JP2016138093A - Minoxidil-containing liquid drug - Google Patents
Minoxidil-containing liquid drug Download PDFInfo
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- JP2016138093A JP2016138093A JP2016006731A JP2016006731A JP2016138093A JP 2016138093 A JP2016138093 A JP 2016138093A JP 2016006731 A JP2016006731 A JP 2016006731A JP 2016006731 A JP2016006731 A JP 2016006731A JP 2016138093 A JP2016138093 A JP 2016138093A
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- minoxidil
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- ZFMITUMMTDLWHR-UHFFFAOYSA-N Minoxidil Chemical compound NC1=[N+]([O-])C(N)=CC(N2CCCCC2)=N1 ZFMITUMMTDLWHR-UHFFFAOYSA-N 0.000 title claims abstract description 125
- 229960003632 minoxidil Drugs 0.000 title claims abstract description 125
- 239000007788 liquid Substances 0.000 title claims abstract description 63
- 229940079593 drug Drugs 0.000 title abstract description 4
- 239000003814 drug Substances 0.000 title abstract description 4
- 239000000049 pigment Substances 0.000 claims abstract description 8
- CQPFMGBJSMSXLP-UHFFFAOYSA-M acid orange 7 Chemical compound [Na+].OC1=CC=C2C=CC=CC2=C1N=NC1=CC=C(S([O-])(=O)=O)C=C1 CQPFMGBJSMSXLP-UHFFFAOYSA-M 0.000 claims abstract description 6
- 239000001052 yellow pigment Substances 0.000 claims abstract description 4
- 239000003795 chemical substances by application Substances 0.000 claims description 13
- 238000002360 preparation method Methods 0.000 claims description 8
- UJMBCXLDXJUMFB-UHFFFAOYSA-K trisodium;5-oxo-1-(4-sulfonatophenyl)-4-[(4-sulfonatophenyl)diazenyl]-4h-pyrazole-3-carboxylate Chemical compound [Na+].[Na+].[Na+].[O-]C(=O)C1=NN(C=2C=CC(=CC=2)S([O-])(=O)=O)C(=O)C1N=NC1=CC=C(S([O-])(=O)=O)C=C1 UJMBCXLDXJUMFB-UHFFFAOYSA-K 0.000 claims description 5
- 239000000975 dye Substances 0.000 claims description 4
- 239000001044 red dye Substances 0.000 claims description 4
- GNCOVOVCHIHPHP-UHFFFAOYSA-N 2-[[4-[4-[(1-anilino-1,3-dioxobutan-2-yl)diazenyl]-3-chlorophenyl]-2-chlorophenyl]diazenyl]-3-oxo-n-phenylbutanamide Chemical compound C=1C=CC=CC=1NC(=O)C(C(=O)C)N=NC(C(=C1)Cl)=CC=C1C(C=C1Cl)=CC=C1N=NC(C(C)=O)C(=O)NC1=CC=CC=C1 GNCOVOVCHIHPHP-UHFFFAOYSA-N 0.000 claims description 3
- CYHOWEBNQPOWEI-UHFFFAOYSA-L calcium 3-carboxy-1-phenyldiazenylnaphthalen-2-olate Chemical compound OC=1C(=CC2=CC=CC=C2C1N=NC1=CC=CC=C1)C(=O)[O-].OC=1C(=CC2=CC=CC=C2C1N=NC1=CC=CC=C1)C(=O)[O-].[Ca+2] CYHOWEBNQPOWEI-UHFFFAOYSA-L 0.000 claims description 3
- CTIQLGJVGNGFEW-UHFFFAOYSA-L naphthol yellow S Chemical compound [Na+].[Na+].C1=C(S([O-])(=O)=O)C=C2C([O-])=C([N+]([O-])=O)C=C([N+]([O-])=O)C2=C1 CTIQLGJVGNGFEW-UHFFFAOYSA-L 0.000 claims description 3
- -1 red 201 Chemical compound 0.000 claims description 3
- JBTHDAVBDKKSRW-UHFFFAOYSA-N chembl1552233 Chemical compound CC1=CC(C)=CC=C1N=NC1=C(O)C=CC2=CC=CC=C12 JBTHDAVBDKKSRW-UHFFFAOYSA-N 0.000 claims description 2
- AJDUTMFFZHIJEM-UHFFFAOYSA-N n-(9,10-dioxoanthracen-1-yl)-4-[4-[[4-[4-[(9,10-dioxoanthracen-1-yl)carbamoyl]phenyl]phenyl]diazenyl]phenyl]benzamide Chemical compound O=C1C2=CC=CC=C2C(=O)C2=C1C=CC=C2NC(=O)C(C=C1)=CC=C1C(C=C1)=CC=C1N=NC(C=C1)=CC=C1C(C=C1)=CC=C1C(=O)NC1=CC=CC2=C1C(=O)C1=CC=CC=C1C2=O AJDUTMFFZHIJEM-UHFFFAOYSA-N 0.000 claims description 2
- 239000001043 yellow dye Substances 0.000 claims description 2
- VPWFPZBFBFHIIL-UHFFFAOYSA-L disodium 4-[(4-methyl-2-sulfophenyl)diazenyl]-3-oxidonaphthalene-2-carboxylate Chemical compound [Na+].[Na+].[O-]S(=O)(=O)C1=CC(C)=CC=C1N=NC1=C(O)C(C([O-])=O)=CC2=CC=CC=C12 VPWFPZBFBFHIIL-UHFFFAOYSA-L 0.000 claims 1
- WPPDXAHGCGPUPK-UHFFFAOYSA-N red 2 Chemical compound C1=CC=CC=C1C(C1=CC=CC=C11)=C(C=2C=3C4=CC=C5C6=CC=C7C8=C(C=9C=CC=CC=9)C9=CC=CC=C9C(C=9C=CC=CC=9)=C8C8=CC=C(C6=C87)C(C=35)=CC=2)C4=C1C1=CC=CC=C1 WPPDXAHGCGPUPK-UHFFFAOYSA-N 0.000 claims 1
- LLELVHKMCSBMCX-UHFFFAOYSA-M sodium 1-[(4-chloro-5-methyl-2-sulfophenyl)diazenyl]naphthalen-2-olate Chemical compound [Na+].Cc1cc(N=Nc2c(O)ccc3ccccc23)c(cc1Cl)S([O-])(=O)=O LLELVHKMCSBMCX-UHFFFAOYSA-M 0.000 claims 1
- JAOZKJMVYIWLKU-UHFFFAOYSA-N sodium 7-hydroxy-8-[(4-sulfonaphthalen-1-yl)diazenyl]naphthalene-1,3-disulfonic acid Chemical compound C1=CC=C2C(=C1)C(=CC=C2S(=O)(=O)O)N=NC3=C(C=CC4=CC(=CC(=C43)S(=O)(=O)O)S(=O)(=O)O)O.[Na+] JAOZKJMVYIWLKU-UHFFFAOYSA-N 0.000 claims 1
- 238000001556 precipitation Methods 0.000 abstract description 21
- 238000004040 coloring Methods 0.000 abstract description 8
- 230000000694 effects Effects 0.000 abstract description 2
- 239000001054 red pigment Substances 0.000 abstract description 2
- 230000002123 temporal effect Effects 0.000 abstract 2
- 238000013329 compounding Methods 0.000 abstract 1
- 230000007547 defect Effects 0.000 abstract 1
- 230000002265 prevention Effects 0.000 abstract 1
- 239000000243 solution Substances 0.000 description 147
- LFQSCWFLJHTTHZ-UHFFFAOYSA-N Ethanol Chemical compound CCO LFQSCWFLJHTTHZ-UHFFFAOYSA-N 0.000 description 70
- 238000003756 stirring Methods 0.000 description 65
- 239000008213 purified water Substances 0.000 description 35
- XLYOFNOQVPJJNP-UHFFFAOYSA-N water Chemical compound O XLYOFNOQVPJJNP-UHFFFAOYSA-N 0.000 description 35
- PUPZLCDOIYMWBV-UHFFFAOYSA-N (+/-)-1,3-Butanediol Chemical compound CC(O)CCO PUPZLCDOIYMWBV-UHFFFAOYSA-N 0.000 description 30
- NBIIXXVUZAFLBC-UHFFFAOYSA-N Phosphoric acid Chemical compound OP(O)(O)=O NBIIXXVUZAFLBC-UHFFFAOYSA-N 0.000 description 30
- DNIAPMSPPWPWGF-UHFFFAOYSA-N Propylene glycol Chemical compound CC(O)CO DNIAPMSPPWPWGF-UHFFFAOYSA-N 0.000 description 30
- 239000006210 lotion Substances 0.000 description 29
- 230000000052 comparative effect Effects 0.000 description 27
- JVTAAEKCZFNVCJ-UHFFFAOYSA-N lactic acid Chemical compound CC(O)C(O)=O JVTAAEKCZFNVCJ-UHFFFAOYSA-N 0.000 description 20
- 239000012085 test solution Substances 0.000 description 20
- 238000012360 testing method Methods 0.000 description 16
- 229940058015 1,3-butylene glycol Drugs 0.000 description 15
- 229910000147 aluminium phosphate Inorganic materials 0.000 description 15
- 235000019437 butane-1,3-diol Nutrition 0.000 description 15
- SMWDFEZZVXVKRB-UHFFFAOYSA-N Quinoline Chemical compound N1=CC=CC2=CC=CC=C21 SMWDFEZZVXVKRB-UHFFFAOYSA-N 0.000 description 10
- 239000004310 lactic acid Substances 0.000 description 10
- 235000014655 lactic acid Nutrition 0.000 description 10
- 238000013112 stability test Methods 0.000 description 10
- LGZQSRCLLIPAEE-UHFFFAOYSA-M sodium 1-[(4-sulfonaphthalen-1-yl)diazenyl]naphthalen-2-olate Chemical compound [Na+].C1=CC=C2C(N=NC3=C4C=CC=CC4=CC=C3O)=CC=C(S([O-])(=O)=O)C2=C1 LGZQSRCLLIPAEE-UHFFFAOYSA-M 0.000 description 8
- GJCOSYZMQJWQCA-UHFFFAOYSA-N 9H-xanthene Chemical compound C1=CC=C2CC3=CC=CC=C3OC2=C1 GJCOSYZMQJWQCA-UHFFFAOYSA-N 0.000 description 7
