200911292 九、發明說明： 【發明所屬之技術領域】 本發明涉及含有高濃度抗壞血酸-2-磷酸酯鎂鹽的水包油型 乳化組合物的技術。 【先前技術】 以往的含抗壞血酸-2-磷酸酿鎮鹽的製劑，為了兼顧抗壞血酸 -2-磷酸酯鎂鹽的有效性和製劑的穩定性，抗壞血酸磷酸酯鎂 鹽的調配濃度-般為3質量％ (專利文獻丨：日本特開平22酬 號公報）。近年來’已開發出含有高濃度抗壞血酸I鱗酸醋鎂鹽、 提高有效性、且確保穩定性的化妝料。然而’在化妝水、美容液 中調配高濃度的抗壞血酸-2-磷酸自旨鎂鹽比較容易，但在水包油型 礼化組合物巾娜高濃度的抗壞血酸〜2_磷_旨賴，並滿足穩定 性、使用感是_的。作為技術課題，可關舉出：電解質以疋 的濃度增高後’在乳_近形成的水合層減少（脫水合），從而促 進乳液的凝結；因為電解質的濃度高，因而不能使用增枯效果古 的陰離子触_絲合物；抗壞血H顧賴躲易析出门。 雖然已知麵包水趣恤合物巾触高濃度抗壞血酸1 魏醋鎂鹽的技術（專敝獻2 :日本_細5_132726 專利文獻3 ··日本特開33_號公報），但在水包 組合物中娜高濃度純域—2_磷_旨_賊闕幾 200911292 進行。雖然已知調配20〜95重量％的白色凡士林，以使抗壞血酸 -2-磷酸酯鎂鹽穩定的技術（專利文獻4 :日本特開2〇〇3_55ΐ9ι 號公報）’但因调配鬲濃度的白色凡士林，而存在發粘的問題。 作為水包油型乳化組合物，已知通過調配羥基亞乙基二膦酸 鹽或二乙稀三胺五乙義，調配了灌抗壞血酸H咖旨鎮鹽的 護膚霜（專利文獻5:日本特開平1〇_147512號公報）。但是，經 基亞乙基二膦酸鹽或二乙烯三胺五乙酸鹽是金屬t合劑，是在化 妝品中娜上限受義定的補，從皮膚舰方面來考慮，較不 佳。已知含有擰檬酸鉀、且含有6%的L_抗壞血酸鱗酸酿鎮鹽的乳 膏（專利文獻6 :日本特開聽—侧8號公報），並記載其不產生 1^壞血__旨_的臟。但是，因為作絲祕性劑調配 了 2%十甘油單硬脂_旨、撕油單硬脂酸S旨，合計6%，所以形成 =的乳膏’使用感不好，魏感和刺激性成為問題。此外，已知 含有通三甲基甘氨酸和·抗壞血__旨鎂鹽的乳膏（專利 文獻7 :日本特開齡嶋號公報），但經時穩定性未得到碎 2雖然記載說通過調配三甲基甘氨酸可抑制發贼，但因為作 ，ί·生劑舰了 2% p〇E單硬脂酸自旨、5%自乳化型單硬 用 °相配了 7%的表面活蝴，所鄉成硬的乳膏， ’發枯感和刺激性成為問題。此外，已知含有院基曱 3有5%L'抗壞血酸魏祕鹽的乳化化妝料（專利 •日本網平U—228378號公報），含有雜乙稀加減麻 200911292 鎂烯:成山梨糖醇脂肪酸酯、含有5%L_抗壞血酸磷酸酯 二ί 、專利文獻9:日本特開256173號公報），含有 一成田·、、象脫石含有5%L-抗壞血酸鱗酸酯鎂鹽的乳膏（專 獻1。.日本特開2005〜6〇239號公報)，穩定性得到確認。1文 【專利文獻1】日本特開平3_2279〇7號公報 【專利文獻2】日本特開2005-132726號公報 【專利文獻3】日本特開2004-339106就公報 【專利文獻4】日本特開2__55191號公報 【專利文獻5】日本特開平10-147512號公報 【專利文獻6】日本特開2005-41808號公報 【專利文獻7】日本特開2GG5-6G236號公報 【專利文獻8】曰本特開平11-228378號公報 【專利文獻9】日本特開2000-256173號公報 【專利文獻10】日本特開2〇〇5_6〇239號公報 【發明内容】 磷酸酯鎂鹽的穩定的 本發明提供調配有冑濃度抗壞血 水包油型乳化組合物。 本1明的主要結構是下述結構。 nil) Γ包油型乳化組合物’其特徵在於，含有5〜8質量％的 几展城-2-魏_鹽、抗壞济2，_雜㈣倍量以上 200911292 的水、碳原子數為16〜22的直鏈飽和高級醇、及黃原膠。 $水包油型乳化組合物，其特徵在於，含有卜8質量％的 几展血H魏驗鹽、抗壞血酸_2_磷_旨鎂鹽㈣倍量以上 、火原子數為16〜22的朗飽和高轉、黃轉、及辛烯基 琥珀酸鋁;殿粉。 (3)上述⑴$⑵所述的水包_乳倾合物，其特徵 在於，碳原子數為16〜22的麵飽和高級醇_ 質量％。 /(4)上述⑴〜⑶中任—項所述的水包油型乳化組合物， 其特徵在於，黃原膠的調配量是0. 05〜0· 5質量％。 (5)上述（丨）〜（4)中任一項所述的水包油型乳化組合物， 其特彳政在於，辛烯基琥珀酸鋁澱粉的配合量是〇. 5〜3質量％。 根據特定的組成’能夠提供娜有5〜8 f量％的抗壞血酸—2_ 磷酸酯鎂鹽的水包油型乳化組合物。 本發明提供的水包油型乳化組合物，抗壞血酸_2_碟酸酯鎮鹽 不會被析出，乳化穩定。 本發明提供的水包油型乳化組合物，發粘感得到抑制，硬度 適中’使用感良好。 本發明的水包油型乳化組合物，可作為乳液、乳膏、美容液、 防曬霜、液體粉底等化妝料、皮膚外用劑使用，可作為醫藥部外 品、醫藥品使用。 200911292 【實施方式】 本發明使用的抗壞血酸-2-填酸酯鎂鹽是使對酶、熱不穩定的 L-抗壞血酸進行鱗酸酯化後形成的穩定的抗壞血酸衍生物，可使 用市售品[(昭和電工（株）制抗壞血酸PM、曰本曰光化學工業 (Nihon Surfactant Kogyo Κ· K.)(株）制 NIKKOL VC-PMG 等）]。 本發明使用的抗壞血酸-2-磷酸酯鎂鹽的調配量為5〜8質量％。調 配1低於5質時，抗壞血酸-2-填酸酷鎮鹽的功效與以往的3 質量%調配品沒有太大的改變，超過5質量％後，與以往產品相比， 抗壞血酸-2-磷酸酯鎂鹽的功效發揮顯著。抗壞血酸_2_磷酸酯鎂 鹽的調配量超過8質量％後，難於獲得穩定的水包油型乳化組合 物。 作為本發明使_碳原子數為16〜22的直鏈飽和高級醇，可 以為錄辦（碳原子數16)、硬脂醇（碳原子數18)、花生醇（碳 原子數20)、山蝓醇（碳原子數22)，均可獲得其市f品。碳原子 數為16〜22的直鏈飽和高級醇的調配量，較佳〇. 5〜4質量％。低 於0. 5質量％或超過4質量辦，均難於獲得水包油型乳化組合物 的穩定性。 本發明使㈣黃轉，是糊黃單胞_ (Xanth_as)菌 使碳水化合物發酵，將鐘外蓄積的多糖類精製後得到的天然膠 質了、使用市απσ[(曰清奥利友集團（株）制丽uc〇AT zz、 200911292 香榮興業（株）製KeltrolT等）]。黃原膠的調配量較佳為〇 〇5 質量％以上、0. 5質量°/◦以下。更佳地為0.05〜0.2質量％。低於〇.05 貝星Z時，難於使本發明的水包油型乳化組合物穩定。黃原膠的濃 度越高，穩定性越好，但調配〇. 5質量％以上時，穩定性就不再提 高。相反，超過〇. 5質量％後，製劑的外觀變差，因產生發粘感， 使用困難。 本發明使用的辛烯基琥珀酸鋁澱粉，是使無水辛烯基琥珀酸 和澱粉反應得到的生成物的鋁鹽，一般作為防固結劑、非水溶性 增粘劑使用。