CN104782915A - Method for preparing microelement-beta-cyclodextrin or derivative inclusion compound thereof - Google Patents
Method for preparing microelement-beta-cyclodextrin or derivative inclusion compound thereof Download PDFInfo
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- CN104782915A CN104782915A CN201510193264.8A CN201510193264A CN104782915A CN 104782915 A CN104782915 A CN 104782915A CN 201510193264 A CN201510193264 A CN 201510193264A CN 104782915 A CN104782915 A CN 104782915A
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- CN
- China
- Prior art keywords
- beta
- cyclodextrin
- zinc
- inclusion compound
- trace element
- Prior art date
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- 238000000034 method Methods 0.000 title claims abstract description 48
- 150000001875 compounds Chemical class 0.000 title claims abstract description 29
- 229920000858 Cyclodextrin Polymers 0.000 title claims abstract description 16
- 239000001116 FEMA 4028 Substances 0.000 title claims abstract description 11
- 229960004853 betadex Drugs 0.000 title claims abstract description 11
- 238000001035 drying Methods 0.000 claims abstract description 46
- 238000003756 stirring Methods 0.000 claims abstract description 45
- 239000000843 powder Substances 0.000 claims abstract description 42
- 239000000463 material Substances 0.000 claims abstract description 37
- XLYOFNOQVPJJNP-UHFFFAOYSA-N water Substances O XLYOFNOQVPJJNP-UHFFFAOYSA-N 0.000 claims abstract description 24
- WHGYBXFWUBPSRW-FOUAGVGXSA-N beta-cyclodextrin Chemical compound OC[C@H]([C@H]([C@@H]([C@H]1O)O)O[C@H]2O[C@@H]([C@@H](O[C@H]3O[C@H](CO)[C@H]([C@@H]([C@H]3O)O)O[C@H]3O[C@H](CO)[C@H]([C@@H]([C@H]3O)O)O[C@H]3O[C@H](CO)[C@H]([C@@H]([C@H]3O)O)O[C@H]3O[C@H](CO)[C@H]([C@@H]([C@H]3O)O)O3)[C@H](O)[C@H]2O)CO)O[C@@H]1O[C@H]1[C@H](O)[C@@H](O)[C@@H]3O[C@@H]1CO WHGYBXFWUBPSRW-FOUAGVGXSA-N 0.000 claims abstract description 6
- 239000002245 particle Substances 0.000 claims description 61
- 235000013855 polyvinylpyrrolidone Nutrition 0.000 claims description 31
- 229920000036 polyvinylpyrrolidone Polymers 0.000 claims description 31
- 239000001267 polyvinylpyrrolidone Substances 0.000 claims description 31
- 239000011573 trace mineral Substances 0.000 claims description 27
- 235000013619 trace mineral Nutrition 0.000 claims description 27
- 238000007908 dry granulation Methods 0.000 claims description 20
- XEEYBQQBJWHFJM-UHFFFAOYSA-N Iron Chemical compound [Fe] XEEYBQQBJWHFJM-UHFFFAOYSA-N 0.000 claims description 8
- BVTBRVFYZUCAKH-UHFFFAOYSA-L disodium selenite Chemical compound [Na+].[Na+].[O-][Se]([O-])=O BVTBRVFYZUCAKH-UHFFFAOYSA-L 0.000 claims description 8
- 238000002360 preparation method Methods 0.000 claims description 8
- 239000011781 sodium selenite Substances 0.000 claims description 8
- 235000015921 sodium selenite Nutrition 0.000 claims description 8
- 229960001471 sodium selenite Drugs 0.000 claims description 8
- JIAARYAFYJHUJI-UHFFFAOYSA-L zinc dichloride Chemical compound [Cl-].[Cl-].[Zn+2] JIAARYAFYJHUJI-UHFFFAOYSA-L 0.000 claims description 8
- YZOUYRAONFXZSI-SBHWVFSVSA-N (1S,3R,5R,6R,8R,10R,11R,13R,15R,16R,18R,20R,21R,23R,25R,26R,28R,30R,31S,33R,35R,36R,37S,38R,39S,40R,41S,42R,43S,44R,45S,46R,47S,48R,49S)-5,10,15,20,25,30,35-heptakis(hydroxymethyl)-37,39,40,41,42,43,44,45,46,47,48,49-dodecamethoxy-2,4,7,9,12,14,17,19,22,24,27,29,32,34-tetradecaoxaoctacyclo[31.2.2.23,6.28,11.213,16.218,21.223,26.228,31]nonatetracontane-36,38-diol Chemical compound O([C@@H]([C@H]([C@@H]1OC)OC)O[C@H]2[C@@H](O)[C@@H]([C@@H](O[C@@H]3[C@@H](CO)O[C@@H]([C@H]([C@@H]3O)OC)O[C@@H]3[C@@H](CO)O[C@@H]([C@H]([C@@H]3OC)OC)O[C@@H]3[C@@H](CO)O[C@@H]([C@H]([C@@H]3OC)OC)O[C@@H]3[C@@H](CO)O[C@@H]([C@H]([C@@H]3OC)OC)O3)O[C@@H]2CO)OC)[C@H](CO)[C@H]1O[C@@H]1[C@@H](OC)[C@H](OC)[C@H]3[C@@H](CO)O1 YZOUYRAONFXZSI-SBHWVFSVSA-N 0.000 claims description 6
- FVAUCKIRQBBSSJ-UHFFFAOYSA-M sodium iodide Chemical compound [Na+].[I-] FVAUCKIRQBBSSJ-UHFFFAOYSA-M 0.000 claims description 6
- ODLHGICHYURWBS-LKONHMLTSA-N trappsol cyclo Chemical compound CC(O)COC[C@H]([C@H]([C@@H]([C@H]1O)O)O[C@H]2O[C@@H]([C@@H](O[C@H]3O[C@H](COCC(C)O)[C@H]([C@@H]([C@H]3O)O)O[C@H]3O[C@H](COCC(C)O)[C@H]([C@@H]([C@H]3O)O)O[C@H]3O[C@H](COCC(C)O)[C@H]([C@@H]([C@H]3O)O)O[C@H]3O[C@H](COCC(C)O)[C@H]([C@@H]([C@H]3O)O)O3)[C@H](O)[C@H]2O)COCC(O)C)O[C@@H]1O[C@H]1[C@H](O)[C@@H](O)[C@@H]3O[C@@H]1COCC(C)O ODLHGICHYURWBS-LKONHMLTSA-N 0.000 claims description 6
- RYGMFSIKBFXOCR-UHFFFAOYSA-N Copper Chemical compound [Cu] RYGMFSIKBFXOCR-UHFFFAOYSA-N 0.000 claims description 5
- 239000010949 copper Substances 0.000 claims description 5
- 229910052802 copper Inorganic materials 0.000 claims description 5
- ORTQZVOHEJQUHG-UHFFFAOYSA-L copper(II) chloride Chemical compound Cl[Cu]Cl ORTQZVOHEJQUHG-UHFFFAOYSA-L 0.000 claims description 5
- 239000011684 sodium molybdate Substances 0.000 claims description 5
- 235000015393 sodium molybdate Nutrition 0.000 claims description 5
- TVXXNOYZHKPKGW-UHFFFAOYSA-N sodium molybdate (anhydrous) Chemical compound [Na+].[Na+].[O-][Mo]([O-])(=O)=O TVXXNOYZHKPKGW-UHFFFAOYSA-N 0.000 claims description 5
- QPLDLSVMHZLSFG-UHFFFAOYSA-N Copper oxide Chemical compound [Cu]=O QPLDLSVMHZLSFG-UHFFFAOYSA-N 0.000 claims description 4
- DHMQDGOQFOQNFH-UHFFFAOYSA-N Glycine Chemical compound NCC(O)=O DHMQDGOQFOQNFH-UHFFFAOYSA-N 0.000 claims description 4
- 229910021380 Manganese Chloride Inorganic materials 0.000 claims description 4
- GLFNIEUTAYBVOC-UHFFFAOYSA-L Manganese chloride Chemical compound Cl[Mn]Cl GLFNIEUTAYBVOC-UHFFFAOYSA-L 0.000 claims description 4