- QDLAGTHXVHQKRE-UHFFFAOYSA-N lichenxanthone Natural products COC1=CC(O)=C2C(=O)C3=C(C)C=C(OC)C=C3OC2=C1 QDLAGTHXVHQKRE-UHFFFAOYSA-N 0.000 description 7
- UBVSIAHUTXHQTD-UHFFFAOYSA-N 2-n-(4-bromophenyl)-1,3,5-triazine-2,4-diamine Chemical compound NC1=NC=NC(NC=2C=CC(Br)=CC=2)=N1 UBVSIAHUTXHQTD-UHFFFAOYSA-N 0.000 description 5
- SGHZXLIDFTYFHQ-UHFFFAOYSA-L Brilliant Blue Chemical compound [Na+].[Na+].C=1C=C(C(=C2C=CC(C=C2)=[N+](CC)CC=2C=C(C=CC=2)S([O-])(=O)=O)C=2C(=CC=CC=2)S([O-])(=O)=O)C=CC=1N(CC)CC1=CC=CC(S([O-])(=O)=O)=C1 SGHZXLIDFTYFHQ-UHFFFAOYSA-L 0.000 description 5
- 235000012732 erythrosine Nutrition 0.000 description 5
- 238000011156 evaluation Methods 0.000 description 5
- AAAQKTZKLRYKHR-UHFFFAOYSA-N triphenylmethane Chemical compound C1=CC=CC=C1C(C=1C=CC=CC=1)C1=CC=CC=C1 AAAQKTZKLRYKHR-UHFFFAOYSA-N 0.000 description 5
- WLDHEUZGFKACJH-ZRUFZDNISA-K Amaranth Chemical group [Na+].[Na+].[Na+].C12=CC=C(S([O-])(=O)=O)C=C2C=C(S([O-])(=O)=O)C(O)=C1\N=N\C1=CC=C(S([O-])(=O)=O)C2=CC=CC=C12 WLDHEUZGFKACJH-ZRUFZDNISA-K 0.000 description 4
- FHNINJWBTRXEBC-UHFFFAOYSA-N Sudan III Chemical compound OC1=CC=C2C=CC=CC2=C1N=NC(C=C1)=CC=C1N=NC1=CC=CC=C1 FHNINJWBTRXEBC-UHFFFAOYSA-N 0.000 description 4
- POJOORKDYOPQLS-UHFFFAOYSA-L barium(2+) 5-chloro-2-[(2-hydroxynaphthalen-1-yl)diazenyl]-4-methylbenzenesulfonate Chemical compound [Ba+2].C1=C(Cl)C(C)=CC(N=NC=2C3=CC=CC=C3C=CC=2O)=C1S([O-])(=O)=O.C1=C(Cl)C(C)=CC(N=NC=2C3=CC=CC=C3C=CC=2O)=C1S([O-])(=O)=O POJOORKDYOPQLS-UHFFFAOYSA-L 0.000 description 3
- GNBHRKFJIUUOQI-UHFFFAOYSA-N fluorescein Chemical compound O1C(=O)C2=CC=CC=C2C21C1=CC=C(O)C=C1OC1=CC(O)=CC=C21 GNBHRKFJIUUOQI-UHFFFAOYSA-N 0.000 description 3
- 238000002156 mixing Methods 0.000 description 3
- 235000012752 quinoline yellow Nutrition 0.000 description 3
- 239000004172 quinoline yellow Substances 0.000 description 3
- 235000009328 Amaranthus caudatus Nutrition 0.000 description 2
- 240000001592 Amaranthus caudatus Species 0.000 description 2
- OIQPTROHQCGFEF-QIKYXUGXSA-L Sunset Yellow FCF Chemical compound [Na+].[Na+].OC1=CC=C2C=C(S([O-])(=O)=O)C=CC2=C1\N=N\C1=CC=C(S([O-])(=O)=O)C=C1 OIQPTROHQCGFEF-QIKYXUGXSA-L 0.000 description 2
- 235000012735 amaranth Nutrition 0.000 description 2
- 239000004178 amaranth Substances 0.000 description 2
- 230000003779 hair growth Effects 0.000 description 2
- 230000003405 preventing effect Effects 0.000 description 2
- VVNRQZDDMYBBJY-UHFFFAOYSA-M sodium 1-[(1-sulfonaphthalen-2-yl)diazenyl]naphthalen-2-olate Chemical compound [Na+].C1=CC=CC2=C(S([O-])(=O)=O)C(N=NC3=C4C=CC=CC4=CC=C3O)=CC=C21 VVNRQZDDMYBBJY-UHFFFAOYSA-M 0.000 description 2
- WDAWIIXWJBEKSA-UHFFFAOYSA-N sodium 4-(5-methyl-3-oxo-4-phenyldiazenyl-1H-pyrazol-2-yl)benzenesulfonic acid Chemical compound CC1=C(C(=O)N(N1)C2=CC=C(C=C2)S(=O)(=O)O)N=NC3=CC=CC=C3.[Na+] WDAWIIXWJBEKSA-UHFFFAOYSA-N 0.000 description 2
- AZLXCBPKSXFMET-UHFFFAOYSA-M sodium 4-[(4-sulfophenyl)diazenyl]naphthalen-1-olate Chemical compound [Na+].C12=CC=CC=C2C(O)=CC=C1N=NC1=CC=C(S([O-])(=O)=O)C=C1 AZLXCBPKSXFMET-UHFFFAOYSA-M 0.000 description 2
- 229940099373 sudan iii Drugs 0.000 description 2
- 235000012751 sunset yellow FCF Nutrition 0.000 description 2
- 239000004173 sunset yellow FCF Substances 0.000 description 2
- UHOVQNZJYSORNB-UHFFFAOYSA-N Benzene Chemical compound C1=CC=CC=C1 UHOVQNZJYSORNB-UHFFFAOYSA-N 0.000 description 1
- KLCDQSGLLRINHY-VHEBQXMUSA-N Yellow AB Chemical compound NC1=CC=C2C=CC=CC2=C1\N=N\C1=CC=CC=C1 KLCDQSGLLRINHY-VHEBQXMUSA-N 0.000 description 1
- BWLVSYUUKOQICP-FMQUCBEESA-N Yellow OB Chemical compound CC1=CC=CC=C1\N=N\C1=C(N)C=CC2=CC=CC=C12 BWLVSYUUKOQICP-FMQUCBEESA-N 0.000 description 1
- 239000002253 acid Substances 0.000 description 1
- 239000000443 aerosol Substances 0.000 description 1
- LFZDEAVRTJKYAF-UHFFFAOYSA-L barium(2+) 2-[(2-hydroxynaphthalen-1-yl)diazenyl]naphthalene-1-sulfonate Chemical compound [Ba+2].C1=CC=CC2=C(S([O-])(=O)=O)C(N=NC3=C4C=CC=CC4=CC=C3O)=CC=C21.C1=CC=CC2=C(S([O-])(=O)=O)C(N=NC3=C4C=CC=CC4=CC=C3O)=CC=C21 LFZDEAVRTJKYAF-UHFFFAOYSA-L 0.000 description 1
- ZLFVRXUOSPRRKQ-UHFFFAOYSA-N chembl2138372 Chemical compound [O-][N+](=O)C1=CC(C)=CC=C1N=NC1=C(O)C=CC2=CC=CC=C12 ZLFVRXUOSPRRKQ-UHFFFAOYSA-N 0.000 description 1
- 238000006243 chemical reaction Methods 0.000 description 1
- 239000002537 cosmetic Substances 0.000 description 1
- 239000000284 extract Substances 0.000 description 1
- 239000000499 gel Substances 0.000 description 1
- 238000011835 investigation Methods 0.000 description 1
- 239000000865 liniment Substances 0.000 description 1
- 239000012669 liquid formulation Substances 0.000 description 1
- SXQCTESRRZBPHJ-UHFFFAOYSA-M lissamine rhodamine Chemical compound [Na+].C=12C=CC(=[N+](CC)CC)C=C2OC2=CC(N(CC)CC)=CC=C2C=1C1=CC=C(S([O-])(=O)=O)C=C1S([O-])(=O)=O SXQCTESRRZBPHJ-UHFFFAOYSA-M 0.000 description 1
- 229940051142 metanil yellow Drugs 0.000 description 1
- NYGZLYXAPMMJTE-UHFFFAOYSA-M metanil yellow Chemical compound [Na+].[O-]S(=O)(=O)C1=CC=CC(N=NC=2C=CC(NC=3C=CC=CC=3)=CC=2)=C1 NYGZLYXAPMMJTE-UHFFFAOYSA-M 0.000 description 1
- 239000000203 mixture Substances 0.000 description 1
- 239000001053 orange pigment Substances 0.000 description 1
- 229940051201 quinoline yellow Drugs 0.000 description 1
- IZMJMCDDWKSTTK-UHFFFAOYSA-N quinoline yellow Chemical compound C1=CC=CC2=NC(C3C(C4=CC=CC=C4C3=O)=O)=CC=C21 IZMJMCDDWKSTTK-UHFFFAOYSA-N 0.000 description 1
- PYWVYCXTNDRMGF-UHFFFAOYSA-N rhodamine B Chemical compound [Cl-].C=12C=CC(=[N+](CC)CC)C=C2OC2=CC(N(CC)CC)=CC=C2C=1C1=CC=CC=C1C(O)=O PYWVYCXTNDRMGF-UHFFFAOYSA-N 0.000 description 1
- DXKDBQWDRGRKGC-UHFFFAOYSA-M sodium;5-chloro-2-[3-methyl-4-[[4-(4-methylphenyl)sulfonyloxyphenyl]diazenyl]-5-oxo-4h-pyrazol-1-yl]benzenesulfonate Chemical compound [Na+].CC1=NN(C=2C(=CC(Cl)=CC=2)S([O-])(=O)=O)C(=O)C1N=NC(C=C1)=CC=C1OS(=O)(=O)C1=CC=C(C)C=C1 DXKDBQWDRGRKGC-UHFFFAOYSA-M 0.000 description 1
- 235000015096 spirit Nutrition 0.000 description 1
- 235000012756 tartrazine Nutrition 0.000 description 1
- 239000004149 tartrazine Substances 0.000 description 1
- 229960000943 tartrazine Drugs 0.000 description 1
- UJMBCXLDXJUMFB-GLCFPVLVSA-K tartrazine Chemical compound [Na+].[Na+].[Na+].[O-]C(=O)C1=NN(C=2C=CC(=CC=2)S([O-])(=O)=O)C(=O)C1\N=N\C1=CC=C(S([O-])(=O)=O)C=C1 UJMBCXLDXJUMFB-GLCFPVLVSA-K 0.000 description 1
- 235000015961 tonic Nutrition 0.000 description 1
- 230000001256 tonic effect Effects 0.000 description 1
- 229960000716 tonics Drugs 0.000 description 1
Landscapes
- Medicinal Preparation (AREA)
- Pharmaceuticals Containing Other Organic And Inorganic Compounds (AREA)
Abstract
Description
本発明は、経時的な着色を防止したミノキシジル含有液剤に関する。 The present invention relates to a minoxidil-containing liquid agent that prevents coloring over time.