辛烯基琥珀酸鋁澱粉可以使用市售品（曰澱化學（株)200911292 IX. Description of the Invention: TECHNICAL FIELD OF THE INVENTION The present invention relates to a technique of an oil-in-water emulsion composition containing a high concentration of magnesium ascorbate-2-phosphate. [Prior Art] In the conventional preparation containing ascorbic acid-2-phosphate salt, in order to balance the effectiveness of the ascorbyl-2-phosphate magnesium salt and the stability of the preparation, the concentration of the ascorbyl phosphate magnesium salt is generally 3 mass. % (Patent Document 丨: Japan Special Kaiping 22 Reward Bulletin). In recent years, a cosmetic material containing a high concentration of ascorbic acid I citrate magnesium salt has been developed to improve the effectiveness and ensure stability. However, it is easier to formulate a high concentration of ascorbic acid-2-phosphate in the lotion or beauty lotion, but in the oil-in-water type ritual composition, the high concentration of ascorbic acid ~2_phosphorus_ Satisfying stability and feeling of use is _. As a technical subject, it can be noted that the electrolyte is reduced in the concentration of strontium, and the hydration layer formed in the vicinity of the milk is reduced (dehydrated), thereby promoting the coagulation of the emulsion; because the concentration of the electrolyte is high, the effect of increasing the aging cannot be used. The anion touch-filament; anti-sickness H is easy to hide. Although it is known that the bread and water funeral towel touches the high concentration of ascorbic acid 1 Wei vinegar magnesium salt technology (Special offer 2: Japan _ fine 5_132726 Patent Document 3 · · Japan Special Open 33_ Bulletin), but in the water bag combination The high-concentration pure domain - 2_phosphorus _ _ thief 阙 several 200911292. It is known that a white petrolatum is blended in an amount of 20 to 95% by weight to stabilize the ascorbyl-2-phosphate magnesium salt (Patent Document 4: Japanese Patent Laid-Open Publication No. 2〇〇3_55ΐ9ι). There is a problem of stickiness. As an oil-in-water emulsion composition, it is known that a skin cream containing ascorbic acid H-salt salt is formulated by blending hydroxyethylidene diphosphonate or diethylenetriamine pentaside (Patent Document 5: Japan Special Kaiping 1〇_147512 bulletin). However, the phenylethylidene diphosphonate or the diethylenetriamine pentaacetate is a metal t-mixer, which is a supplement to the upper limit of the cosmetics, and is not preferable from the viewpoint of the skin ship. A cream containing potassium hexanoate and containing 6% of L_ascorbyl sulphate salt is known (Patent Document 6: JP-A No. 8), and it is described that it does not cause 1? _ _ dirty. However, since the silky secret agent is formulated with 2% of glycerin monostearate, and the oleic acid monostearic acid S is used for a total of 6%, the cream formed = has a bad feeling of use, and is sensitive and irritating. Become a problem. In addition, a cream containing a trimethylglycine and an anti-scurvy-magnesium salt is known (Patent Document 7: Japanese Patent Publication No. 