- BUGBHKTXTAQXES-UHFFFAOYSA-N Selenium Chemical compound [Se] BUGBHKTXTAQXES-UHFFFAOYSA-N 0.000 claims description 4
- HCHKCACWOHOZIP-UHFFFAOYSA-N Zinc Chemical compound [Zn] HCHKCACWOHOZIP-UHFFFAOYSA-N 0.000 claims description 4
- XLOMVQKBTHCTTD-UHFFFAOYSA-N Zinc monoxide Chemical compound [Zn]=O XLOMVQKBTHCTTD-UHFFFAOYSA-N 0.000 claims description 4
- 229940011182 cobalt acetate Drugs 0.000 claims description 4
- GVPFVAHMJGGAJG-UHFFFAOYSA-L cobalt dichloride Chemical compound [Cl-].[Cl-].[Co+2] GVPFVAHMJGGAJG-UHFFFAOYSA-L 0.000 claims description 4
- QAHREYKOYSIQPH-UHFFFAOYSA-L cobalt(II) acetate Chemical compound [Co+2].CC([O-])=O.CC([O-])=O QAHREYKOYSIQPH-UHFFFAOYSA-L 0.000 claims description 4
- ARUVKPQLZAKDPS-UHFFFAOYSA-L copper(II) sulfate Chemical compound [Cu+2].[O-][S+2]([O-])([O-])[O-] ARUVKPQLZAKDPS-UHFFFAOYSA-L 0.000 claims description 4
- 239000011640 ferrous citrate Substances 0.000 claims description 4
- 235000019850 ferrous citrate Nutrition 0.000 claims description 4
- AMWRITDGCCNYAT-UHFFFAOYSA-L hydroxy(oxo)manganese;manganese Chemical compound [Mn].O[Mn]=O.O[Mn]=O AMWRITDGCCNYAT-UHFFFAOYSA-L 0.000 claims description 4
- 229910052742 iron Inorganic materials 0.000 claims description 4
- APVZWAOKZPNDNR-UHFFFAOYSA-L iron(ii) citrate Chemical compound [Fe+2].OC(=O)CC(O)(C([O-])=O)CC([O-])=O APVZWAOKZPNDNR-UHFFFAOYSA-L 0.000 claims description 4
- 239000011565 manganese chloride Substances 0.000 claims description 4
- 235000002867 manganese chloride Nutrition 0.000 claims description 4
- 229940099607 manganese chloride Drugs 0.000 claims description 4
- 229910052711 selenium Inorganic materials 0.000 claims description 4
- 239000011669 selenium Substances 0.000 claims description 4
- 229940091258 selenium supplement Drugs 0.000 claims description 4
- 239000011701 zinc Substances 0.000 claims description 4
- 229910052725 zinc Inorganic materials 0.000 claims description 4
- 239000011592 zinc chloride Substances 0.000 claims description 4
- 235000005074 zinc chloride Nutrition 0.000 claims description 4
- VEXZGXHMUGYJMC-UHFFFAOYSA-M Chloride anion Chemical compound [Cl-] VEXZGXHMUGYJMC-UHFFFAOYSA-M 0.000 claims description 3
- ZOKXTWBITQBERF-UHFFFAOYSA-N Molybdenum Chemical compound [Mo] ZOKXTWBITQBERF-UHFFFAOYSA-N 0.000 claims description 3
- 239000010941 cobalt Substances 0.000 claims description 3
- 229910017052 cobalt Inorganic materials 0.000 claims description 3
- GUTLYIVDDKVIGB-UHFFFAOYSA-N cobalt atom Chemical compound [Co] GUTLYIVDDKVIGB-UHFFFAOYSA-N 0.000 claims description 3
- 239000011790 ferrous sulphate Substances 0.000 claims description 3
- 235000003891 ferrous sulphate Nutrition 0.000 claims description 3
- PNDPGZBMCMUPRI-UHFFFAOYSA-N iodine Chemical compound II PNDPGZBMCMUPRI-UHFFFAOYSA-N 0.000 claims description 3
- BAUYGSIQEAFULO-UHFFFAOYSA-L iron(2+) sulfate (anhydrous) Chemical compound [Fe+2].[O-]S([O-])(=O)=O BAUYGSIQEAFULO-UHFFFAOYSA-L 0.000 claims description 3
- 229910000359 iron(II) sulfate Inorganic materials 0.000 claims description 3
- 229940099596 manganese sulfate Drugs 0.000 claims description 3
- 239000011702 manganese sulphate Substances 0.000 claims description 3
- 235000007079 manganese sulphate Nutrition 0.000 claims description 3
- WPBNNNQJVZRUHP-UHFFFAOYSA-L manganese(2+);methyl n-[[2-(methoxycarbonylcarbamothioylamino)phenyl]carbamothioyl]carbamate;n-[2-(sulfidocarbothioylamino)ethyl]carbamodithioate Chemical compound [Mn+2].[S-]C(=S)NCCNC([S-])=S.COC(=O)NC(=S)NC1=CC=CC=C1NC(=S)NC(=O)OC WPBNNNQJVZRUHP-UHFFFAOYSA-L 0.000 claims description 3
- SQQMAOCOWKFBNP-UHFFFAOYSA-L manganese(II) sulfate Chemical compound [Mn+2].[O-]S([O-])(=O)=O SQQMAOCOWKFBNP-UHFFFAOYSA-L 0.000 claims description 3
- NLKNQRATVPKPDG-UHFFFAOYSA-M potassium iodide Substances [K+].[I-] NLKNQRATVPKPDG-UHFFFAOYSA-M 0.000 claims description 3
- NWONKYPBYAMBJT-UHFFFAOYSA-L zinc sulfate Chemical compound [Zn+2].[O-]S([O-])(=O)=O NWONKYPBYAMBJT-UHFFFAOYSA-L 0.000 claims description 3
- 229960001763 zinc sulfate Drugs 0.000 claims description 3
- 229910000368 zinc sulfate Inorganic materials 0.000 claims description 3
- 239000004151 Calcium iodate Substances 0.000 claims description 2
- 239000004277 Ferrous carbonate Substances 0.000 claims description 2
- PMVSDNDAUGGCCE-TYYBGVCCSA-L Ferrous fumarate Chemical compound [Fe+2].[O-]C(=O)\C=C\C([O-])=O PMVSDNDAUGGCCE-TYYBGVCCSA-L 0.000 claims description 2
- DKKCQDROTDCQOR-UHFFFAOYSA-L Ferrous lactate Chemical compound [Fe+2].CC(O)C([O-])=O.CC(O)C([O-])=O DKKCQDROTDCQOR-UHFFFAOYSA-L 0.000 claims description 2
- 239000004471 Glycine Substances 0.000 claims description 2
- DQMUQFUTDWISTM-UHFFFAOYSA-N O.[O-2].[Fe+2].[Fe+2].[O-2] Chemical compound O.[O-2].[Fe+2].[Fe+2].[O-2] DQMUQFUTDWISTM-UHFFFAOYSA-N 0.000 claims description 2
- FMRLDPWIRHBCCC-UHFFFAOYSA-L Zinc carbonate Chemical compound [Zn+2].[O-]C([O-])=O FMRLDPWIRHBCCC-UHFFFAOYSA-L 0.000 claims description 2
- CANRESZKMUPMAE-UHFFFAOYSA-L Zinc lactate Chemical compound [Zn+2].CC(O)C([O-])=O.CC(O)C([O-])=O CANRESZKMUPMAE-UHFFFAOYSA-L 0.000 claims description 2
- 229950003143 basic zinc acetate Drugs 0.000 claims description 2
- UHWJJLGTKIWIJO-UHFFFAOYSA-L calcium iodate Chemical compound [Ca+2].[O-]I(=O)=O.[O-]I(=O)=O UHWJJLGTKIWIJO-UHFFFAOYSA-L 0.000 claims description 2
- 235000019390 calcium iodate Nutrition 0.000 claims description 2
- 229910021446 cobalt carbonate Inorganic materials 0.000 claims description 2
- KTVIXTQDYHMGHF-UHFFFAOYSA-L cobalt(2+) sulfate Chemical compound [Co+2].[O-]S([O-])(=O)=O KTVIXTQDYHMGHF-UHFFFAOYSA-L 0.000 claims description 2
- ZOTKGJBKKKVBJZ-UHFFFAOYSA-L cobalt(2+);carbonate Chemical compound [Co+2].[O-]C([O-])=O ZOTKGJBKKKVBJZ-UHFFFAOYSA-L 0.000 claims description 2