ミノキシジルは、外用塗布により優れた育毛・発毛効果を発揮する薬剤であり、ローション又はエアゾールタイプのミノキシジル含有外用剤が国内外で市販されている(特許文献1参照)。しかしながら、ミノキシジルを溶液状態で保存すると経時的に着色しやすいという欠点があり、商品価値の低下を招くおそれがあった。 Minoxidil is a drug that exhibits an excellent hair-growth / hair-growth effect by external application, and a lotion or aerosol-type external preparation containing minoxidil is commercially available in Japan and overseas (see Patent Document 1). However, when minoxidil is stored in a solution state, there is a drawback that it tends to be colored with time, which may cause a reduction in commercial value.
本発明は、ミノキシジルを配合した液剤の継時的な着色を防止することを目的とする。 An object of this invention is to prevent the coloring over time of the liquid agent which mix | blended minoxidil.
一般的に着色しやすい成分を液剤に配合するには、色素などをあらかじめ配合することにより、色変化を目立たなくすることが考えられる。しかしながら、ミノキシジル含有液剤にあっては色素を配合すると、光によりミノキシジルと色素が反応し沈殿を生じる場合や、更には熱または光によって、着色を防止するどころかむしろ色変化が目立つ場合があることを本発明者らは発見した。 In general, in order to blend easily colored components into the liquid, it is conceivable to make the color change inconspicuous by blending pigments and the like in advance. However, in the case of a minoxidil-containing liquid agent, when a pigment is added, it may cause precipitation when the minoxidil and the pigment react with light, and further, color change may be noticeable rather than preventing coloration due to heat or light. The inventors have discovered.
そこで、この問題を解決すべく鋭意検討した結果、特定の色素を配合したミノキシジル含有液剤は、上記のような不利益がなく、継時的な着色及び沈殿防止効果が得られることを見出し、本発明を完成するに至った。かかる知見により得られた本発明の態様は次のとおりである。 Therefore, as a result of diligent investigations to solve this problem, it was found that the minoxidil-containing liquid formulation containing a specific dye has the above disadvantages and can obtain a continuous coloring and precipitation preventing effect. The invention has been completed. The embodiments of the present invention obtained from such findings are as follows.
(1)ミノキシジル、並びに、黄色色素、アゾ系赤色色素、橙色205号及び橙色402号からなる群から選ばれる1種以上を含有することを特徴とする液剤、
(2)黄色色素が、黄色4号、黄色5号、黄色201号、黄色202号の(1)、黄色202号の(2)、黄色203号、黄色204号、黄色205号、黄色401号、黄色402号、黄色403号の(1)、黄色404号、黄色405号、黄色406号及び黄色407号からなる群から選ばれる1種以上である前記(1)の液剤、
(3)アゾ系赤色色素が、赤色2号、赤色102号、赤色201号、赤色202号、赤色203号、赤色204号、赤色205号、赤色206号、赤色207号、赤色208号、赤色219号、赤色220号、赤色221号、赤色225号、赤色227号、赤色228号、赤色404号、赤色405号、赤色501号、赤色502号、赤色503号、赤色504号、赤色505号及び赤色506号からなる群から選ばれる1種以上である前記(1)の液剤、
(4)ミノキシジルの含有量が1w/v%以上である前記(1)〜(3)のいずれかに記載の液剤、
(5)色素の含有量が5w/v%以下である前記(1)〜(4)のいずれかに記載の液剤、
(6)液剤のpHが4.5〜9.5である前記(1)〜(5)のいずれかに記載の液剤である。
(1) A liquid agent characterized by containing minoxidil and one or more selected from the group consisting of yellow dye, azo red dye, orange No. 205 and orange No. 402,
(2) The yellow pigment is yellow 4, yellow 5, yellow 201, yellow 202 (1), yellow 202 (2), yellow 203, yellow 204, yellow 205, yellow 401 Yellow No. 402, Yellow No. 403 (1), Yellow No. 404, Yellow No. 405, Yellow No. 406 and Yellow No. 407
(3) The azo red pigment is red No. 2, Red No. 102, Red No. 201, Red No. 202, Red No. 203, Red No. 204, Red No. 205, Red No. 206, Red No. 207, Red No. 208, Red 219, Red 220, Red 221, Red 225, Red 227, Red 228, Red 404, Red 405, Red 501, Red 502, Red 503, Red 504, Red 505 And at least one selected from the group consisting of Red No. 506, (1)
(4) The liquid agent according to any one of (1) to (3), wherein the content of minoxidil is 1 w / v% or more,
(5) The liquid agent according to any one of (1) to (4), wherein the pigment content is 5 w / v% or less,
(6) The liquid according to any one of (1) to (5), wherein the pH of the liquid is 4.5 to 9.5.
本発明の液剤に含まれるミノキシジルの含有量は、1w/v%以上、好ましくは、3w/v%以上、より好ましくは、5w/v%以上である。 The content of minoxidil contained in the liquid preparation of the present invention is 1 w / v% or more, preferably 3 w / v% or more, more preferably 5 w / v% or more.
本発明の色素は、合成色素又は天然色素であってもよく、可視光域における極大波長が395nm〜527nmであるものが好ましい。 The coloring matter of the present invention may be a synthetic coloring matter or a natural coloring matter, and preferably has a maximum wavelength in the visible light range of 395 nm to 527 nm.
本発明の黄色色素としては、黄色4号(別名タートラジン)、黄色5号(別名サンセットイエローFCF)、黄色201号(別名フルオレセイン)、黄色202号の(1)(別名ウラニン)、黄色202号の(2)(別名ウラニンK)、黄色203号(別名キノリンイエローWS)、黄色204号(別名キノリンイエローSS)、黄色205号(別名ベンチジンイエローG)、黄色401号(別名ハンサイエロー)、黄色402号(別名ポーライエロー5G)、黄色403号の(1)(別名ナフトールイエローS)、黄色404号(別名イエローAB)、黄色405号(別名イエローOB)、黄色406号(別名メタニルイエロー)、黄色407号(別名ファストライトイエロー3G)が好ましく、特に好ましくは、黄色4号(別名タートラジン)、黄色5号(別名サンセットイエローFCF)、黄色203号(別名キノリンイエローWS)、黄色406号(別名メタニルイエロー)、黄色407号(別名ファストライトイエロー3G)である。これらは1種のみが用いられても良く、2種以上が併用されてもよい。 As yellow pigments of the present invention, yellow No. 4 (also known as tartrazine), yellow No. 5 (also known as Sunset Yellow FCF), yellow 201 (also known as fluorescein), yellow 202 (1) (also known as uranin), yellow 202 (2) (also known as uranin K), yellow 203 (also known as quinoline yellow WS), yellow 204 (also known as quinoline yellow SS), yellow 205 (also known as benzine yellow G), yellow 401 (also known as Hansa Yellow), Yellow 402 (also known as Polar Yellow 5G), Yellow 403 (1) (also known as Naphthol Yellow S), Yellow 404 (also known as Yellow AB), Yellow 405 (also known as Yellow OB), Yellow 406 (also known as Methanil Yellow) ), Yellow 407 (also known as fast light yellow 3G), and particularly preferably yellow 4 (also known as tartra) Emissions), Yellow No. 5 (also known as Sunset Yellow FCF), Yellow No. 203 (also known as quinoline yellow WS), Yellow 406 No. (aka metanil yellow), a yellow 407 No. (aka Fast Light Yellow 3G). Only 1 type may be used for these and 2 or more types may be used together.