公报), but the stability over time is not broken. The formulation of trimethylglycine can inhibit the thief, but because of the work, ί·sheng agent has 2% p〇E monostearic acid, 5% self-emulsifying type, single hard, matching 7% of the surface, The hard cream of the hometown, 'dryness and irritation become a problem. In addition, it is known that an emulsified cosmetic containing 5% L' ascorbyl sulphate salt in a hospital base (3 (patent • Japanese Net No. U-228378) contains miscellaneous ethylene plus hemp 200911292 magnesium alkene: sorbitol fat The acid ester contains 5% L_ascorbic acid phosphate, and the patent document 9: JP-A-256173, contains a cream of 5% L-ascorbyl magnesium sulphate. Special offer 1. Japanese special open 2005~6〇239 bulletin), the stability was confirmed. [Patent Document 1] Japanese Patent Laid-Open No. Hei. No. 2005-132726 (Patent Document 3) Japanese Patent Laid-Open Publication No. 2004-339106 (Patent Document 4) Japanese Patent Laid-Open No. 2__55191 [Patent Document 5] Japanese Patent Laid-Open Publication No. Hei. No. Hei. No. Hei. No. Hei. No. 2005-41808. JP-A-2000-256173 [Patent Document 10] Japanese Patent Laid-Open Publication No. Hei. No. Hei. No. Hei. An antimony concentration ascorbic oil-in-water emulsion composition. The main structure of the present invention is the following structure. Nil) an oil-in-oil type emulsified composition characterized in that it contains 5 to 8 mass% of several exhibiting city-2-wei_salt, anti-bad metal 2,_hetero (four) times more than 200911292, and the number of carbon atoms is 16 to 22 linear saturated higher alcohols and xanthan gum. The oil-in-water emulsified composition is characterized in that it contains 8% by mass of several blood-extracting salt, ascorbic acid, _2_phosphorus-magnesium salt (four), and a fire atom number of 16 to 22 Saturated high-turning, yellow-turning, and octenyl aluminum succinate; (3) The water-packed milk-deposited product according to the above (1), wherein the surface saturated high alcohol having a carbon number of 16 to 22 is _ mass%. 5%质量质量。 The amount of the xanthan gum is 0. 05~0· 5 mass%. (5) The oil-in-water emulsion composition according to any one of the above (A) to (4), wherein the amount of the octenyl succinate aluminum starch is 〇. 5 to 3 mass% . According to the specific composition, it is possible to provide an oil-in-water emulsion composition in which the amount of ascorbic acid-2-phosphate phosphate is 5 to 8 f%. According to the oil-in-water emulsion composition provided by the present invention, ascorbic acid 2 - disc acid ester salt is not precipitated and is emulsified stably. The oil-in-water emulsion composition provided by the present invention has suppressed stickiness and moderate hardness, and has a good feeling of use. The oil-in-water emulsion composition of the present invention can be used as a cosmetic, an external preparation for skin, such as an emulsion, a cream, a cosmetic liquid, a sunscreen, a liquid foundation, and the like, and can be used as an external product or a pharmaceutical product of the Ministry of Medicine. 