- 229940079721 copper chloride Drugs 0.000 claims description 2
- 229960004643 cupric oxide Drugs 0.000 claims description 2
- 235000019268 ferrous carbonate Nutrition 0.000 claims description 2
- RAQDACVRFCEPDA-UHFFFAOYSA-L ferrous carbonate Chemical compound [Fe+2].[O-]C([O-])=O RAQDACVRFCEPDA-UHFFFAOYSA-L 0.000 claims description 2
- 229960004652 ferrous carbonate Drugs 0.000 claims description 2
- 239000011773 ferrous fumarate Substances 0.000 claims description 2
- 235000002332 ferrous fumarate Nutrition 0.000 claims description 2
- 229960000225 ferrous fumarate Drugs 0.000 claims description 2
- 239000004225 ferrous lactate Substances 0.000 claims description 2
- 235000013925 ferrous lactate Nutrition 0.000 claims description 2
- 229940037907 ferrous lactate Drugs 0.000 claims description 2
- 229960001781 ferrous sulfate Drugs 0.000 claims description 2
- CPSYWNLKRDURMG-UHFFFAOYSA-L hydron;manganese(2+);phosphate Chemical compound [Mn+2].OP([O-])([O-])=O CPSYWNLKRDURMG-UHFFFAOYSA-L 0.000 claims description 2
- 229910000015 iron(II) carbonate Inorganic materials 0.000 claims description 2
- 239000011656 manganese carbonate Substances 0.000 claims description 2
- 235000006748 manganese carbonate Nutrition 0.000 claims description 2
- 229940093474 manganese carbonate Drugs 0.000 claims description 2
- 229910000016 manganese(II) carbonate Inorganic materials 0.000 claims description 2
- XMWCXZJXESXBBY-UHFFFAOYSA-L manganese(ii) carbonate Chemical compound [Mn+2].[O-]C([O-])=O XMWCXZJXESXBBY-UHFFFAOYSA-L 0.000 claims description 2
- 239000001230 potassium iodate Substances 0.000 claims description 2
- 235000006666 potassium iodate Nutrition 0.000 claims description 2
- JLKDVMWYMMLWTI-UHFFFAOYSA-M potassium iodate Chemical compound [K+].[O-]I(=O)=O JLKDVMWYMMLWTI-UHFFFAOYSA-M 0.000 claims description 2
- 229940093930 potassium iodate Drugs 0.000 claims description 2
- 235000009518 sodium iodide Nutrition 0.000 claims description 2
- JCPDISNOORFYFA-UHFFFAOYSA-H tetrazinc;oxygen(2-);hexaacetate Chemical compound [O-2].[Zn+2].[Zn+2].[Zn+2].[Zn+2].CC([O-])=O.CC([O-])=O.CC([O-])=O.CC([O-])=O.CC([O-])=O.CC([O-])=O JCPDISNOORFYFA-UHFFFAOYSA-H 0.000 claims description 2
- 239000011667 zinc carbonate Substances 0.000 claims description 2
- 235000004416 zinc carbonate Nutrition 0.000 claims description 2
- 229910000010 zinc carbonate Inorganic materials 0.000 claims description 2
- 229940043825 zinc carbonate Drugs 0.000 claims description 2
- 229960001939 zinc chloride Drugs 0.000 claims description 2
- 239000011576 zinc lactate Substances 0.000 claims description 2
- 235000000193 zinc lactate Nutrition 0.000 claims description 2
- 229940050168 zinc lactate Drugs 0.000 claims description 2
- 239000011787 zinc oxide Substances 0.000 claims description 2
- 229960001296 zinc oxide Drugs 0.000 claims description 2
- 235000014692 zinc oxide Nutrition 0.000 claims description 2
- XDWXRAYGALQIFG-UHFFFAOYSA-L zinc;propanoate Chemical compound [Zn+2].CCC([O-])=O.CCC([O-])=O XDWXRAYGALQIFG-UHFFFAOYSA-L 0.000 claims description 2
- 238000000227 grinding Methods 0.000 abstract description 19
- 238000001816 cooling Methods 0.000 abstract description 6
- 239000008187 granular material Substances 0.000 abstract description 6
- 238000002156 mixing Methods 0.000 abstract description 5
- 235000011175 beta-cyclodextrine Nutrition 0.000 abstract description 3
- 238000003825 pressing Methods 0.000 abstract 1
- 238000012216 screening Methods 0.000 abstract 1
- 238000004519 manufacturing process Methods 0.000 description 15
- 229950005162 benexate Drugs 0.000 description 11
- 230000008569 process Effects 0.000 description 8
- 238000007599 discharging Methods 0.000 description 7
- 238000005516 engineering process Methods 0.000 description 7
- 238000012545 processing Methods 0.000 description 7
- 230000000694 effects Effects 0.000 description 6
- HFHDHCJBZVLPGP-UHFFFAOYSA-N schardinger α-dextrin Chemical compound O1C(C(C2O)O)C(CO)OC2OC(C(C2O)O)C(CO)OC2OC(C(C2O)O)C(CO)OC2OC(C(O)C2O)C(CO)OC2OC(C(C2O)O)C(CO)OC2OC2C(O)C(O)C1OC2CO HFHDHCJBZVLPGP-UHFFFAOYSA-N 0.000 description 5
- 239000000203 mixture Substances 0.000 description 4
- 230000009471 action Effects 0.000 description 3
- 238000004108 freeze drying Methods 0.000 description 3
- 238000005498 polishing Methods 0.000 description 3
- 239000011782 vitamin Substances 0.000 description 3
- GVJHHUAWPYXKBD-UHFFFAOYSA-N (±)-α-Tocopherol Chemical compound OC1=C(C)C(C)=C2OC(CCCC(C)CCCC(C)CCCC(C)C)(C)CCC2=C1C GVJHHUAWPYXKBD-UHFFFAOYSA-N 0.000 description 2
- UNMYWSMUMWPJLR-UHFFFAOYSA-L Calcium iodide Chemical compound [Ca+2].[I-].[I-] UNMYWSMUMWPJLR-UHFFFAOYSA-L 0.000 description 2
- DGAQECJNVWCQMB-PUAWFVPOSA-M Ilexoside XXIX Chemical compound C[C@@H]1CC[C@@]2(CC[C@@]3(C(=CC[C@H]4[C@]3(CC[C@@H]5[C@@]4(CC[C@@H](C5(C)C)OS(=O)(=O)[O-])C)C)[C@@H]2[C@]1(C)O)C)C(=O)O[C@H]6[C@@H]([C@H]([C@@H]([C@H](O6)CO)O)O)O.[Na+] DGAQECJNVWCQMB-PUAWFVPOSA-M 0.000 description 2
- PWHULOQIROXLJO-UHFFFAOYSA-N Manganese Chemical compound [Mn] PWHULOQIROXLJO-UHFFFAOYSA-N 0.000 description 2
- ZOIORXHNWRGPMV-UHFFFAOYSA-N acetic acid;zinc Chemical compound [Zn].CC(O)=O.CC(O)=O ZOIORXHNWRGPMV-UHFFFAOYSA-N 0.000 description 2
- 230000009286 beneficial effect Effects 0.000 description 2
- 229940046413 calcium iodide Drugs 0.000 description 2
- 229910001640 calcium iodide Inorganic materials 0.000 description 2
- 230000008859 change Effects 0.000 description 2
- 230000006378 damage Effects 0.000 description 2
- 238000000354 decomposition reaction Methods 0.000 description 2
- 238000001727 in vivo Methods 0.000 description 2