本発明のアゾ系赤色色素としては、赤色2号(別名アマランス)、赤色102号(別名ニューコクシン)、赤色201号(別名リソールルビンB)、赤色202号(別名リソールルビンBCA)、赤色203号(別名レーキレッドC)、赤色204号(別名レーキレッドCBA)、赤色205号(別名リソールレッド)、赤色206号(別名リソールレッドCA)、赤色207号(別名リソールレッドBA)、赤色208号(別名リソールレッドSR)、赤色219号(別名ブリリアントレーキレッドR)、赤色220号(別名ディープマルーン)、赤色221号(別名トルイジンレッド)、赤色225号(別名スダンIII)、赤色227号(別名ファストアシッドマゲンタ)、赤色228号(別名パーマトンレッド)、赤色404号(別名ブリリアントファストスカーレット)、赤色405号(別名パーマネントレッドF5R)、赤色501号(別名スカーレットレッドNF)、赤色502号(別名ポンソー3R)、赤色503号(別名ポンソーR)、赤色504号(別名ポンソーSX)、赤色505号(別名オイルレッドXO)、赤色506号(別名ファストレッドS)が好ましく、特に好ましくは、赤色2号(別名アマランス)、赤色225号(別名スダンIII)である。これらは1種のみが用いられても良く、2種以上が併用されてもよい。 Examples of the azo red dye of the present invention include Red No. 2 (also known as Amaranth), Red No. 102 (also known as New Coxin), Red No. 201 (also known as Risol Rubin BCA), Red No. 202 (also known as Risol Rubin BCA), and Red No. 203 ( Also known as Lake Red C), Red 204 (aka Lake Red CBA), Red 205 (aka Resor Red), Red 206 (aka Resor Red CA), Red 207 (aka Resor Red BA), Red 208 (alias Resor Red SR), Red 219 (also known as Brillant Lake Red R), Red 220 (also known as Deep Maroon), Red 221 (also known as Toluidine Red), Red 225 (also known as Sudan III), Red 227 (also known as Fast Acid) Magenta), Red 228 (aka Palmaton Red), Red 404 (aka Brilliant Fasts) Red) 405 (aka Permanent Red F5R), red 501 (aka Scarlet Red NF), red 502 (aka Ponso 3R), red 503 (aka Ponso R), red 504 (aka Ponso SX), Red No. 505 (aka Oil Red XO) and Red No. 506 (aka Fast Red S) are preferred, and Red No. 2 (aka Amaranth) and Red No. 225 (aka Sudan III) are particularly preferred. Only 1 type may be used for these and 2 or more types may be used together.
本発明の橙色205号は別名オレンジIIと称し、橙色402号は別名オレンジIと称する橙色色素である。これらは1種のみが用いられても良く、2種以上が併用されてもよい。 Orange No. 205 of the present invention is an alias pigment referred to as Orange II, and Orange No. 402 is an orange pigment referred to as Orange I. Only 1 type may be used for these and 2 or more types may be used together.
本発明の液剤に含まれる色素の含有量は、5w/v%以下、好ましくは、3w/v%以下、より好ましくは、0.0001〜0.1w/v%以下である。 Content of the pigment | dye contained in the liquid agent of this invention is 5 w / v% or less, Preferably, it is 3 w / v% or less, More preferably, it is 0.0001-0.1 w / v% or less.
本発明の液剤のpHは、4.5〜9.5、好ましくは、4.9〜9.1、より好ましくは、5.5〜8.5である。 The pH of the liquid preparation of the present invention is 4.5 to 9.5, preferably 4.9 to 9.1, and more preferably 5.5 to 8.5.
本発明の液剤は、ローション剤、ゲル剤、エキス剤、酒精剤、チンキ剤、リニメント剤、エアゾール剤が含まれる。さらに、ローション、ヘアトニック、ヘアリキッド等の化粧料も本発明の液剤に含まれる。 The liquid preparation of the present invention includes lotions, gels, extracts, spirits, tinctures, liniments, and aerosols. Furthermore, cosmetics such as lotions, hair tonics and hair liquids are also included in the liquid preparation of the present invention.
以下に、実施例、比較例及び試験例を記載し、本発明をさらに具体的に説明するが、本発明はこれら実施例等により何ら制約されるものではない。 EXAMPLES Examples, comparative examples, and test examples will be described below, and the present invention will be described more specifically. However, the present invention is not limited by these examples.
(実施例1)
ミノキシジル5g、1,3−ブチレングリコール10g、エタノール60gにリン酸適量を添加し、精製水で全量を100mLとし、撹拌溶解してミノキシジル溶液を調製した。このミノキシジル溶液44mLに赤色2号(アゾ系)0.0044gを添加し、撹拌溶解してミノキシジル-赤色2号0.01w/v%溶液を調製した。さらに、ミノキシジル-赤色2号0.01w/v%溶液4mLをミノキシジル溶液36mLに添加混合することにより、ローションタイプの液剤を得た。液剤のpHは6.1、可視光域における極大波長は527nmであった。
Example 1
An appropriate amount of phosphoric acid was added to 5 g of minoxidil, 10 g of 1,3-butylene glycol and 60 g of ethanol, and the total amount was adjusted to 100 mL with purified water, and dissolved by stirring to prepare a minoxidil solution. To 44 mL of this minoxidil solution, 0.0044 g of red No. 2 (azo) was added and dissolved by stirring to prepare a minoxidil-red No. 2 0.01 w / v% solution. Furthermore, a lotion-type liquid was obtained by adding 4 mL of Minoxidil-Red No. 2 0.01 w / v% solution to 36 mL of Minoxidil solution. The pH of the solution was 6.1, and the maximum wavelength in the visible light range was 527 nm.
(実施例2)
ミノキシジル5g、1,3−ブチレングリコール10g、エタノール60gにリン酸適量を添加し、精製水で全量を100mLとし、撹拌溶解してミノキシジル溶液を調製した。このミノキシジル溶液44mLに赤色225号(アゾ系)0.0044gを添加し、撹拌溶解してミノキシジル-赤色225号0.01w/v%溶液を調製した。さらに、ミノキシジル-赤色225号0.01w/v%溶液4mLをミノキシジル溶液36mLに添加混合することにより、ローションタイプの液剤を得た。液剤のpHは6.1、可視光域における極大波長は512nmであった。
(Example 2)
An appropriate amount of phosphoric acid was added to 5 g of minoxidil, 10 g of 1,3-butylene glycol and 60 g of ethanol, and the total amount was adjusted to 100 mL with purified water, and dissolved by stirring to prepare a minoxidil solution. To 44 ml of this minoxidil solution, 0.0044 g of red No. 225 (azo) was added and dissolved by stirring to prepare a minoxidil-red No. 225 0.01 w / v% solution. Furthermore, a lotion-type liquid was obtained by adding 4 mL of Minoxidil-Red 225 0.01 w / v% solution to 36 mL of Minoxidil solution. The pH of the solution was 6.1, and the maximum wavelength in the visible light region was 512 nm.
(実施例3)
ミノキシジル5g、1,3−ブチレングリコール10g、エタノール60gにリン酸適量を添加し、精製水で全量を100mLとし、撹拌溶解してミノキシジル溶液を調製した。このミノキシジル溶液44mLに黄色4号(アゾ系)0.0044gを添加し、撹拌溶解してミノキシジル-黄色4号0.01w/v%溶液を調製した。さらに、ミノキシジル-黄色4号0.01w/v%溶液4mLをミノキシジル溶液36mLに添加混合することにより、ローションタイプの液剤を得た。液剤のpHは6.1、可視光域における極大波長は431nmであった。
(Example 3)
An appropriate amount of phosphoric acid was added to 5 g of minoxidil, 10 g of 1,3-butylene glycol and 60 g of ethanol, and the total amount was adjusted to 100 mL with purified water, and dissolved by stirring to prepare a minoxidil solution. To 44 mL of this minoxidil solution, 0.0044 g of yellow No. 4 (azo type) was added and dissolved by stirring to prepare a 0.01 w / v% solution of minoxidil-yellow No. 4. Further, 4 ml of Minoxidil-Yellow No. 4 0.01 w / v% solution was added to and mixed with 36 mL of Minoxidil solution to obtain a lotion type liquid. The pH of the solution was 6.1, and the maximum wavelength in the visible light range was 431 nm.
