JP6233999B1 - 育毛剤 - Google Patents
育毛剤 Download PDFInfo
- Publication number
- JP6233999B1 JP6233999B1 JP2017000752A JP2017000752A JP6233999B1 JP 6233999 B1 JP6233999 B1 JP 6233999B1 JP 2017000752 A JP2017000752 A JP 2017000752A JP 2017000752 A JP2017000752 A JP 2017000752A JP 6233999 B1 JP6233999 B1 JP 6233999B1
- Authority
- JP
- Japan
- Prior art keywords
- hair
- fulvic acid
- humus
- acid
- hair restorer
- Prior art date
- Legal status (The legal status is an assumption and is not a legal conclusion. Google has not performed a legal analysis and makes no representation as to the accuracy of the status listed.)
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- 210000004209 hair Anatomy 0.000 title claims abstract description 71
- 239000002509 fulvic acid Substances 0.000 claims abstract description 57
- 239000003864 humus Substances 0.000 claims abstract description 56
- PUKLDDOGISCFCP-JSQCKWNTSA-N 21-Deoxycortisone Chemical compound C1CC2=CC(=O)CC[C@]2(C)[C@@H]2[C@@H]1[C@@H]1CC[C@@](C(=O)C)(O)[C@@]1(C)CC2=O PUKLDDOGISCFCP-JSQCKWNTSA-N 0.000 claims abstract description 54
- FCYKAQOGGFGCMD-UHFFFAOYSA-N Fulvic acid Natural products O1C2=CC(O)=C(O)C(C(O)=O)=C2C(=O)C2=C1CC(C)(O)OC2 FCYKAQOGGFGCMD-UHFFFAOYSA-N 0.000 claims abstract description 54
- 229940095100 fulvic acid Drugs 0.000 claims abstract description 54
- 239000000284 extract Substances 0.000 claims abstract description 49
- 238000010521 absorption reaction Methods 0.000 claims abstract description 16
- 238000000034 method Methods 0.000 claims abstract description 15
- 238000000862 absorption spectrum Methods 0.000 claims abstract description 12
- 238000005033 Fourier transform infrared spectroscopy Methods 0.000 claims abstract description 9
- 239000000654 additive Substances 0.000 claims abstract description 4
- 235000013373 food additive Nutrition 0.000 claims abstract description 4
- 239000002778 food additive Substances 0.000 claims abstract description 4
- 239000003795 chemical substances by application Substances 0.000 claims description 22
- 239000000839 emulsion Substances 0.000 claims description 12
- 239000000243 solution Substances 0.000 claims description 12
- XLYOFNOQVPJJNP-UHFFFAOYSA-N water Substances O XLYOFNOQVPJJNP-UHFFFAOYSA-N 0.000 claims description 11
- 239000000843 powder Substances 0.000 claims description 8
- 239000006071 cream Substances 0.000 claims description 4
- 239000002775 capsule Substances 0.000 claims description 3
- 239000007910 chewable tablet Substances 0.000 claims description 3
- 239000004927 clay Substances 0.000 claims description 3
- 239000006196 drop Substances 0.000 claims description 3
- 239000008187 granular material Substances 0.000 claims description 3