- 229910052500 inorganic mineral Inorganic materials 0.000 description 2
- 229910052748 manganese Inorganic materials 0.000 description 2
- 239000011572 manganese Substances 0.000 description 2
- 235000010755 mineral Nutrition 0.000 description 2
- 239000011707 mineral Substances 0.000 description 2
- 235000016709 nutrition Nutrition 0.000 description 2
- 230000035764 nutrition Effects 0.000 description 2
- 238000001556 precipitation Methods 0.000 description 2
- 238000000275 quality assurance Methods 0.000 description 2
- 239000011734 sodium Substances 0.000 description 2
- 229910052708 sodium Inorganic materials 0.000 description 2
- 239000000243 solution Substances 0.000 description 2
- 238000001694 spray drying Methods 0.000 description 2
- 238000012360 testing method Methods 0.000 description 2
- 235000013343 vitamin Nutrition 0.000 description 2
- 229930003231 vitamin Natural products 0.000 description 2
- 229940088594 vitamin Drugs 0.000 description 2
- 150000003722 vitamin derivatives Chemical class 0.000 description 2
- 239000004246 zinc acetate Substances 0.000 description 2
- FPIPGXGPPPQFEQ-UHFFFAOYSA-N 13-cis retinol Natural products OCC=C(C)C=CC=C(C)C=CC1=C(C)CCCC1(C)C FPIPGXGPPPQFEQ-UHFFFAOYSA-N 0.000 description 1
- WIGIZIANZCJQQY-UHFFFAOYSA-N 4-ethyl-3-methyl-N-[2-[4-[[[(4-methylcyclohexyl)amino]-oxomethyl]sulfamoyl]phenyl]ethyl]-5-oxo-2H-pyrrole-1-carboxamide Chemical compound O=C1C(CC)=C(C)CN1C(=O)NCCC1=CC=C(S(=O)(=O)NC(=O)NC2CCC(C)CC2)C=C1 WIGIZIANZCJQQY-UHFFFAOYSA-N 0.000 description 1
- OYPRJOBELJOOCE-UHFFFAOYSA-N Calcium Chemical compound [Ca] OYPRJOBELJOOCE-UHFFFAOYSA-N 0.000 description 1
- ZAMOUSCENKQFHK-UHFFFAOYSA-N Chlorine atom Chemical compound [Cl] ZAMOUSCENKQFHK-UHFFFAOYSA-N 0.000 description 1
- 208000027219 Deficiency disease Diseases 0.000 description 1
- CWYNVVGOOAEACU-UHFFFAOYSA-N Fe2+ Chemical compound [Fe+2] CWYNVVGOOAEACU-UHFFFAOYSA-N 0.000 description 1
- PXGOKWXKJXAPGV-UHFFFAOYSA-N Fluorine Chemical compound FF PXGOKWXKJXAPGV-UHFFFAOYSA-N 0.000 description 1
- FYYHWMGAXLPEAU-UHFFFAOYSA-N Magnesium Chemical compound [Mg] FYYHWMGAXLPEAU-UHFFFAOYSA-N 0.000 description 1
- OAICVXFJPJFONN-UHFFFAOYSA-N Phosphorus Chemical compound [P] OAICVXFJPJFONN-UHFFFAOYSA-N 0.000 description 1
- ZLMJMSJWJFRBEC-UHFFFAOYSA-N Potassium Chemical compound [K] ZLMJMSJWJFRBEC-UHFFFAOYSA-N 0.000 description 1
- NINIDFKCEFEMDL-UHFFFAOYSA-N Sulfur Chemical compound [S] NINIDFKCEFEMDL-UHFFFAOYSA-N 0.000 description 1
- 239000005864 Sulphur Substances 0.000 description 1
- FPIPGXGPPPQFEQ-BOOMUCAASA-N Vitamin A Natural products OC/C=C(/C)\C=C\C=C(\C)/C=C/C1=C(C)CCCC1(C)C FPIPGXGPPPQFEQ-BOOMUCAASA-N 0.000 description 1
- 229930003427 Vitamin E Natural products 0.000 description 1
- 239000002253 acid Substances 0.000 description 1
- 239000000654 additive Substances 0.000 description 1
- 230000000996 additive effect Effects 0.000 description 1
- FPIPGXGPPPQFEQ-OVSJKPMPSA-N all-trans-retinol Chemical compound OC\C=C(/C)\C=C\C=C(/C)\C=C\C1=C(C)CCCC1(C)C FPIPGXGPPPQFEQ-OVSJKPMPSA-N 0.000 description 1
- 239000003674 animal food additive Substances 0.000 description 1
- 230000003064 anti-oxidating effect Effects 0.000 description 1
- 238000009360 aquaculture Methods 0.000 description 1
- 244000144974 aquaculture Species 0.000 description 1
- QVGXLLKOCUKJST-UHFFFAOYSA-N atomic oxygen Chemical compound [O] QVGXLLKOCUKJST-UHFFFAOYSA-N 0.000 description 1
- 230000008901 benefit Effects 0.000 description 1
- 230000015572 biosynthetic process Effects 0.000 description 1
- 238000009395 breeding Methods 0.000 description 1
- 230000001488 breeding effect Effects 0.000 description 1
- 239000011575 calcium Substances 0.000 description 1
- 229910052791 calcium Inorganic materials 0.000 description 1
- 150000001768 cations Chemical class 0.000 description 1
- IAXUQWSLRKIRFR-SAABIXHNSA-N chembl2104696 Chemical compound C1C[C@@H](CNC(=N)N)CC[C@@H]1C(=O)OC1=CC=CC=C1C(=O)OCC1=CC=CC=C1 IAXUQWSLRKIRFR-SAABIXHNSA-N 0.000 description 1
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Landscapes
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Abstract
The invention discloses a method for preparing microelement-beta-cyclodextrin or a derivative inclusion compound thereof. The microelement-beta-cyclodextrin or the derivative inclusion compound consists of microelements, beta-cyclodextrin or a derivative of beta-cyclodextrin and PVP which are in the weight ratio of 1:(18-98):(0.5-1.0). The method comprises the following steps: (1) mixing the microelements and PVP according to the ratio, grinding in a ball mill, and screening by using a sieve of 150-300 meshes, thereby preparing fine microelement powder; (2) mixing the fine microelement powder with beta-cyclodextrin or the derivative of beta-cyclodextrin by using an equivalent amount progressiveincrease method, putting into a double-shaft paddle high-efficiency mixing machine, and uniformly stirring for 5-8 minutes; (3) directly pressing the uniformly mixed material by using a dry granulator to obtain granules of 10-15 meshes; (4) putting the prepared granules of 10-15 meshes into a counter-current cooler, and performing cooling drying for 10-15 minutes until the water content is less than 10% under the conditions that the vibration frequency is 25-33 times/minute, the vibration amplitude is 30mm, the air sucking amount is 13500-18000m<3>/hour, and the air pressure is greater than or equal to 200mmHg; (5) crushing the granules after cooling drying by using a crushing machine until the granularity of the granules is 75-85 meshes, thereby obtaining the product.