(実施例4)
ミノキシジル5g、1,3−ブチレングリコール10g、エタノール60gにリン酸適量を添加し、精製水で全量を100mLとし、撹拌溶解してミノキシジル溶液を調製した。このミノキシジル溶液44mLに黄色5号(アゾ系)0.0044gを添加し、撹拌溶解してミノキシジル-黄色5号0.01w/v%溶液を調製した。さらに、ミノキシジル-黄色5号0.01w/v%溶液4mLをミノキシジル溶液36mLに添加混合することにより、ローションタイプの液剤を得た。液剤のpHは6.1、可視光域における極大波長は486nmであった。
Example 4
An appropriate amount of phosphoric acid was added to 5 g of minoxidil, 10 g of 1,3-butylene glycol and 60 g of ethanol, and the total amount was adjusted to 100 mL with purified water, and dissolved by stirring to prepare a minoxidil solution. To 44 mL of this minoxidil solution, 0.0044 g of yellow No. 5 (azo type) was added and dissolved by stirring to prepare a 0.01 w / v% solution of minoxidil-yellow No. 5. Furthermore, a lotion-type liquid was obtained by adding 4 mL of a minoxidil-yellow No. 5 0.01 w / v% solution to 36 mL of the minoxidil solution. The pH of the solution was 6.1, and the maximum wavelength in the visible light region was 486 nm.
(実施例5)
ミノキシジル5g、1,3−ブチレングリコール10g、エタノール60gにリン酸適量を添加し、精製水で全量を100mLとし、撹拌溶解してミノキシジル溶液を調製した。このミノキシジル溶液44mLに黄色203号(キノリン系)0.0044gを添加し、撹拌溶解してミノキシジル-黄色203号0.01w/v%溶液を調製した。さらに、ミノキシジル-黄色203号0.01w/v%溶液4mLをミノキシジル溶液36mLに添加混合することにより、ローションタイプの液剤を得た。液剤のpHは6.1、可視光域における極大波長は420nmであった。
(Example 5)
An appropriate amount of phosphoric acid was added to 5 g of minoxidil, 10 g of 1,3-butylene glycol and 60 g of ethanol, and the total amount was adjusted to 100 mL with purified water, and dissolved by stirring to prepare a minoxidil solution. To 44 mL of this minoxidil solution, 0.0044 g of yellow No. 203 (quinoline) was added and dissolved by stirring to prepare a minoxidil-yellow No. 203 0.01 w / v% solution. Furthermore, a lotion-type liquid was obtained by adding 4 mL of Minoxidil-Yellow No. 203 0.01 w / v% solution to 36 mL of Minoxidil solution. The pH of the solution was 6.1, and the maximum wavelength in the visible light range was 420 nm.
(実施例6)
ミノキシジル5g、1,3−ブチレングリコール10g、エタノール60gにリン酸適量を添加し、精製水で全量を100mLとし、撹拌溶解してミノキシジル溶液を調製した。このミノキシジル溶液44mLに黄色406号(アゾ系)0.0044gを添加し、撹拌溶解してミノキシジル-黄色406号0.01w/v%溶液を調製した。さらに、ミノキシジル-黄色406号0.01w/v%溶液4mLをミノキシジル溶液36mLに添加混合することにより、ローションタイプの液剤を得た。液剤のpHは6.1、可視光域における極大波長は423nmであった。
(Example 6)
An appropriate amount of phosphoric acid was added to 5 g of minoxidil, 10 g of 1,3-butylene glycol and 60 g of ethanol, and the total amount was adjusted to 100 mL with purified water, and dissolved by stirring to prepare a minoxidil solution. To 44 mL of this minoxidil solution, 0.0044 g of yellow 406 (azo) was added and dissolved by stirring to prepare a 0.01 w / v% solution of minoxidil-yellow 406. Furthermore, a lotion-type liquid was obtained by adding 4 mL of a minoxidil-yellow 406 0.01 w / v% solution to 36 mL of the minoxidil solution. The pH of the solution was 6.1, and the maximum wavelength in the visible light region was 423 nm.
(比較例1)
ミノキシジル5g、1,3−ブチレングリコール10g、エタノール60gにリン酸適量を添加し、精製水で全量を100mLとし、撹拌溶解してミノキシジル溶液を調製した。このミノキシジル溶液44mLに赤色3号(キサンテン系)0.0044gを添加し、撹拌溶解してミノキシジル-赤色3号0.01w/v%溶液を調製した。さらに、ミノキシジル-赤色3号0.01w/v%溶液4mLをミノキシジル溶液36mLに添加混合することにより、ローションタイプの液剤を得た。液剤のpHは6.1、可視光域における極大波長は539nmであった。
(Comparative Example 1)
An appropriate amount of phosphoric acid was added to 5 g of minoxidil, 10 g of 1,3-butylene glycol and 60 g of ethanol, and the total amount was adjusted to 100 mL with purified water, and dissolved by stirring to prepare a minoxidil solution. To 44 mL of this minoxidil solution, 0.0044 g of red No. 3 (xanthene) was added and dissolved by stirring to prepare a minoxidil-red No. 3 0.01 w / v% solution. Further, 4 ml of Minoxidil-Red No. 3 0.01 w / v% solution was added to and mixed with 36 mL of Minoxidil solution to obtain a lotion type liquid. The pH of the solution was 6.1, and the maximum wavelength in the visible light region was 539 nm.
(比較例2)
ミノキシジル5g、1,3−ブチレングリコール10g、エタノール60gにリン酸適量を添加し、精製水で全量を100mLとし、撹拌溶解してミノキシジル溶液を調製した。このミノキシジル溶液44mLに赤色106号(キサンテン系)0.0044gを添加し、撹拌溶解してミノキシジル-赤色106号0.01w/v%溶液を調製した。さらに、ミノキシジル-赤色106号0.01w/v%溶液4mLをミノキシジル溶液36mLに添加混合することにより、ローションタイプの液剤を得た。液剤のpHは6.1、可視光域における極大波長は561nmであった。
(Comparative Example 2)
An appropriate amount of phosphoric acid was added to 5 g of minoxidil, 10 g of 1,3-butylene glycol and 60 g of ethanol, and the total amount was adjusted to 100 mL with purified water, and dissolved by stirring to prepare a minoxidil solution. To 44 mL of this minoxidil solution, 0.0044 g of red No. 106 (xanthene) was added and dissolved by stirring to prepare a minoxidil-red No. 106 0.01 w / v% solution. Furthermore, a lotion-type liquid was obtained by adding 4 mL of Minoxidil-Red 106 0.01 w / v% solution to 36 mL of Minoxidil solution. The pH of the solution was 6.1, and the maximum wavelength in the visible light region was 561 nm.
(比較例3)
ミノキシジル5g、1,3−ブチレングリコール10g、エタノール60gにリン酸適量を添加し、精製水で全量を100mLとし、撹拌溶解してミノキシジル溶液を調製した。このミノキシジル溶液44mLに赤色213号(キサンテン系)0.0044gを添加し、撹拌溶解してミノキシジル-赤色213号0.01w/v%溶液を調製した。さらに、ミノキシジル-赤色213号0.01w/v%溶液4mLをミノキシジル溶液36mLに添加混合することにより、ローションタイプの液剤を得た。液剤のpHは6.1、可視光域における極大波長は551nmであった。
(Comparative Example 3)
An appropriate amount of phosphoric acid was added to 5 g of minoxidil, 10 g of 1,3-butylene glycol and 60 g of ethanol, and the total amount was adjusted to 100 mL with purified water, and dissolved by stirring to prepare a minoxidil solution. To 44 mL of this minoxidil solution, 0.0044 g of red No. 213 (xanthene) was added and dissolved by stirring to prepare a 0.01 w / v% solution of minoxidil-red No. 213. Furthermore, a lotion-type liquid was obtained by adding and mixing 4 mL of a minoxidil-red 213 0.01 w / v% solution to 36 mL of the minoxidil solution. The pH of the solution was 6.1, and the maximum wavelength in the visible light range was 551 nm.
(比較例4)
ミノキシジル5g、1,3−ブチレングリコール10g、エタノール60gにリン酸適量を添加し、精製水で全量を100mLとし、撹拌溶解してミノキシジル溶液を調製した。このミノキシジル溶液44mLに青色1号(トリフェニルメタン系)0.0044gを添加し、撹拌溶解してミノキシジル-青色1号0.01w/v%溶液を調製した。さらに、ミノキシジル-青色1号0.01w/v%溶液4mLをミノキシジル溶液36mLに添加混合することにより、ローションタイプの液剤を得た。液剤のpHは6.1、可視光域における極大波長は630nmであった。
(Comparative Example 4)
An appropriate amount of phosphoric acid was added to 5 g of minoxidil, 10 g of 1,3-butylene glycol and 60 g of ethanol, and the total amount was adjusted to 100 mL with purified water, and dissolved by stirring to prepare a minoxidil solution. To 44 mL of this minoxidil solution, 0.0044 g of blue No. 1 (triphenylmethane) was added and dissolved by stirring to prepare a minoxidil-blue No. 1 0.01 w / v% solution. Furthermore, a lotion-type liquid was obtained by adding 4 mL of Minoxidil-Blue No. 1 0.01 w / v% solution to 36 mL of Minoxidil solution. The pH of the solution was 6.1, and the maximum wavelength in the visible light region was 630 nm.
