity of the solution is less than or equal to. See.
    The solution is then applied to the methionine to be coated in a device that allows the application of a protective coating in a fluidized bed of air.
    The vinyl-2-pyridine styrene copolymer used in the containment shell was prepared as follows.
    14 g of met1-cellulose are dissolved in 9334 g of distilled water in a 25 liter reactor. The solution is heated to 60 ° C, then a mixture of 1200 g of styrene, 2800 g of vinyl-2-pyridine and 40 g of azodiisobutyronitrile is added with stirring at 150 rpm. With stirring, the temperature is maintained (60-63 C) for 4 hours and 30 minutes. The slurry is then dehydrated. The polymer obtained is washed in distilled water and dried at 60 ° C under reduced pressure of 3100 ml of mercury. Art. to constant weight.
    3-142,8178
    Thus, get 3,630 kg
    styrene-vinyl-2-pyridine copolymer (28.6-71.4) with a specific viscosity of 0.520 Oe (determination in solution of dimethylformamide 5g / l at 23 ° C) and with a weight mole. weighing about 410,000. The polymerization factor is 91%.
    Cellulose acetobutyrate has the following properties: the average molecular weight is 57,000, the content of the groups: acetate 1.2; Butirate 1.8 is not a cellulose unit.
    Example 2. Proceed as in example 1, but using 1200 g of granulated methionine, titrated to 98%, thus obtaining granules with the following characteristics: methionine content 77.5% j ability to be extracted in water at 10.7% after 16 h, 21% after 48 h; resistance in the first chamber of the ruminant's stomach after 48 hours;
    Example 3. A protective sheath is coated with 400 g of granulated methionine in the form of titrated to 98%.
    with spherical particles with a diameter of 0.5-0.63 mm using a fluidized bed technology of 120 g of a protective shell consisting of 70 hours of Vinsh1-2-pyridine styrene copolymer (70-30) and 30 hours of acetobutyr
    10 that pulp.
    In addition, under the same conditions, a control product is carried out, the protective shell of which consists of 100% of a vinyl-2-pyridine-15 styrene copolymer (70-30).
    So get the granules with the characteristics summarized in the table ..
    Example 4. Cover with protective
    20 shells 400 g of granulated methionine in the form of titrated to 98% spherical units with a diameter of 0.5-0.63 mm using fluidized bed technology of 80 g of a protective shell consisting of
    the ability to be extracted in acidic 25 of 70 parts of a copolymer of vinyl-2-pyridine medium at pH 1.5 94% after 15 min, 98% after 30 min, 100% after 1 h.
    These granules are subjected to fistulase chewing. The coated methionine is fed through the fistula for 1 week and added to the concentrated feed for 1 week. Between these two weeks, one week is established, corresponding to the control period (no methionine added).
    Different levels of methionine in the blood are caused by chewing action. This is recorded
    decrease in the content of methionine in the blood by 13-15%.
    The granules thus obtained are tested in preparing feed for chickens with a content of 0.2% (preparation of 100 kg of feed in a Gondar mixer). The percentage of methionine that is able to be extracted in the ved in the prepared feed corresponds to the percentage obtained for the initial coating of methionine. So for 2 hours, the percentage of methionine capable of being extracted in water (relative to the methionine present) is 3.8% in the feed, while it is 4.4% for the initial coated methionine.
    Example 3. A protective sheath is coated with 400 g of granulated methionine in the form of titrated to 98%.
    spherical particles with a diameter of 0.5-0.63 mm using a fluidized bed technology of 120 g of a protective shell consisting of 70 h of Vinsh1-2-pyridin-styrene copolymer (70-30) and 30 h of cellulose acetobutyrate.
    In addition, under the same conditions, a control product is carried out, the protective sheath of which consists of 100% of a vinyl-2-pyridine styrene copolymer (70-30).
    So get the granules with the characteristics summarized in the table ..
    Example 4. Cover with protective
    shell 400 g of granulated methionine in the form of titrated to 98% spherical units with a diameter of 0.5-0.63 mm using fluidized bed technology of 80 g of a protective shell consisting of
    from 70 including copolymer of vinyl-2-pyridine
    styrene 20 hours, cellulose acetobutyrate and 10 hours benzene dicarboxylic acid.
    Get granules with the following characteristics: the content of methionine 66.3%; the ability to be extracted in water 5.2% for 16 hours, 8.3% for 48 hours; resistance in the first chamber of the ventricle crap 64.0% after 48 h; the ability to be extracted in an acidic environment
    at pH 1.5 77% after 15 min, 95% setting 30 min, 100% after 1 h; at pHZ 10.5% after 15 min, 16% after 30 min, 28% after 1 hour.
    At the same time, the product coated with only vinyl-2-pyridine styrene copolymer (70-30), under the conditions described in example 1, has the following extraction rate at a pH of 36% after 15 minutes, 8%
    after 30 min, 15% after 1 h.
    Example 5: A protective sheath is coated with 400 g of granulated methionine in the form of spherical particles titrated to 98% with a diameter of 0.5-0.63 mm using a fluidized bed technology of 72 g of a protective shell consisting of 70 h. Vinsh-1-2-pyridine-styrene copolymer (90-10) and 30 parts of cellulose acetobutyrate.