Description
Technical field
The present invention relates to field of feed processing, also relate to field of feed additive technology, be specifically related to the preparation method of a kind of trace element-beta-schardinger dextrin-or derivatives thereof inclusion compound.
Background technology
Though mineral matter element in animal body content is little, play an important role, detect that more than 40 plant inorganic elements (also known as mineral element) in animal body, there will be a known now more than ten and planted trophism.Sodium, potassium, calcium, magnesium, phosphorus, chlorine, sulphur are macroelement, and iron, copper, zinc, manganese, cobalt, selenium, iodine, fluorine and molybdenum etc. are trace element.Their valence state, lewis' acid form are in close relations with the biochemical action played, and trace element can not synthesize in vivo, can only by drinking water and feed supply.Different elements morphosis is in vivo different, ion, molecule or baroque complex compound state, different shape the biochemical action that rises also different, they are to the health of maintenance animal, optimum growth and breeding, the production of livestock products all plays an important role.Various element can produce deficiency disease very little, but too much also can poisoning or generation imbalance.These all can make the animal husbandry underproduction, can make animal dead time serious.Intensive farm and artificial formula feed, make the mass exchange relation of animal and the natural ecological balance change.Thus according to the growth needs of animal, in feed, add mineral trace element is very necessary.In feed manufacturing industry, add the trace element applied as additive use is also the indispensable important nutriment of feed formulation.For strengthening the management of feed addictive, ensureing cultured product quality safety, promoting feed industry sustainable and healthy development, the Ministry of Agriculture of China discloses " feed addictive kind catalogue (2013) " (Ministry of Agriculture announces No. 2045) defines the kind permitting using.
Because the consumption of trace element is little, safe range is narrow, and some trace elements such as selenium is extremely toxic substance.The stability of trace element and be always the difficult problem troubling feed manufacturing emterprise to the destructiveness of other nutrition, as the cations such as the iron in trace element, copper, manganese directly can cause the rapid decomposition inactivation of vitamin particularly vitamin A, vitamine D3 and vitamin E.The destruction of trace element is more accelerated in the existence of free moisture.Due to the impact of micro-light, oxygen, heat and moisture content, make finished product quality instability or therefore cause product defective and affect effect, bringing economic loss to manufacturing and processing enterprise and aquaculture.As in standard GB/T/T 18823-2002 " allowable error that feed testing result judges " table 3 feed, vitamin and micronutrient levels testing result judge in allowable error, to the scope of its allowable error (relative error)/(%) all more than-10%, what have reaches-45%.Therefrom can find out the unstability of the Trace Elements content in feed.
Cyclodextrin inclusion compound technology is serving good effect to the application of trace element, its inclusion technique is also progressively applied in feed, feed addictive, because inclusion technique can change the physicochemical property of trace element, increase stability in the application, improve its solubility, reduce excitant, improve and badly smell taste, reduce toxic and side effect, trace element particularly after cyclodextrin encapsulated process, very effectively can reduce or avoid the destruction to other nutrition, thus improve the stability of product.The application of trace element cyclodextrin inclusion compound all can play good beneficial effect to the validity of product and stability undoubtedly.With regard to the preparation method of its inclusion compound, mostly adopt inclusion aqua-solution method (i.e. recrystallization or coprecipitation), supercritical ultrasonics technology at present, polishing, spray drying process and freeze-drying etc.Because saturated water solution method is through refrigeration after the stirring or vibration of uniform temperature and certain hour, filter, dry obtained cyclodextrin inclusion compound, because the operating time is long, large during energy charge, although select supercritical ultrasonics technology to utilize the intensity of sonicator or supersonic wave cleaning machine, the alternative mixing power of ultrasonic appropriate time, but ultrasonic equipment increases the equipment investment of medium-sized and small enterprises, simultaneously to its precipitation, filter and the link of drying also essential, still for enterprise is difficult to acceptance.Although polishing technique is simple, be easy to operation, because output is less, be difficult to form scale production technology.Freeze-drying is to cyclodextrin inclusion compound soluble in water not easily crystallization precipitation, or easily decompose when heat drying, variable color, the method can be adopted, due to apparatus expensive, manufacturing cost is large, only apply preparing in powder-injection product and some biological products at present, be not suitable for feed processing industry application.Spraying dry is suitable for heat stable in properties, and the product using spray seasoning obtaining inclusion compound soluble in water prepares inclusion compound, and because in process, baking temperature is higher, heated time is short, productive rate is high, applies comparatively extensive in pharmacy, food service industry.Because most micro-series products all has temperature instability, so be also difficult to be used widely in feed processing industry.
Summary of the invention
The present invention adopts the conventional equipment of existing feed manufacturing, adopt beta-schardinger dextrin-or derivatives thereof to carry out inclusion to micro-series products, overcome that the method production cycles such as existing full Heshui solwution method, supercritical ultrasonics technology, polishing, freeze-drying, spray drying process are long, consume energy high, many unfavorable factors such as equipment investment is large, production cost is high, product is unstable.Make feed manufacturing emterprise under the condition not increasing equipment, can Produce on a large scale be realized, saved production cost, expanded Business Economic Benefit, realize self-produced personal, solve the problem for quality assurance of trace element materials safe handling.
The object of this invention is to provide the preparation method of a kind of trace element-beta-schardinger dextrin-or derivatives thereof inclusion compound.The method can overcome the deficiency of existing preparation method preferably, overcome production equipment input cost large, production is taken a lot of work, time-consuming, the unfavorable factors such as quality cannot ensure, solve convenient processing and the application of microelement kind inclusion compound preferably, for the application of trace element materials in feed manufacturing provides quality assurance.The mass effect of feed product is provided further.
The invention provides the preparation method of a kind of trace element-beta-schardinger dextrin-or derivatives thereof inclusion compound.
To achieve these goals, present invention employs following technical scheme:
The preparation method of a kind of trace element-beta-schardinger dextrin-or derivatives thereof inclusion compound, it is characterized in that by the trace element of weight ratio: beta-schardinger dextrin-or derivatives thereof: polyvinylpyrrolidone (PVP) forms for 1:18-98:0.5-1.0 ratio, is made by following technique:
(1) trace element taking formula ratio mixes with PVP, grinds with ball mill, crosses 150-300 sieve, obtained micro-fine powder;
(2) the beta-schardinger dextrin-or derivatives thereof of micro-fine powder and formula ratio is mixed by equivalent method of progressively increasing, insert in twin shaft paddle high efficient mixer, stir 5-8min, make it to stir;
(3) the material dry granulation machine stirred is directly compressed into 10-15 order particle;
(4) by obtained 10-15 order particle, inserting counterflow cooler, is 25-33 time/min in vibration frequency, amplitude 30mm, suction air volume 13500-18000m
3/ h, under blast>=200mmHg condition, cool drying 10-15min, makes water content be less than 10%;
(5) particle after cool drying, by crusher in crushing, makes grain graininess be 75-85 order, obtains micro--beta-schardinger dextrin-or derivatives thereof inclusion compound.