(比較例5)
ミノキシジル5g、1,3−ブチレングリコール10g、エタノール60gにリン酸適量を添加し、精製水で全量を100mLとし、撹拌溶解してミノキシジル溶液を調製した。このミノキシジル溶液44mLに橙色204号0.0044gを添加し、撹拌溶解してミノキシジル-橙色204号(アゾ系)0.01w/v%溶液を調製した。さらに、ミノキシジル-橙色204号0.01w/v%溶液4mLをミノキシジル溶液36mLに添加混合することにより、ローションタイプの液剤を得た。本液剤は調製直後に沈殿が認められた。
(Comparative Example 5)
An appropriate amount of phosphoric acid was added to 5 g of minoxidil, 10 g of 1,3-butylene glycol and 60 g of ethanol, and the total amount was adjusted to 100 mL with purified water, and dissolved by stirring to prepare a minoxidil solution. To 44 mL of this minoxidil solution, 0.0044 g of orange No. 204 was added and dissolved by stirring to prepare a 0.01 w / v% solution of minoxidil-orange No. 204 (azo). Furthermore, a lotion-type liquid was obtained by adding and mixing 4 mL of a minoxidil-orange 204 0.01 w / v% solution to 36 mL of the minoxidil solution. Precipitation was observed immediately after preparation of this solution.
(比較例6)
ミノキシジル5g、1,3−ブチレングリコール10g、エタノール60gにリン酸適量を添加し、精製水で全量を100mLとし、撹拌溶解してローションタイプの液剤を得た。液剤のpHは6.2であった。
(Comparative Example 6)
An appropriate amount of phosphoric acid was added to 5 g of minoxidil, 10 g of 1,3-butylene glycol, and 60 g of ethanol, and the total amount was adjusted to 100 mL with purified water, and dissolved by stirring to obtain a lotion type liquid. The pH of the solution was 6.2.
(試験例1:光安定性試験)
実施例1〜6及び比較例1〜6の試験液を白色蛍光灯光源下で3000Lux×30日間曝光させた。これらの試験液を目視で観察し、色調及び沈殿の有無を確認した。結果を表1に示す。
(Test Example 1: Light stability test)
The test solutions of Examples 1 to 6 and Comparative Examples 1 to 6 were exposed to 3000 Lux × 30 days under a white fluorescent light source. These test solutions were visually observed to confirm the color tone and the presence or absence of precipitation. The results are shown in Table 1.
(試験例2:熱安定性試験)
実施例1〜6及び比較例1〜6の試験液を65℃(相対湿度成り行き)で14日間保管した。これらの試験液を目視で観察し、色調を確認した。結果を表2に示す。
(Test Example 2: Thermal stability test)
The test solutions of Examples 1-6 and Comparative Examples 1-6 were stored at 65 ° C. (relative humidity) for 14 days. These test solutions were visually observed to confirm the color tone. The results are shown in Table 2.
試験例1及び2の結果より、色調の変化がなかったものを○、変化したものを×、沈殿が発生しなかったものを○、沈殿が発生したものを×とした。さらに総合評価として、光及び熱いずれの条件にも安定であったものを○、いずれかの条件に安定でなかったものを×とした。結果を表3に示す。 From the results of Test Examples 1 and 2, the case in which there was no change in color tone was indicated as ◯, the change in color was indicated as ×, the case where precipitation did not occur was indicated as ◯, and the case where precipitation occurred was indicated as x. Further, as a comprehensive evaluation, a sample that was stable under both light and heat conditions was rated as ○, and a sample that was not stable under either condition was marked as ×. The results are shown in Table 3.
(実施例7)
ミノキシジル10g、エタノール60gに乳酸適量を添加し、精製水で全量を100mLとし、撹拌溶解してミノキシジル溶液を調製した。このミノキシジル溶液50mLに1w/v%黄色4号(アゾ系)液を50μL添加し、撹拌溶解してローションタイプの液剤を得た。液剤のpHは5.4であった。
(Example 7)
A suitable amount of lactic acid was added to 10 g of minoxidil and 60 g of ethanol, and the total amount was adjusted to 100 mL with purified water, and dissolved by stirring to prepare a minoxidil solution. 50 μL of 1 w / v% yellow No. 4 (azo) liquid was added to 50 mL of this minoxidil solution, and dissolved by stirring to obtain a lotion type liquid. The pH of the solution was 5.4.
(実施例8)
ミノキシジル10g、エタノール60gに乳酸適量を添加し、精製水で全量を100mLとし、撹拌溶解してミノキシジル溶液を調製した。このミノキシジル溶液50mLに1w/v%黄色203号(キノリン系)液を50μL添加し、撹拌溶解してローションタイプの液剤を得た。液剤のpHは5.4であった。
(Example 8)
A suitable amount of lactic acid was added to 10 g of minoxidil and 60 g of ethanol, and the total amount was adjusted to 100 mL with purified water, and dissolved by stirring to prepare a minoxidil solution. 50 μL of 1 w / v% yellow No. 203 (quinoline) solution was added to 50 mL of this minoxidil solution, and dissolved by stirring to obtain a lotion type solution. The pH of the solution was 5.4.
(比較例7)
ミノキシジル10g、エタノール60gに乳酸適量を添加し、精製水で全量を100mLとし、撹拌溶解してミノキシジル溶液を調製した。このミノキシジル溶液50mLに1w/v%赤色3号(キサンテン系)液を50μL添加し、撹拌溶解してローションタイプの液剤を得た。液剤のpHは5.4であった。
(Comparative Example 7)
A suitable amount of lactic acid was added to 10 g of minoxidil and 60 g of ethanol, and the total amount was adjusted to 100 mL with purified water, and dissolved by stirring to prepare a minoxidil solution. 50 μL of 1 w / v% Red No. 3 (xanthene) solution was added to 50 mL of this minoxidil solution, and dissolved by stirring to obtain a lotion type liquid. The pH of the solution was 5.4.
(比較例8)
ミノキシジル10g、エタノール60gに乳酸適量を添加し、精製水で全量を100mLとし、撹拌溶解してミノキシジル溶液を調製した。このミノキシジル溶液50mLに1w/v%青色1号(トリフェニルメタン系)液を50μL添加し、撹拌溶解してローションタイプの液剤を得た。液剤のpHは5.4であった。
(Comparative Example 8)
A suitable amount of lactic acid was added to 10 g of minoxidil and 60 g of ethanol, and the total amount was adjusted to 100 mL with purified water, and dissolved by stirring to prepare a minoxidil solution. 50 μL of 1 w / v% Blue No. 1 (triphenylmethane) solution was added to 50 mL of this minoxidil solution, and dissolved by stirring to obtain a lotion type liquid. The pH of the solution was 5.4.
(比較例9)
ミノキシジル10g、エタノール60gに乳酸適量を添加し、精製水で全量を100mLとし、撹拌溶解してローションタイプの液剤を得た。液剤のpHは5.4であった。
(Comparative Example 9)
An appropriate amount of lactic acid was added to 10 g of minoxidil and 60 g of ethanol, and the total amount was adjusted to 100 mL with purified water, and dissolved by stirring to obtain a lotion type liquid. The pH of the solution was 5.4.
(試験例3:光安定性試験)
実施例7〜8及び比較例7〜9の試験液を白色蛍光灯光源下で3000Lux×30日間曝光させた。これらの試験液を目視で観察し、色調及び沈殿の有無を確認した。結果を表4に示す。
(Test Example 3: Light stability test)
The test solutions of Examples 7 to 8 and Comparative Examples 7 to 9 were exposed to 3000 Lux × 30 days under a white fluorescent light source. These test solutions were visually observed to confirm the color tone and the presence or absence of precipitation. The results are shown in Table 4.
(試験例4:熱安定性試験)
実施例7〜8及び比較例7〜9の試験液を65℃(相対湿度成り行き)で7日間保管した。これらの試験液を目視で観察し、色調を確認した。結果を表5に示す。
(Test Example 4: Thermal stability test)
The test solutions of Examples 7-8 and Comparative Examples 7-9 were stored at 65 ° C. (relative humidity) for 7 days. These test solutions were visually observed to confirm the color tone. The results are shown in Table 5.
試験例3及び4の結果より、色調の変化がなかったものを○、変化したものを×、沈殿が発生しなかったものを○、沈殿が発生したものを×とした。さらに総合評価として、光及び熱いずれの条件にも安定であったものを○、いずれかの条件に安定でなかったものを×とした。結果を表6に示す。 From the results of Test Examples 3 and 4, the case where there was no change in color tone was indicated as ◯, the case where the color tone was changed as x, the case where no precipitation occurred as ○, and the case where precipitation occurred as x. Further, as a comprehensive evaluation, a sample that was stable under both light and heat conditions was rated as ○, and a sample that was not stable under either condition was marked as ×. The results are shown in Table 6.
(実施例9)
ミノキシジル8g、エタノール50gに乳酸適量を添加し、精製水で全量を100mLとし、撹拌溶解してミノキシジル溶液を調製した。このミノキシジル溶液50mLに1w/v%黄色4号(アゾ系)液を50μL添加し、撹拌溶解してローションタイプの液剤を得た。液剤のpHは4.9であった。
Example 9
A suitable amount of lactic acid was added to 8 g of minoxidil and 50 g of ethanol, and the total amount was adjusted to 100 mL with purified water, and dissolved by stirring to prepare a minoxidil solution. 50 μL of 1 w / v% yellow No. 4 (azo) liquid was added to 50 mL of this minoxidil solution, and dissolved by stirring to obtain a lotion type liquid. The pH of the solution was 4.9.