- 239000006187 pill Substances 0.000 claims description 3
- 239000006188 syrup Substances 0.000 claims description 3
- 235000020357 syrup Nutrition 0.000 claims description 3
- 239000003826 tablet Substances 0.000 claims description 3
- 125000001624 naphthyl group Chemical group 0.000 claims description 2
- 230000000996 additive effect Effects 0.000 claims 1
- 229940068682 chewable tablet Drugs 0.000 claims 1
- 229940023488 pill Drugs 0.000 claims 1
- 230000003779 hair growth Effects 0.000 abstract description 24
- 230000000694 effects Effects 0.000 abstract description 13
- 239000002537 cosmetic Substances 0.000 abstract description 2
- 210000004027 cell Anatomy 0.000 description 28
- 230000000052 comparative effect Effects 0.000 description 25
- 238000012360 testing method Methods 0.000 description 15
- 239000000047 product Substances 0.000 description 14
- 125000003178 carboxy group Chemical group [H]OC(*)=O 0.000 description 11
- -1 tri-substituted benzene Chemical class 0.000 description 11
- QJZYHAIUNVAGQP-UHFFFAOYSA-N 3-nitrobicyclo[2.2.1]hept-5-ene-2,3-dicarboxylic acid Chemical compound C1C2C=CC1C(C(=O)O)C2(C(O)=O)[N+]([O-])=O QJZYHAIUNVAGQP-UHFFFAOYSA-N 0.000 description 10
- 230000010261 cell growth Effects 0.000 description 10
- 239000004021 humic acid Substances 0.000 description 10
- 239000007788 liquid Substances 0.000 description 10
- 230000002500 effect on skin Effects 0.000 description 9
- 239000002689 soil Substances 0.000 description 9
- 239000002253 acid Substances 0.000 description 8
- 230000009471 action Effects 0.000 description 8
- 230000004663 cell proliferation Effects 0.000 description 8
- 229960004039 finasteride Drugs 0.000 description 8
- DBEPLOCGEIEOCV-WSBQPABSSA-N finasteride Chemical compound N([C@@H]1CC2)C(=O)C=C[C@]1(C)[C@@H]1[C@@H]2[C@@H]2CC[C@H](C(=O)NC(C)(C)C)[C@@]2(C)CC1 DBEPLOCGEIEOCV-WSBQPABSSA-N 0.000 description 8
- 239000000126 substance Substances 0.000 description 8
- 239000007864 aqueous solution Substances 0.000 description 6
- 239000002609 medium Substances 0.000 description 6
- OKTJSMMVPCPJKN-UHFFFAOYSA-N Carbon Chemical compound [C] OKTJSMMVPCPJKN-UHFFFAOYSA-N 0.000 description 5
- KFZMGEQAYNKOFK-UHFFFAOYSA-N Isopropanol Chemical compound CC(C)O KFZMGEQAYNKOFK-UHFFFAOYSA-N 0.000 description 5
- 229910052799 carbon Inorganic materials 0.000 description 5
- 238000002189 fluorescence spectrum Methods 0.000 description 5
- 239000005416 organic matter Substances 0.000 description 5
- 239000013641 positive control Substances 0.000 description 5
- 230000035755 proliferation Effects 0.000 description 5
- ALYNCZNDIQEVRV-UHFFFAOYSA-N 4-aminobenzoic acid Chemical compound NC1=CC=C(C(O)=O)C=C1 ALYNCZNDIQEVRV-UHFFFAOYSA-N 0.000 description 4