Trace element described above is containing iron, zinc, manganese, copper, cobalt, iodine, the compound of selenium and molybdenum element, as ferrous citrate, ferrous fumarate, ferrous sulfate, ferrous lactate, ferrous carbonate, frerrous chloride, di-iron trioxide, copper chloride, copper sulphate, basic copper chloride, cupric oxide, zinc oxide, zinc chloride, zinc carbonate, zinc sulfate, zinc acetate, basic zinc chloride, zinc propionate, zinc lactate, glycine zine, manganese chloride, manganese sulfate, manganese carbonate, manganese hydrogen phosphate, manganese oxide, KI, sodium iodide, Potassiumiodate, calcium iodate, cobalt chloride, cobalt acetate, cobaltous sulfate, cobalt carbonate, sodium selenite, any one in sodium molybdate.
Beta-schardinger dextrin-(β-Cyclodextrin described above, be called for short β-CD) derivative is any one in methyl-B-cyclodextrin, DM-β-CD, TM-β-CD, 2-second group-beta-cyclodextrin, 2-hydroxyethyl-β-cyclodextrin, 3-hydroxyethyl-β-cyclodextrin, HP-β-CD.
Polyvinylpyrrolidone (PVP) described above is polyvinylpyrrolidone (PVP)
k25or polyvinylpyrrolidone
k30.
The equipment that the present invention adopts, is the conventional equipment in mixed feed processing.Twin shaft paddle high efficient mixer is the SSHJI high efficient mixer that Zhengchang Foodstuff Machinery Co., Ltd., Jiangsu produces, and this machine is equipped with sealing device, and discharging controls.The operation principle of this machine is made up of the rotor that two direction of rotation are contrary, and rotor is welded with the paddle of multiple special angle, paddle drives material to be rotated counterclockwise along trough inwall on the one hand.Stir about driving material on the one hand; weightless district is formed at the juxtaposition place of two rotors; in this region; no matter how the shape of material, size and density can make material float and be in instantaneous weight loss state; this makes material in trough, form comprehensive continuous circulation to stir; mutually extensively be staggered to form fluidized bed mixing; simultaneously; material is also promoted by paddle; extend axially through and trace element can be protected to prevent light or thermoinducible decomposition to inclusion; anti-oxidation or and other Organic Ingredients compositions between react, increase solubility, improve dissolution rate.Radial motion, thus form comprehensive combined-circulation, reaches soft, the inclusion effect that mixes fast.
SKLN1-5 counterflow cooler, its principle and the course of work are then that pile up gradually, until reach a certain height, when material contacts upper level detector, the motor of marker gear is started working by the granule materials of heat after rotating feeder and entering intermediate bin.Motor drives discharge fence to move back and forth by decelerator and eccentric stiffener, carries out discharging, the action of discharge grid.This time relay is started working, and by arranging certain time delay discharge time, carries out automatic discharging.The discharging quantity cooling material in storehouse during discharging is greater than inlet amount, in storehouse, material drops to certain controlling level, if the time delay discharge time of the time relay terminates, spacing indicator board now on discharge fence reaccees the horizontal level detector be arranged on base time, motor just stops immediately, and discharge fence just rests on fixing position.
When bed depth reaches upper level detector again, discharge fence is setting in motion, discharging again.Constantly repeat the discharge process continued above.In above-mentioned whole process, cooling blower is open all the time.
Along with the reciprocating motion discharging of discharge fence, material is progressively slowly descending, and cooling air from bottom to top, by cold heating, like this, in the course of the work, what the material of top heat ran into is hot blast, and what what bottom was cold ran into is cold wind, material in descending process through all even sufficient cooling, become hard and solid, further reduce moisture, make particle reach further drying purpose.
Beneficial effect of the present invention
The present invention adopts SSHJl high efficient mixer, utilize the state of weightlessness formed in body, the comprehensive continuous circulation of formation that material can be floated stirs, interlaced shearing, can effectively reach quick suspension, impact dynamics, mixture homogeneity coefficient is high, its mixture homogeneity coefficient reaches≤2.0%(CV%≤2.0), granulate through compacting again, cool drying, broken sub-sieve, the inclusion rate of its inclusion compound reaches more than 95%, make the clathrate process saving of labor of microelement medicine, save time, reduce power consumption, reduce equipment cost, stability is improve to the application of trace element in feed, improve the effect of trace element in feed valuably.The inventive method adopts the conventional equipment of mixed feed processing, effectively can solve the useful use of trace element under the condition not increasing equipment, solves the vantageous methods of application trace element to feed manufacturing emterprise.
Detailed description of the invention
Embodiment 1
(1) ferrous sulfate 1kg and PVP is taken
k301kg mixes, and inserts grinding in ball mill, sieves, make 150 order powder; (2) progressively increase after method carries out premixed by 150 obtained order powder and beta-schardinger dextrin-18kg by equivalent, be placed in twin shaft paddle high efficient mixer, stirring 5min, makes it to stir; (3) dry granulation machine is adopted to be directly compressed into 15 order particles the material stirred; (4) 15 obtained order particles are inserted counterflow cooler, be 33 times in vibration frequency, amplitude 30mm, suction air volume is 13500m
3/ h, under blast>=200mmHg condition, cool drying 15min, makes water content be less than 10%; (5) particle after cool drying, by crusher in crushing, makes grain graininess be 75 orders, obtains ferrous sulfate-Benexate Hydrochloride product.
Embodiment 2
(1) ferrous citrate 1kg and PVP is taken
k251kg mixes, and inserts grinding in ball mill, sieves, make 150 order powder; (2) progressively increase after method carries out premixed by 150 obtained order powder and 2-second group-beta-cyclodextrin 23kg by equivalent, be placed in twin shaft paddle high efficient mixer, stirring 5min, makes it to stir; (3) dry granulation machine is adopted to be directly compressed into 15 order particles the material stirred; (4) 15 obtained order particles are inserted counterflow cooler, be 33 times in vibration frequency, amplitude 30mm, suction air volume is 13500m
3/ h, under blast>=200mmHg condition, cool drying 15min, makes water content be less than 10%; (5) particle after cool drying, by crusher in crushing, makes grain graininess be 75 orders, obtains ferrous citrate 2-ethyl-Benexate Hydrochloride product.
Embodiment 3
(1) frerrous chloride 1kg and PVP is taken
k300.5kg mixes, and inserts grinding in ball mill, sieves, make 200 order powder; (2) progressively increase after method carries out premixed by 200 obtained order powder and beta-schardinger dextrin-23.5kg by equivalent, be placed in twin shaft paddle high efficient mixer, stirring 6min, makes it to stir; (3) dry granulation machine is adopted to be directly compressed into 14 order particles the material stirred; (4) 14 obtained order particles are inserted counterflow cooler, be 33 times in vibration frequency, amplitude 30mm, suction air volume is 13500m
3/ h, under blast>=200mmHg condition, cool drying 10min, makes water content be less than 10%; (5) particle after cool drying, by crusher in crushing, makes grain graininess be 80 orders, obtains frerrous chloride-Benexate Hydrochloride product.