(実施例10)
ミノキシジル8g、エタノール50gに乳酸適量を添加し、精製水で全量を100mLとし、撹拌溶解してミノキシジル溶液を調製した。このミノキシジル溶液50mLに1w/v%黄色203号(キノリン系)液を50μL添加し、撹拌溶解してローションタイプの液剤を得た。液剤のpHは4.9であった。
(Example 10)
A suitable amount of lactic acid was added to 8 g of minoxidil and 50 g of ethanol, and the total amount was adjusted to 100 mL with purified water, and dissolved by stirring to prepare a minoxidil solution. 50 μL of 1 w / v% yellow No. 203 (quinoline) solution was added to 50 mL of this minoxidil solution, and dissolved by stirring to obtain a lotion type solution. The pH of the solution was 4.9.
(比較例10)
ミノキシジル8g、エタノール50gに乳酸適量を添加し、精製水で全量を100mLとし、撹拌溶解してミノキシジル溶液を調製した。このミノキシジル溶液50mLに1w/v%赤色3号(キサンテン系)液を50μL添加し、撹拌溶解してローションタイプの液剤を得た。液剤のpHは4.9であった。
(Comparative Example 10)
A suitable amount of lactic acid was added to 8 g of minoxidil and 50 g of ethanol, and the total amount was adjusted to 100 mL with purified water, and dissolved by stirring to prepare a minoxidil solution. 50 μL of 1 w / v% Red No. 3 (xanthene) solution was added to 50 mL of this minoxidil solution, and dissolved by stirring to obtain a lotion type liquid. The pH of the solution was 4.9.
(比較例11)
ミノキシジル8g、エタノール50gに乳酸適量を添加し、精製水で全量を100mLとし、撹拌溶解してミノキシジル溶液を調製した。このミノキシジル溶液50mLに1w/v%青色1号(トリフェニルメタン系)液を50μL添加し、撹拌溶解してローションタイプの液剤を得た。液剤のpHは4.9であった。
(Comparative Example 11)
A suitable amount of lactic acid was added to 8 g of minoxidil and 50 g of ethanol, and the total amount was adjusted to 100 mL with purified water, and dissolved by stirring to prepare a minoxidil solution. 50 μL of 1 w / v% Blue No. 1 (triphenylmethane) solution was added to 50 mL of this minoxidil solution, and dissolved by stirring to obtain a lotion type liquid. The pH of the solution was 4.9.
(比較例12)
ミノキシジル8g、エタノール50gに乳酸適量を添加し、精製水で全量を100mLとし、撹拌溶解してローションタイプの液剤を得た。液剤のpHは4.9であった。
(Comparative Example 12)
An appropriate amount of lactic acid was added to 8 g of minoxidil and 50 g of ethanol, and the total amount was adjusted to 100 mL with purified water, and dissolved by stirring to obtain a lotion type liquid. The pH of the solution was 4.9.
(試験例5:光安定性試験)
実施例9〜10及び比較例10〜12の試験液を白色蛍光灯光源下で3000Lux×30日間曝光させた。これらの試験液を目視で観察し、色調及び沈殿の有無を確認した。結果を表7に示す。
(Test Example 5: Light stability test)
The test solutions of Examples 9 to 10 and Comparative Examples 10 to 12 were exposed to 3000 Lux × 30 days under a white fluorescent light source. These test solutions were visually observed to confirm the color tone and the presence or absence of precipitation. The results are shown in Table 7.
(試験例6:熱安定性試験)
実施例9〜10及び比較例10〜12の試験液を65℃(相対湿度成り行き)で7日間保管した。これらの試験液を目視で観察し、色調を確認した。結果を表8に示す。
(Test Example 6: Thermal stability test)
The test solutions of Examples 9 to 10 and Comparative Examples 10 to 12 were stored at 65 ° C. (relative humidity) for 7 days. These test solutions were visually observed to confirm the color tone. The results are shown in Table 8.
試験例5及び6の結果より、色調の変化がなかったものを○、変化したものを×、沈殿が発生しなかったものを○、沈殿が発生したものを×とした。さらに総合評価として、光及び熱いずれの条件にも安定であったものを○、いずれかの条件に安定でなかったものを×とした。結果を表9に示す。 From the results of Test Examples 5 and 6, the case where there was no change in color tone was indicated as ◯, the case where the color tone was changed as x, the case where no precipitation occurred as ○, and the case where precipitation occurred as x. Further, as a comprehensive evaluation, a sample that was stable under both light and heat conditions was rated as ○, and a sample that was not stable under either condition was marked as ×. The results are shown in Table 9.
(実施例11)
ミノキシジル5g、プロピレングリコール10g、エタノール60gを精製水で全量を100mLとし、撹拌溶解してミノキシジル溶液を調製した。このミノキシジル溶液50mLに1w/v%黄色4号(アゾ系)液を25μL添加し、撹拌溶解してローションタイプの液剤を得た。液剤のpHは9.1であった。
(Example 11)
Minoxidil 5 g, propylene glycol 10 g, and ethanol 60 g were made up to 100 mL with purified water and dissolved by stirring to prepare a minoxidil solution. To 50 mL of this minoxidil solution, 25 μL of 1 w / v% Yellow No. 4 (azo) liquid was added and dissolved by stirring to obtain a lotion type liquid. The pH of the solution was 9.1.
(実施例12)
ミノキシジル5g、プロピレングリコール10g、エタノール60gを精製水で全量を100mLとし、撹拌溶解してミノキシジル溶液を調製した。このミノキシジル溶液50mLに1w/v%黄色203号(キノリン系)液を25μL添加し、撹拌溶解してローションタイプの液剤を得た。液剤のpHは8.8であった。
(Example 12)
Minoxidil 5 g, propylene glycol 10 g, and ethanol 60 g were made up to 100 mL with purified water and dissolved by stirring to prepare a minoxidil solution. To 50 mL of this minoxidil solution, 25 μL of 1 w / v% yellow No. 203 (quinoline) solution was added and dissolved by stirring to obtain a lotion type solution. The pH of the solution was 8.8.
(実施例13)
ミノキシジル5g、プロピレングリコール20g、エタノール50gを精製水で全量を100mLとし、撹拌溶解してミノキシジル溶液を調製した。このミノキシジル溶液50mLに1w/v%黄色4号(アゾ系)液を25μL添加し、撹拌溶解してローションタイプの液剤を得た。液剤のpHは8.8であった。
(Example 13)
Minoxidil 5 g, propylene glycol 20 g, and ethanol 50 g were made up to 100 mL with purified water and dissolved by stirring to prepare a minoxidil solution. To 50 mL of this minoxidil solution, 25 μL of 1 w / v% Yellow No. 4 (azo) liquid was added and dissolved by stirring to obtain a lotion type liquid. The pH of the solution was 8.8.
(実施例14)
ミノキシジル5g、プロピレングリコール20g、エタノール50gを精製水で全量を100mLとし、撹拌溶解してミノキシジル溶液を調製した。このミノキシジル溶液50mLに1w/v%黄色203号(キノリン系)液を25μL添加し、撹拌溶解してローションタイプの液剤を得た。液剤のpHは8.9であった。
(Example 14)
Minoxidil 5 g, propylene glycol 20 g, and ethanol 50 g were made up to 100 mL with purified water and dissolved by stirring to prepare a minoxidil solution. To 50 mL of this minoxidil solution, 25 μL of 1 w / v% yellow No. 203 (quinoline) solution was added and dissolved by stirring to obtain a lotion type solution. The pH of the solution was 8.9.
(比較例13)
ミノキシジル5g、プロピレングリコール10g、エタノール60gを精製水で全量を100mLとし、撹拌溶解してミノキシジル溶液を調製した。このミノキシジル溶液50mLに1w/v%赤色3号(キサンテン系)液を25μL添加し、撹拌溶解してローションタイプの液剤を得た。液剤のpHは8.9であった。
(Comparative Example 13)
Minoxidil 5 g, propylene glycol 10 g, and ethanol 60 g were made up to 100 mL with purified water and dissolved by stirring to prepare a minoxidil solution. 25 μL of 1 w / v% Red No. 3 (xanthene) solution was added to 50 mL of this minoxidil solution, and dissolved by stirring to obtain a lotion type liquid. The pH of the solution was 8.9.
(比較例14)
ミノキシジル5g、プロピレングリコール10g、エタノール60gを精製水で全量を100mLとし、撹拌溶解してミノキシジル溶液を調製した。このミノキシジル溶液50mLに1w/v%青色1号(トリフェニルメタン系)液を25μL添加し、撹拌溶解してローションタイプの液剤を得た。液剤のpHは8.9であった。
(Comparative Example 14)
Minoxidil 5 g, propylene glycol 10 g, and ethanol 60 g were made up to 100 mL with purified water and dissolved by stirring to prepare a minoxidil solution. To 50 mL of this minoxidil solution, 25 μL of 1 w / v% Blue No. 1 (triphenylmethane) solution was added and dissolved by stirring to obtain a lotion type solution. The pH of the solution was 8.9.
(比較例15)
ミノキシジル5g、プロピレングリコール10g、エタノール60gを精製水で全量を100mLとし、撹拌溶解してローションタイプの液剤を得た。液剤のpHは9.3であった。
(Comparative Example 15)
Minoxidil 5 g, propylene glycol 10 g, and ethanol 60 g were made up to 100 mL with purified water and dissolved with stirring to obtain a lotion type liquid. The pH of the solution was 9.3.