- 241000196324 Embryophyta Species 0.000 description 4
- LFQSCWFLJHTTHZ-UHFFFAOYSA-N Ethanol Chemical compound CCO LFQSCWFLJHTTHZ-UHFFFAOYSA-N 0.000 description 4
- 238000004458 analytical method Methods 0.000 description 4
- 150000007524 organic acids Chemical class 0.000 description 4
- 150000003839 salts Chemical class 0.000 description 4
- LYCAIKOWRPUZTN-UHFFFAOYSA-N Ethylene glycol Chemical compound OCCO LYCAIKOWRPUZTN-UHFFFAOYSA-N 0.000 description 3
- 238000000134 MTT assay Methods 0.000 description 3
- 231100000002 MTT assay Toxicity 0.000 description 3
- OKKJLVBELUTLKV-UHFFFAOYSA-N Methanol Chemical compound OC OKKJLVBELUTLKV-UHFFFAOYSA-N 0.000 description 3
- 239000002202 Polyethylene glycol Substances 0.000 description 3
- DNIAPMSPPWPWGF-UHFFFAOYSA-N Propylene glycol Chemical compound CC(O)CO DNIAPMSPPWPWGF-UHFFFAOYSA-N 0.000 description 3
- HEMHJVSKTPXQMS-UHFFFAOYSA-M Sodium hydroxide Chemical compound [OH-].[Na+] HEMHJVSKTPXQMS-UHFFFAOYSA-M 0.000 description 3
- 239000003513 alkali Substances 0.000 description 3
- 239000006285 cell suspension Substances 0.000 description 3
- 239000003205 fragrance Substances 0.000 description 3
- 238000004519 manufacturing process Methods 0.000 description 3
- 239000000203 mixture Substances 0.000 description 3
- 230000000704 physical effect Effects 0.000 description 3
- 229920001223 polyethylene glycol Polymers 0.000 description 3
- PRAKJMSDJKAYCZ-UHFFFAOYSA-N squalane Chemical compound CC(C)CCCC(C)CCCC(C)CCCCC(C)CCCC(C)CCCC(C)C PRAKJMSDJKAYCZ-UHFFFAOYSA-N 0.000 description 3
- 239000002562 thickening agent Substances 0.000 description 3
- 229930003231 vitamin Natural products 0.000 description 3
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- PUPZLCDOIYMWBV-UHFFFAOYSA-N (+/-)-1,3-Butanediol Chemical compound CC(O)CCO PUPZLCDOIYMWBV-UHFFFAOYSA-N 0.000 description 2
- 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
- XDOFQFKRPWOURC-UHFFFAOYSA-N 16-methylheptadecanoic acid Chemical compound CC(C)CCCCCCCCCCCCCCC(O)=O XDOFQFKRPWOURC-UHFFFAOYSA-N 0.000 description 2
- NVKAWKQGWWIWPM-ABEVXSGRSA-N 17-β-hydroxy-5-α-Androstan-3-one Chemical compound C1C(=O)CC[C@]2(C)[C@H]3CC[C@](C)([C@H](CC4)O)[C@@H]4[C@@H]3CC[C@H]21 NVKAWKQGWWIWPM-ABEVXSGRSA-N 0.000 description 2
- 241000894006 Bacteria Species 0.000 description 2
- QFOHBWFCKVYLES-UHFFFAOYSA-N Butylparaben Chemical compound CCCCOC(=O)C1=CC=C(O)C=C1 QFOHBWFCKVYLES-UHFFFAOYSA-N 0.000 description 2
- FBPFZTCFMRRESA-FSIIMWSLSA-N D-Glucitol Natural products OC[C@H](O)[C@H](O)[C@@H](O)[C@H](O)CO FBPFZTCFMRRESA-FSIIMWSLSA-N 0.000 description 2