Embodiment 4
(1) copper sulphate 1kg and PVP is taken
k301kg mixes, and inserts grinding in ball mill, sieves, make 200 order powder; (2) progressively increase after method carries out premixed by 200 obtained order powder and methyl-B-cyclodextrin 48kg by equivalent, be placed in twin shaft paddle high efficient mixer, stirring 8min, makes it to stir; (3) dry granulation machine is adopted to be directly compressed into 10 order particles the material stirred; (4) 10 obtained order particles are inserted counterflow cooler, be 33 times in vibration frequency, amplitude 30mm, suction air volume is 13500m
3/ h, under blast>=200mmHg condition, cool drying 15min, makes water content be less than 10%; (5) particle after cool drying, by crusher in crushing, makes grain graininess be 80 orders, obtains copper sulphate methyl-B-cyclodextrin inclusion compound product.
Embodiment 5
(1) copper chloride 1kg and PVP is taken
k250.5kg mixes, and inserts grinding in ball mill, sieves, make 200 order powder; (2) progressively increase after method carries out premixed by 200 obtained order powder and beta-schardinger dextrin-38.5kg by equivalent, be placed in twin shaft paddle high efficient mixer, stirring 6min, makes it to stir; (3) dry granulation machine is adopted to be directly compressed into 12 order particles the material stirred; (4) 12 obtained order particles are inserted counterflow cooler, be 25 times in vibration frequency, amplitude 30mm, suction air volume is 18000m
3/ h, under blast>=200mmHg condition, cool drying 12min, makes water content be less than 10%; (5) particle after cool drying, by crusher in crushing, makes grain graininess be 80 orders, obtains copper chloride-Benexate Hydrochloride product.
Embodiment 6
(1) zinc sulfate 1kg and PVP is taken
k301kg mixes, and inserts grinding in ball mill, sieves, make 200 order powder; (2) progressively increase after method carries out premixed by 200 obtained order powder and beta-schardinger dextrin-38kg by equivalent, be placed in twin shaft paddle high efficient mixer, stirring 7min, makes it to stir; (3) dry granulation machine is adopted to be directly compressed into 15 order particles the material stirred; (4) 15 obtained order particles are inserted counterflow cooler, be 25 times in vibration frequency, amplitude 30mm, suction air volume is 18000m
3/ h, under blast>=200mmHg condition, cool drying 15min, makes water content be less than 10%; (5) particle after cool drying, by crusher in crushing, makes grain graininess be 75 orders, obtains zinc sulfate-Benexate Hydrochloride product.
Embodiment 7
(1) zinc acetate 1kg and PVP is taken
k250.5kg mixes, and inserts grinding in ball mill, sieves, make 200 order powder; (2) progressively increase after method carries out premixed by 200 obtained order powder and HP-β-CD 48.5kg by equivalent, be placed in twin shaft paddle high efficient mixer, stirring 8min, makes it to stir; (3) dry granulation machine is adopted to be directly compressed into 10 order particles the material stirred; (4) 10 obtained order particles are inserted counterflow cooler, be 33 times in vibration frequency, amplitude 30mm, suction air volume is 13500m
3/ h, under blast>=200mmHg condition, cool drying 10min, makes water content be less than 10%; (5) particle after cool drying, by crusher in crushing, makes grain graininess be 80 orders, obtains zinc acetate hydroxypropyl-beta-cyclodextrin inclusion product.
Embodiment 8
(1) manganese sulfate 1kg and PVP is taken
k251kg mixes, and inserts grinding in ball mill, sieves, make 180 order powder; (2) progressively increase after method carries out premixed by 180 obtained order powder and beta-schardinger dextrin-38kg by equivalent, be placed in twin shaft paddle high efficient mixer, stirring 6min, makes it to stir; (3) dry granulation machine is adopted to be directly compressed into 15 order particles the material stirred; (4) 15 obtained order particles are inserted counterflow cooler, be 33 times in vibration frequency, amplitude 30mm, suction air volume is 13500m
3/ h, under blast>=200mmHg condition, cool drying 12min, makes water content be less than 10%; (5) particle after cool drying, by crusher in crushing, makes grain graininess be 75 orders, obtains manganese sulfate-Benexate Hydrochloride product.
Embodiment 9
(1) manganese chloride 1kg and PVP is taken
k300.5kg mixes, and inserts grinding in ball mill, sieves, make 200 order powder; (2) progressively increase after method carries out premixed by 200 obtained order powder and TM-β-CD 23.5kg by equivalent, be placed in twin shaft paddle high efficient mixer, stirring 6min, makes it to stir; (3) dry granulation machine is adopted to be directly compressed into 15 order particles the material stirred; (4) 15 obtained order particles are inserted counterflow cooler, be 33 times in vibration frequency, amplitude 30mm, suction air volume is 13500m
3/ h, under blast>=200mmHg condition, cool drying 13min, makes water content be less than 10%; (5) particle after cool drying, by crusher in crushing, makes grain graininess be 80 orders, obtains manganese chloride TM-β-CD inclusion compound product.
Embodiment 10
(1) KI 1kg and PVP is taken
k251kg mixes, and inserts grinding in ball mill, sieves, make 250 order powder; (2) progressively increase after method carries out premixed by 250 obtained order powder and beta-schardinger dextrin-78kg by equivalent, be placed in twin shaft paddle high efficient mixer, stirring 8min, makes it to stir; (3) dry granulation machine is adopted to be directly compressed into 10 order particles the material stirred; (4) 10 obtained order particles are inserted counterflow cooler, be 33 times in vibration frequency, amplitude 30mm, suction air volume is 13500m
3/ h, under blast>=200mmHg condition, cool drying 11min, makes water content be less than 10%; (5) particle after cool drying, by crusher in crushing, makes grain graininess be 85 orders, obtains KI-Benexate Hydrochloride product.
Embodiment 11
(1) calcium iodide 1kg and PVP is taken
k301kg mixes, and inserts grinding in ball mill, sieves, make 250 order powder; (2) progressively increase after method carries out premixed by 250 obtained order powder and 2-hydroxyethyl-β-cyclodextrin 68kg by equivalent, be placed in twin shaft paddle high efficient mixer, stirring 8min, makes it to stir; (3) dry granulation machine is adopted to be directly compressed into 10 order particles the material stirred; (4) 10 obtained order particles are inserted counterflow cooler, be 33 times in vibration frequency, amplitude 30mm, suction air volume is 13500m
3/ h, under blast>=200mmHg condition, cool drying 12min, makes water content be less than 10%; (5) particle after cool drying, by crusher in crushing, makes grain graininess be 85 orders, obtains calcium iodide 2-hydroxyethyl-β-cyclodextrin inclusion compound product.
Embodiment 12
(1) cobalt chloride 1kg and PVP is taken
k251kg mixes, and inserts grinding in ball mill, sieves, make 250 order powder; (2) progressively increase after method carries out premixed by 250 obtained order powder and TM-β-CD 78kg by equivalent, be placed in twin shaft paddle high efficient mixer, stirring 8min, makes it to stir; (3) dry granulation machine is adopted to be directly compressed into 10 order particles the material stirred; (4) 10 obtained order particles are inserted counterflow cooler, be 25 times in vibration frequency, amplitude 30mm, suction air volume is 18000m
3/ h, under blast>=200mmHg condition, cool drying 13min, makes water content be less than 10%; (5) particle after cool drying, by crusher in crushing, makes grain graininess be 80 orders, obtains cobalt chloride TM-β-CD inclusion compound product.