(比較例16)
ミノキシジル5g、プロピレングリコール20g、エタノール50gを精製水で全量を100mLとし、撹拌溶解してミノキシジル溶液を調製した。このミノキシジル溶液50mLに1w/v%赤色3号(キサンテン系)液を25μL添加し、撹拌溶解してローションタイプの液剤を得た。液剤のpHは8.8であった。
(Comparative Example 16)
Minoxidil 5 g, propylene glycol 20 g, and ethanol 50 g were made up to 100 mL with purified water and dissolved by stirring to prepare a minoxidil solution. 25 μL of 1 w / v% Red No. 3 (xanthene) solution was added to 50 mL of this minoxidil solution, and dissolved by stirring to obtain a lotion type liquid. The pH of the solution was 8.8.
(比較例17)
ミノキシジル5g、プロピレングリコール20g、エタノール50gを精製水で全量を100mLとし、撹拌溶解してミノキシジル溶液を調製した。このミノキシジル溶液50mLに1w/v%青色1号(トリフェニルメタン系)液を25μL添加し、撹拌溶解してローションタイプの液剤を得た。液剤のpHは8.9であった。
(Comparative Example 17)
Minoxidil 5 g, propylene glycol 20 g, and ethanol 50 g were made up to 100 mL with purified water and dissolved by stirring to prepare a minoxidil solution. To 50 mL of this minoxidil solution, 25 μL of 1 w / v% Blue No. 1 (triphenylmethane) solution was added and dissolved by stirring to obtain a lotion type solution. The pH of the solution was 8.9.
(比較例18)
ミノキシジル5g、プロピレングリコール20g、エタノール50gを精製水で全量を100mLとし、撹拌溶解してローションタイプの液剤を得た。液剤のpHは8.9であった。
(Comparative Example 18)
Minoxidil 5 g, propylene glycol 20 g, and ethanol 50 g were made up to 100 mL with purified water and dissolved by stirring to obtain a lotion type liquid. The pH of the solution was 8.9.
(試験例7:光安定性試験)
実施例11〜14及び比較例13〜18の試験液を白色蛍光灯光源下で3000Lux×30日間曝光させた。これらの試験液を目視で観察し、色調及び沈殿の有無を確認した。結果を表10に示す。
(Test Example 7: Light stability test)
The test solutions of Examples 11 to 14 and Comparative Examples 13 to 18 were exposed to 3000 Lux × 30 days under a white fluorescent light source. These test solutions were visually observed to confirm the color tone and the presence or absence of precipitation. The results are shown in Table 10.
(試験例8:熱安定性試験)
実施例11〜14及び比較例13〜18の試験液を65℃(相対湿度成り行き)で14日間保管した。これらの試験液を目視で観察し、色調を確認した。結果を表11に示す。
(Test Example 8: Thermal stability test)
The test solutions of Examples 11 to 14 and Comparative Examples 13 to 18 were stored at 65 ° C. (relative humidity) for 14 days. These test solutions were visually observed to confirm the color tone. The results are shown in Table 11.
試験例7及び8の結果より、色調の変化がなかったものを○、変化したものを×、沈殿が発生しなかったものを○、沈殿が発生したものを×とした。さらに総合評価として、光及び熱いずれの条件にも安定であったものを○、いずれかの条件に安定でなかったものを×とした。結果を表12に示す。 From the results of Test Examples 7 and 8, the case in which there was no change in color tone was indicated as ◯, the change was indicated as x, the case where precipitation did not occur was indicated as ◯, and the case where precipitation occurred was indicated as x. Further, as a comprehensive evaluation, a sample that was stable under both light and heat conditions was rated as ○, and a sample that was not stable under either condition was marked as ×. The results are shown in Table 12.
(実施例15)
ミノキシジル5g、1,3−ブチレングリコール10g、エタノール60gにリン酸適量を添加し、精製水で全量を100mLとし、撹拌溶解してミノキシジル溶液を調製した。このミノキシジル溶液50mLに1w/v%橙色205号(アゾ系)液を50μL添加し、撹拌溶解してローションタイプの液剤を得た。液剤のpHは6.1、可視光域における極大波長は486nmであった。
(Example 15)
An appropriate amount of phosphoric acid was added to 5 g of minoxidil, 10 g of 1,3-butylene glycol and 60 g of ethanol, and the total amount was adjusted to 100 mL with purified water, and dissolved by stirring to prepare a minoxidil solution. 50 μL of 1 w / v% orange No. 205 (azo) liquid was added to 50 mL of this minoxidil solution, and dissolved by stirring to obtain a lotion type liquid. The pH of the solution was 6.1, and the maximum wavelength in the visible light region was 486 nm.
(実施例16)
ミノキシジル5g、1,3−ブチレングリコール10g、エタノール60gにリン酸適量を添加し、精製水で全量を100mLとし、撹拌溶解してミノキシジル溶液を調製した。このミノキシジル溶液50mLに1w/v%橙色402号(アゾ系)液を50μL添加し、撹拌溶解してローションタイプの液剤を得た。液剤のpHは6.1、可視光域における極大波長は475nmであった。
(Example 16)
An appropriate amount of phosphoric acid was added to 5 g of minoxidil, 10 g of 1,3-butylene glycol and 60 g of ethanol, and the total amount was adjusted to 100 mL with purified water, and dissolved by stirring to prepare a minoxidil solution. To 50 mL of this minoxidil solution, 50 μL of 1 w / v% orange No. 402 (azo) liquid was added, dissolved by stirring to obtain a lotion type liquid. The pH of the solution was 6.1, and the maximum wavelength in the visible light region was 475 nm.
(実施例17)
ミノキシジル5g、1,3−ブチレングリコール10g、エタノール60gにリン酸適量を添加し、精製水で全量を100mLとし、撹拌溶解してミノキシジル溶液を調製した。このミノキシジル溶液50mLに1w/v%黄色407号(アゾ系)液を50μL添加し、撹拌溶解してローションタイプの液剤を得た。液剤のpHは6.1、可視光域における極大波長は395nmであった。
(Example 17)
An appropriate amount of phosphoric acid was added to 5 g of minoxidil, 10 g of 1,3-butylene glycol and 60 g of ethanol, and the total amount was adjusted to 100 mL with purified water, and dissolved by stirring to prepare a minoxidil solution. 50 μL of 1 w / v% yellow 407 (azo) liquid was added to 50 mL of this minoxidil solution, and dissolved by stirring to obtain a lotion type liquid. The pH of the solution was 6.1, and the maximum wavelength in the visible light region was 395 nm.
(試験例9:光安定性試験)
実施例15〜17の試験液を白色蛍光灯光源下で3000Lux×30日間曝光させた。これらの試験液を目視で観察し、色調及び沈殿の有無を確認した。結果を表13に示す。
(Test Example 9: Light stability test)
The test solutions of Examples 15 to 17 were exposed to 3000 Lux × 30 days under a white fluorescent light source. These test solutions were visually observed to confirm the color tone and the presence or absence of precipitation. The results are shown in Table 13.
(試験例10:熱安定性試験)
実施例15〜17の試験液を65℃(相対湿度成り行き)で14日間保管した。これらの試験液を目視で観察し、色調を確認した。結果を表14に示す。
(Test Example 10: Thermal stability test)
The test solutions of Examples 15 to 17 were stored at 65 ° C. (relative humidity) for 14 days. These test solutions were visually observed to confirm the color tone. The results are shown in Table 14.
試験例9及び10の結果より、色調の変化がなかったものを○、変化したものを×、沈殿が発生しなかったものを○、沈殿が発生したものを×とした。さらに総合評価として、光及び熱いずれの条件にも安定であったものを○、いずれかの条件に安定でなかったものを×とした。結果を表15に示す。 From the results of Test Examples 9 and 10, the case in which there was no change in color tone was indicated as ◯, the change in color was indicated as x, the case where precipitation did not occur was indicated as ◯, and the case where precipitation occurred was indicated as x. Further, as a comprehensive evaluation, a sample that was stable under both light and heat conditions was rated as ○, and a sample that was not stable under either condition was marked as ×. The results are shown in Table 15.
本発明により、ミノキシジルと色素が反応して沈殿を生じることなく、且つ経時的な色変化及び沈殿の発生が無い、品質が良好なミノキシジル含有液剤を提供することが可能となった。 According to the present invention, it is possible to provide a minoxidil-containing liquid agent having good quality without causing precipitation due to reaction of minoxidil and a dye, and without causing color change and precipitation over time.
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KR20180123997A (en) | 2018-10-31 | 2018-11-20 | 김현수 | Composition for external use for hair growth and hair growth |
CN109557212A (en) * | 2018-12-21 | 2019-04-02 | 康美药业股份有限公司 | A kind of detection method of Chinese medicine red colour system coloring agent |
JP2022540062A (en) * | 2019-06-28 | 2022-09-14 | 深▲せん▼市三啓薬物開発有限公司 | Hydrazoneamide derivatives and their application in the preparation of drugs for preventing and treating hair loss |
CN116919892A (en) * | 2023-08-03 | 2023-10-24 | 济南中海医药科技有限公司 | Preparation method of minoxidil external solution |
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KR20180123997A (en) | 2018-10-31 | 2018-11-20 | 김현수 | Composition for external use for hair growth and hair growth |
CN109557212A (en) * | 2018-12-21 | 2019-04-02 | 康美药业股份有限公司 | A kind of detection method of Chinese medicine red colour system coloring agent |
JP2022540062A (en) * | 2019-06-28 | 2022-09-14 | 深▲せん▼市三啓薬物開発有限公司 | Hydrazoneamide derivatives and their application in the preparation of drugs for preventing and treating hair loss |
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