- FBPFZTCFMRRESA-JGWLITMVSA-N D-glucitol Chemical compound OC[C@H](O)[C@@H](O)[C@H](O)[C@H](O)CO FBPFZTCFMRRESA-JGWLITMVSA-N 0.000 description 2
- WQZGKKKJIJFFOK-GASJEMHNSA-N Glucose Natural products OC[C@H]1OC(O)[C@H](O)[C@@H](O)[C@@H]1O WQZGKKKJIJFFOK-GASJEMHNSA-N 0.000 description 2
- PEDCQBHIVMGVHV-UHFFFAOYSA-N Glycerine Chemical compound OCC(O)CO PEDCQBHIVMGVHV-UHFFFAOYSA-N 0.000 description 2
- VEXZGXHMUGYJMC-UHFFFAOYSA-N Hydrochloric acid Chemical compound Cl VEXZGXHMUGYJMC-UHFFFAOYSA-N 0.000 description 2
- UQSXHKLRYXJYBZ-UHFFFAOYSA-N Iron oxide Chemical compound [Fe]=O UQSXHKLRYXJYBZ-UHFFFAOYSA-N 0.000 description 2
- LRHPLDYGYMQRHN-UHFFFAOYSA-N N-Butanol Chemical compound CCCCO LRHPLDYGYMQRHN-UHFFFAOYSA-N 0.000 description 2
- ISWSIDIOOBJBQZ-UHFFFAOYSA-N Phenol Chemical compound OC1=CC=CC=C1 ISWSIDIOOBJBQZ-UHFFFAOYSA-N 0.000 description 2
- XLOMVQKBTHCTTD-UHFFFAOYSA-N Zinc monoxide Chemical compound [Zn]=O XLOMVQKBTHCTTD-UHFFFAOYSA-N 0.000 description 2
- 238000002835 absorbance Methods 0.000 description 2
- 150000001298 alcohols Chemical class 0.000 description 2
- 239000003963 antioxidant agent Substances 0.000 description 2
- 235000006708 antioxidants Nutrition 0.000 description 2
- WPYMKLBDIGXBTP-UHFFFAOYSA-N benzoic acid Chemical compound OC(=O)C1=CC=CC=C1 WPYMKLBDIGXBTP-UHFFFAOYSA-N 0.000 description 2
- 239000006143 cell culture medium Substances 0.000 description 2
- HVYWMOMLDIMFJA-DPAQBDIFSA-N cholesterol Chemical compound C1C=C2C[C@@H](O)CC[C@]2(C)[C@@H]2[C@@H]1[C@@H]1CC[C@H]([C@H](C)CCCC(C)C)[C@@]1(C)CC2 HVYWMOMLDIMFJA-DPAQBDIFSA-N 0.000 description 2
- 239000003086 colorant Substances 0.000 description 2
- 238000000354 decomposition reaction Methods 0.000 description 2
- UKMSUNONTOPOIO-UHFFFAOYSA-N docosanoic acid Chemical compound CCCCCCCCCCCCCCCCCCCCCC(O)=O UKMSUNONTOPOIO-UHFFFAOYSA-N 0.000 description 2
- POULHZVOKOAJMA-UHFFFAOYSA-N dodecanoic acid Chemical compound CCCCCCCCCCCC(O)=O POULHZVOKOAJMA-UHFFFAOYSA-N 0.000 description 2
- 235000013399 edible fruits Nutrition 0.000 description 2
- 150000002148 esters Chemical class 0.000 description 2
- 230000005284 excitation Effects 0.000 description 2
- 230000007717 exclusion Effects 0.000 description 2
- 239000008103 glucose Substances 0.000 description 2
- 239000003102 growth factor Substances 0.000 description 2
- 239000003966 growth inhibitor Substances 0.000 description 2
- 239000003676 hair preparation Substances 0.000 description 2
- IPCSVZSSVZVIGE-UHFFFAOYSA-N hexadecanoic acid Chemical compound CCCCCCCCCCCCCCCC(O)=O IPCSVZSSVZVIGE-UHFFFAOYSA-N 0.000 description 2
- 229910052500 inorganic mineral Inorganic materials 0.000 description 2
- ZXEKIIBDNHEJCQ-UHFFFAOYSA-N isobutanol Chemical compound CC(C)CO ZXEKIIBDNHEJCQ-UHFFFAOYSA-N 0.000 description 2