    Thus, granules with the following characteristics are obtained: the content of methionine is 72.2%; the ability to be extracted in water 11.8% for 1.6 h, 24.5% for 48 h; sustainability in
    514281786
    the first chamber of the stomach of ruminants 85.5% ronitrile. After A h 30 min heating; after 48 h; the capacity of extraction at 60 ° С with mixing is con sistent in an acidic medium at pH 1.5 with a speed of 150 rpm; the polymer is curtailed — 85.6% after 15 min, 100% after 30 min, s. After selection, found at 100% after 1 h; at pH 3 5% after 15 min, 15% after 30 min, 26% 1h.
    Example 6, Top Protective
    7 liters of dimethylformamide are added to the surface of the liquid.
    The resulting solution is poured into water at the rate of 1 liter of solution per 10 l of water. The precipitated polymer is dewatered, washed in distilled water and dried at a reduced pressure (too mm Hg) until a constant weight is obtained.
    ten
    The resulting solution is poured into water at the rate of 1 liter of solution per 10 l of water. The precipitated polymer is dewatered, washed in distilled water and dried at a reduced pressure (too mm Hg) until a constant weight is obtained.
    In this way, 4200 g of copolymer metsch1-5-vinyl-2-pyridine styrene (77.3-22.6) with a specific viscosity of 0.486 are obtained (determined in solution 20 at 5 g / l of dimethylformamide at). The polymerization factor is 84%.
    15
    400 g granulated shell; methion in the form of spherical particles titrated to 98% with a diameter of 0.5-0.63 mm using a fluidized bed technology of 120 g of a protective shell consisting of a mixture of 67 parts of methyl 2-vinyl-5-pyridine styrene copolymer (77.4 -22.6) and 33 parts ethylcellulose.
    Thus, granules with the following characteristics are obtained: the content of methion is 66.2%; the ability to be extracted in water 11.3% for 16 hours, 20.1% for 48 hours; resistance in the first chamber of the ruminant stomach
    权利要求:
    Claims (1)
    [1]
    84% after 48 hours, extractive ability. The formula of the invention is cut in an acidic medium at pH 1.5 25 27% after 15 minutes, 50% after 30 minutes, 66% after 1 hour.
    While the granules obtained from 400 g of methionine and 120 g of the copolymer of methyl-2-vinyl-5-pyridines, have the following characteristics: the content of methionine 62.9%; the ability to be extracted in water 14.5% after 16 h, 20.1% after 48 h; the ability to be extracted in an acidic medium at pH 1.5 18% after 15 min, 35% after 30 min, 48% after 1 hour.
    A methyl-2-vinsh-5-pyridine-styrene copolymer (77-23) can be prepared as follows.
    Into a 25 liter reactor, 17.5 g of methylcellulose is dissolved in 11667 g of distilled water. The solution is heated until a mixture of 1050 g of styrene, 3950 g of methyl-2- 45 vinyl-5-pyridine and 50 g of azodiisobuth is added. Composition of protective coating for biologically active substances containing styrene vinyl pyridine
    copolymers.
    distinguishing 30
    so that, in order to improve the release of the active substance at a pH of 1.5-3.0, the composition as a styrene vinylpyridine copolymer contains a pH-sensitive copolymer of vinyl-2-pyridine styrene or methyl-2-vinyl-5-pyridine styrene, which is sensitive to 35 and cellulose acetobutyrate or ethylcellulose 40, which is additionally insensitive to pH changes, in the following ratio of components, wt%:
    Sinil-2-pyridinestirol or methyl-2-vinyl-5-pyridin-styrene67-70
    Cellulose Acetabutyrate
    or ethylcellulose 30-33
    ronitrile. After A h 30 min heating at 60 ° C with stirring with a speed of 150 rpm, the polymer coagulates. After being selected,
    7 liters of dimethylformamide are added to the surface of the liquid.
    The resulting solution is poured into water at the rate of 1 liter of solution per 10 l of water. The precipitated polymer is dewatered, washed in distilled water and dried at a reduced pressure (too mm Hg) until a constant weight is obtained.
    In this way, 4200 g of copolymer metsch1-5-vinyl-2-pyridine styrene (77.3-22.6) with a specific viscosity of 0.486 are obtained (determined in solution at 5 g / l of dimethylformamide at). The polymerization factor is 84%.
    Invention Formula
    Protective coating composition for biologically active substances containing styrenovinyl-pyridine
    copolymers.
    featuring 45
    thirty
    so that, in order to improve the release of the active substance at a pH of 1.5-3.0, the composition as a styrene vinylpyridine copolymer contains a pH-sensitive copolymer of vinyl-2-pyridine styrene or methyl-2-vinyl-5-pyridine styrene, which is sensitive to 35 and acetobutyrate of cellulose or ethyl cellulose 40 which is also insensitive to changes in pH of the polymer in the following ratio of components, wt%:
    Sinil-2-pyridinestirol or methyl-2-vinyl-5-pyridin-styrene67-70
    Cellulose Acetabutyrate
    or ethylcellulose 30-33
    Indicators
    Methion content,%
    The ability to be extracted in water,%, after, h 16
    - 48
    Stability in the first chamber of the ruminant stomach, 7 ° - after 48 h
    Ability to be extracted in acidic medium at pH 1.5,% after 15 min.
    30 min
    1h
    Methioninemia
    (} 2 g / day x 7 day
    1 mg of methionine per 100 g of blood
    A coated product containing cellulose acetobutyrate
    62.5
    7.1 19.1
    86
    24 45 47
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    引用文献:
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    法律状态:
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