Embodiment 13
(1) cobalt acetate 1kg and PVP is taken
k301kg mixes, and inserts grinding in ball mill, sieves, make 250 order powder; (2) progressively increase after method carries out premixed by 250 obtained order powder and 2-second group-beta-cyclodextrin 48kg by equivalent, be placed in twin shaft paddle high efficient mixer, stirring 8min, makes it to stir; (3) dry granulation machine is adopted to be directly compressed into 10 order particles the material stirred; (4) 10 obtained order particles are inserted counterflow cooler, be 33 times in vibration frequency, amplitude 30mm, suction air volume is 13500m
3/ h, under blast>=200mmHg condition, cool drying 13min, makes water content be less than 10%; (5) particle after cool drying, by crusher in crushing, makes grain graininess be 80 orders, obtains cobalt acetate 2-ethyl-Benexate Hydrochloride product.
Embodiment 14
(1) sodium selenite 1kg and PVP is taken
k301kg mixes, and inserts grinding in ball mill, sieves, make 300 order powder; (2) progressively increase after method carries out premixed by 300 obtained order powder and beta-schardinger dextrin-98kg by equivalent, be placed in twin shaft paddle high efficient mixer, stirring 8min, makes it to stir; (3) dry granulation machine is adopted to be directly compressed into 10 order particles the material stirred; (4) 10 obtained order particles are inserted counterflow cooler, be 25 times in vibration frequency, amplitude 30mm, suction air volume is 18000m
3/ h, under blast>=200mmHg condition, cool drying 10min, makes water content be less than 10%; (5) particle after cool drying, by crusher in crushing, makes grain graininess be 85 orders, obtains sodium selenite Benexate Hydrochloride product.
Embodiment 15
(1) sodium selenite 1kg and PVP is taken
k251kg mixes, and inserts grinding in ball mill, sieves, make 300 order powder; (2) progressively increase after method carries out premixed by 300 obtained order powder and 2-second group-beta-cyclodextrin 48kg by equivalent, be placed in twin shaft paddle high efficient mixer, stirring 8min, makes it to stir; (3) dry granulation machine is adopted to be directly compressed into 10 order particles the material stirred; (4) 10 obtained order particles are inserted counterflow cooler, be 25 times in vibration frequency, amplitude 30mm, suction air volume is 18000m
3/ h, under blast>=200mmHg condition, cool drying 12min, makes water content be less than 10%; (5) particle after cool drying, by crusher in crushing, makes grain graininess be 85 orders, obtains sodium selenite 2-ethyl-Benexate Hydrochloride product.
Embodiment 16
(1) sodium selenite 1kg and PVP is taken
k301kg mixes, and inserts grinding in ball mill, sieves, make 300 order powder; (2) progressively increase after method carries out premixed by 300 obtained order powder and HP-β-CD 88kg by equivalent, be placed in twin shaft paddle high efficient mixer, stirring 8min, makes it to stir; (3) dry granulation machine is adopted to be directly compressed into 10 order particles the material stirred; (4) 10 obtained order particles are inserted counterflow cooler, be 33 times in vibration frequency, amplitude 30mm, suction air volume is 13500m
3/ h, under blast>=200mmHg condition, cool drying 12min, makes water content be less than 10%; (5) particle after cool drying, by crusher in crushing, makes grain graininess be 85 orders, obtains sodium selenite hydroxypropyl-beta-cyclodextrin inclusion product.
Embodiment 17
(1) sodium molybdate 1kg and PVP is taken
k301kg mixes, and inserts grinding in ball mill, sieves, make 300 order powder; (2) progressively increase after method carries out premixed by 300 obtained order powder and beta-schardinger dextrin-98kg by equivalent, be placed in twin shaft paddle high efficient mixer, stirring 8min, makes it to stir; (3) dry granulation machine is adopted to be directly compressed into 10 order particles the material stirred; (4) 10 obtained order particles are inserted counterflow cooler, be 25 times in vibration frequency, amplitude 30mm, suction air volume is 18000m
3/ h, under blast>=200mmHg condition, cool drying 12min, makes water content be less than 10%; (5) particle after cool drying, by crusher in crushing, makes grain graininess be 85 orders, obtains sodium molybdate-Benexate Hydrochloride product.
Embodiment 18
(1) sodium molybdate 1kg and PVP is taken
k251kg mixes, and inserts grinding in ball mill, sieves, make 300 order powder; (2) progressively increase after method carries out premixed by 300 obtained order powder and methyl-B-cyclodextrin 88kg by equivalent, be placed in twin shaft paddle high efficient mixer, stirring 8min, makes it to stir; (3) dry granulation machine is adopted to be directly compressed into 10 order particles the material stirred; (4) 10 obtained order particles are inserted counterflow cooler, be 33 times in vibration frequency, amplitude 30mm, suction air volume is 13500m
3/ h, under blast>=200mmHg condition, cool drying 12min, makes water content be less than 10%; (5) particle after cool drying, by crusher in crushing, makes grain graininess be 85 orders, obtains sodium molybdate methyl-B-cyclodextrin inclusion compound product.
Claims (5)
1. the preparation method of trace element-beta-schardinger dextrin-or derivatives thereof inclusion compound, it is characterized in that by the trace element of weight ratio: beta-schardinger dextrin-or derivatives thereof: polyvinylpyrrolidone is that 1:18-98:0.5-1.0 ratio forms, and is made by following technique:
(1) trace element taking formula ratio mixes with polyvinylpyrrolidone, grinds with ball mill, crosses 150-300 sieve, obtained micro-fine powder;
(2) the beta-schardinger dextrin-or derivatives thereof of micro-fine powder and formula ratio is mixed by equivalent method of progressively increasing, insert in twin shaft paddle high efficient mixer, stir 5-8min, make it to stir;
(3) the material dry granulation machine stirred is directly compressed into 10-15 order particle;
(4) by obtained 10-15 order particle, inserting counterflow cooler, is 25-33 time/min in vibration frequency, amplitude 30mm, suction air volume 13500-18000m
3/ h, under blast>=200mmHg condition, cool drying 10-15min, makes water content be less than 10%;
(5) particle after cool drying, by crusher in crushing, makes grain graininess be 75-85 order, obtains micro--beta-schardinger dextrin-or derivatives thereof inclusion compound.
2. the method for claim 1, it is characterized in that, described trace element is containing iron, zinc, manganese, copper, cobalt, iodine, the compound of selenium and molybdenum element, for ferrous citrate, ferrous fumarate, ferrous sulfate, ferrous lactate, ferrous carbonate, frerrous chloride, di-iron trioxide, copper chloride, copper sulphate, basic copper chloride, cupric oxide, zinc oxide, zinc chloride, zinc carbonate, zinc sulfate, zinc acetate, basic zinc chloride, zinc propionate, zinc lactate, glycine zine, manganese chloride, manganese sulfate, manganese carbonate, manganese hydrogen phosphate, manganese oxide, KI, sodium iodide, Potassiumiodate, calcium iodate, cobalt chloride, cobalt acetate, cobaltous sulfate, cobalt carbonate, sodium selenite, any one in sodium molybdate.
3. the method for claim 1, it is characterized in that, described beta-cyclodextrin derivative is any one in methyl-B-cyclodextrin, DM-β-CD, TM-β-CD, 2-second group-beta-cyclodextrin, 2-hydroxyethyl-β-cyclodextrin, 3-hydroxyethyl-β-cyclodextrin, HP-β-CD.
4. polyvinylpyrrolidone described above is polyvinylpyrrolidone
k25or polyvinylpyrrolidone
k30.
5. trace element-beta-schardinger dextrin-or derivatives thereof inclusion compound the product of the method for claim 1 acquisition.
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