- 230000014759 maintenance of location Effects 0.000 description 2
- VAMXMNNIEUEQDV-UHFFFAOYSA-N methyl anthranilate Chemical compound COC(=O)C1=CC=CC=C1N VAMXMNNIEUEQDV-UHFFFAOYSA-N 0.000 description 2
- LXCFILQKKLGQFO-UHFFFAOYSA-N methylparaben Chemical compound COC(=O)C1=CC=C(O)C=C1 LXCFILQKKLGQFO-UHFFFAOYSA-N 0.000 description 2
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- BDERNNFJNOPAEC-UHFFFAOYSA-N propan-1-ol Chemical compound CCCO BDERNNFJNOPAEC-UHFFFAOYSA-N 0.000 description 2
- 239000012925 reference material Substances 0.000 description 2
- YGSDEFSMJLZEOE-UHFFFAOYSA-N salicylic acid Chemical compound OC(=O)C1=CC=CC=C1O YGSDEFSMJLZEOE-UHFFFAOYSA-N 0.000 description 2
- 238000000926 separation method Methods 0.000 description 2
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- 150000003722 vitamin derivatives Chemical class 0.000 description 2
- HDTRYLNUVZCQOY-UHFFFAOYSA-N α-D-glucopyranosyl-α-D-glucopyranoside Natural products OC1C(O)C(O)C(CO)OC1OC1C(O)C(O)C(O)C(CO)O1 HDTRYLNUVZCQOY-UHFFFAOYSA-N 0.000 description 1
- JSPNNZKWADNWHI-PNANGNLXSA-N (2r)-2-hydroxy-n-[(2s,3r,4e,8e)-3-hydroxy-9-methyl-1-[(2r,3r,4s,5s,6r)-3,4,5-trihydroxy-6-(hydroxymethyl)oxan-2-yl]oxyoctadeca-4,8-dien-2-yl]heptadecanamide Chemical compound CCCCCCCCCCCCCCC[C@@H](O)C(=O)N[C@H]([C@H](O)\C=C\CC\C=C(/C)CCCCCCCCC)CO[C@@H]1O[C@H](CO)[C@@H](O)[C@H](O)[C@H]1O JSPNNZKWADNWHI-PNANGNLXSA-N 0.000 description 1
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- 239000008159 sesame oil Substances 0.000 description 1
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- TUNFSRHWOTWDNC-HKGQFRNVSA-N tetradecanoic acid Chemical compound CCCCCCCCCCCCC[14C](O)=O TUNFSRHWOTWDNC-HKGQFRNVSA-N 0.000 description 1
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- 239000011787 zinc oxide Substances 0.000 description 1
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- FYGDTMLNYKFZSV-BYLHFPJWSA-N β-1,4-galactotrioside Chemical compound O[C@@H]1[C@@H](O)[C@H](O)[C@@H](CO)O[C@H]1O[C@@H]1[C@H](CO)O[C@@H](O[C@@H]2[C@@H](O[C@@H](O)[C@H](O)[C@H]2O)CO)[C@H](O)[C@H]1O FYGDTMLNYKFZSV-BYLHFPJWSA-N 0.000 description 1
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Abstract
Description
ヒューミクルの4%水溶液の3次元励起−蛍光スペクトル(測定装置JASCO FP−8200)を図3に示す。比較のため、愛知県段戸森林土壌から抽出精製されたフルボ酸及びフミン酸(いずれも、日本腐植物質学会から「日本腐植物質学会 標準資料」として頒布されている、以下、それぞれ、段戸産フルボ酸及び段戸産フミン酸という)の3次元蛍光スペクトルを図4に示す。ヒューミクル及び段戸産フルボ酸の3次元励起−蛍光スペクトルには、フルボ酸由来の蛍光の特徴である、励起250nm付近−蛍光430nm付近のピーク及び、励起320nm付近−蛍光430nm付近のピークが出現している。
GPC−UV/TC分析法は、水中溶存有機物を分子の大きさや排除の程度によって高速に分離し、分離した溶存分子をUV検出器及びTC検出器(Total Carbon Analyzer)でモニタリングする手法である。以下GPC−TC装置:
GPC:Shodex GPC SYSTEM 21
分離カラム TOSO HW−50S
溶離液 30mM Na2HPO4
UV吸収(220nm)検出器:GL7450(GL サイエンス製)
TC検出器:LCT−100(東レエンジニアリング製)
を用いて、ヒューミクル及び段戸産フルボ酸の分子量を測定した。
前記フルボ酸分画のATR法(Attenuated Total Reflection、全反射吸収法)にて赤外線吸収スペクトルを取得した。具体的には、前記フルボ酸分画をDax−8樹脂(Spelco社製)に施用し、そこに吸着した有機物をアルカリ性溶液で脱着した。脱着した有機物を、さらにイオン交換樹脂に通して不要な塩類を取り除いた。得られた試料をATR法に基づくFT−IR分光分析(PerkinElmer Spectrum 65)に供した。
本発明の育毛剤が育毛作用を有するか否かを、毛乳頭細胞の実験モデル系である毛乳頭細胞増殖効果試験(in vitro)で調べた。具体的には、毛乳頭細胞へ本発明の育毛剤を添加し、MTTアッセイによって毛乳頭細胞の細胞増殖促進率を測定し、さらに毛乳頭細胞増殖率を算出した。
実施例1として、米国ユタ産の腐植の水性抽出物を乾固した腐植抽出物製品「ヒューミクル」(株式会社スタイルアンドバリュージャパン製)を用意した。ヒューミクルに含まれるフルボ酸分画の物性は、上記したとおりである。
比較例1:果物や植物の発酵により得られたフルボ酸100%のM社製健康飲料
比較例2:長崎県北高来郡森山町唐比西産の腐植抽出物(フルボ酸)を含んだN社製清涼飲料水
比較例3:段戸産フルボ酸(腐植酸標準物質、日本腐植物質学会製)
比較例4:琵琶湖産フルボ酸(腐植酸標準物質、日本腐植物質学会製)
試験用細胞には、ヒト頭髪毛乳頭細胞(タカラバイオ社製)を用いた。培養フラスコ(培養面積75cm2)にヒト頭髪毛乳頭細胞培地及びヒト頭髪毛乳頭細胞懸濁液を培養液中の細胞の最終濃度が2.5×104cells/mL、全量10mLとなるように添加し、CO2インキュベーター(37℃、CO2 5%)で、7日培養して必要細胞数を確保した。
実施例1及び比較例1〜4の育毛剤試験品を、それぞれ、試験品濃度が125、31.25、7.81、1.95、0.48、又は0.12μg/mlとなるように、順次、毛乳頭細胞培地で希釈した。陽性対照のFinasterideは、3ng/mLとなるように希釈した。
4.1 ヒト頭髪毛乳頭細胞の培養
培養したヒト頭髪毛乳頭細胞をTrypsin処理により培養フラスコから回収し、細胞数をカウントした。細胞を毛乳頭細胞培地で懸濁し、細胞濃度が1×104cells/mLの細胞懸濁液を調製した。調製した細胞懸濁液を試験プレート(96well micro plate)に0.2mLずつ、各wellに添加し、室温で20分静置した。CO2インキュベーター(37℃、CO2 5%)にて18時間の前培養した。前培養後、試験プレート各ウェルの培地と調製した試験品溶液を置き換え、さらにCO2インキュベーター(37℃、CO2 5%)にて72時間培養した。72時間後、MTTアッセイによる生存率を確認した。※独立3回にて試験結果を算出した。
培養終了後のプレートの培地を捨て、新たにMTT試薬含有培地(1mgMTT/mL培地)を0.1mLずつ各Wellに添加した。CO2インキュベーター(37℃、CO2 5%)にて3時間培養し、呈色反応を行った。MTT可溶化溶液(イソプロパノール)を0.1mLずつ各wellに添加し、生細胞に取り込まれたMTTを抽出した。マイクロプレートリーダーを使用してMTT抽出液の吸光度を570nmで測定した。下記式に示すように、コントロール(試験品未処理細胞)の吸光度を100とした場合の百分率で細胞増殖率を算出した。
得られたデータについて、分散分析を行い、等分散が確認された場合には統計解析として対応のないt検定を実施し、対照区との比較を実施した。試験結果を表4及び図5に示す。
Claims (7)
- FT−IR法における赤外線吸収スペクトルにおいて波数3362,2875,1675,1559,1360,1200,1047及び835cm−1に赤外線吸収ピークを有し、4,000よりも小さい平均分子量を有するフルボ酸を含有する腐植抽出物を有効量含み、そして化粧品学的、皮膚病学的及び/又は薬学的に許容される添加剤あるいは食品添加物を含んでなる育毛剤。
- 前記腐植抽出物は、図1に示す赤外線吸収スペクトルを示すフルボ酸を含有する、請求項1に記載の育毛剤。
- 前記腐植抽出物は、ナフタレン環構造を有さないことを特徴とする、請求項1又は2に記載の育毛剤。
- 経皮投与用である、請求項1〜3のいずれか一項に記載の育毛剤。
- 水剤、液剤、乳剤、乳液、エマルション、クリーム、粉体、又はクレイパックの形態である、請求項4に記載の育毛剤。
- 経口投与用である、請求項1〜3のいずれか一項に記載の育毛剤。
- 散剤、顆粒剤、カプセル剤、丸剤、錠剤、チュアブル錠、ドロップ、水剤、シロップ、又はドリンク剤の形態である、請求項6に記載の育毛剤。
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WO2007102813A1 (en) * | 2006-03-07 | 2007-09-13 | Advantage Marketing, Inc. | Compositions and methods for human use containing fulvic acid |
JP2013107857A (ja) * | 2011-11-22 | 2013-06-06 | Funao Kurosawa | 皮膚外用剤 |
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JP2006327978A (ja) * | 2005-05-25 | 2006-12-07 | Myubio Co Ltd | 育毛剤 |
WO2007102813A1 (en) * | 2006-03-07 | 2007-09-13 | Advantage Marketing, Inc. | Compositions and methods for human use containing fulvic acid |
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