200911292 [Embodiment] The ascorbic acid-2-golate magnesium salt used in the present invention is a stable ascorbic acid derivative formed by scalaging an enzyme or heat-labile L-ascorbic acid, and a commercially available product can be used. (Ascorbic acid PM manufactured by Showa Denko Co., Ltd., NIKKOL VC-PMG manufactured by Nihon Surfactant Kogyo K.K.). The amount of the ascorbic acid-2-phosphate magnesium salt used in the present invention is 5 to 8 mass%. When the ratio of 1 is less than 5, the effect of ascorbic acid-2-acidic salt is not much changed from that of the previous 3 mass%. After more than 5% by mass, ascorbic acid-2-phosphate is compared with the previous product. The efficacy of the ester magnesium salt plays a significant role. When the amount of the ascorbic acid-2-phosphate phosphate salt is more than 8% by mass, it is difficult to obtain a stable oil-in-water emulsion composition. As the linear saturated higher alcohol having 16 carbon atoms in the present invention, it can be recorded (carbon number 16), stearyl alcohol (carbon number 18), peanut alcohol (carbon number 20), mountain The decyl alcohol (having 22 carbon atoms) can be obtained from the market. The blending amount of the linear saturated higher alcohol having a carbon number of 16 to 22 is preferably 〇 5 to 4% by mass. When it is less than 0.5% by mass or more than 4%, it is difficult to obtain the stability of the oil-in-water emulsion composition. The invention makes (4) yellow turn, is a natural gum of the Xanth_as strain which ferments the carbohydrate, and refines the polysaccharide accumulated outside the clock, and uses the city απσ [(曰清奥利友集团) ) 丽 〇 〇 2009, 200911292 (Keltrol T, etc.) The amount of the xanthan gum is preferably 5% by mass or more, and 0.5 or less by mass. More preferably, it is 0.05 to 0.2% by mass. When it is lower than 〇.05 Baystar Z, it is difficult to stabilize the oil-in-water emulsion composition of the present invention. The higher the concentration of xanthan gum, the better the stability, but when it is formulated at 5% by mass or more, the stability is no longer improved. On the other hand, when it exceeds 5% by mass, the appearance of the preparation is deteriorated, and it is difficult to use because of the sticky feeling. The aluminum octenyl succinate used in the present invention is an aluminum salt of a product obtained by reacting anhydrous octenyl succinic acid with starch, and is generally used as an anti-consolidation agent or a water-insoluble tackifier. Commercially available products of octenyl succinate aluminum starch (Mindong Chemical Co., Ltd.)
裝的辛細基號始酸紹玉米殿粉ALUMINUM STARCH OCTEMYLSUC CINATE)。辛烯基琥珀酸鋁澱粉的調配量較佳為〇. 5〜3質量％。低 於0. 5貝里％或超過3質置％後，都難於使本發明的水包油型乳化 組合物穩定。 本發明的水包油型乳化組合物的硬度，從穩定性、使用感來 看，較佳為3〜10g重（裝置：（株）壯leotech製FUDOH RHE0 METER ’壓敏軸直徑：10. 0mm、試樣台速度：6cm/min、浸入量： 30刪、負荷200g)。硬度低於3g重時，難於獲得乳化穩定性，超 過l〇g重後，使用感變差。 製備本發明的水包油型乳化組合物時，除抗壞血酸_2_碟酸醋 鎂鹽、純淨水、碳原子數為16〜22的直鏈飽和高級醇、黃原膠' 辛烯基琥珀酸鋁澱粉以外，在不損壞本發明效果的範圍内，還能 10 200911292 夠調配非離子性表祕_、齡子性表面活轉 面活性劑、兩性表面活性劑、油劑、保酬 =性表 氧化劑、線吸收劑、螯合劑、防腐劑、抗 料等。此外，還可以調配生育紛、視黃醇衍生 ^香 物提取液等美容成分。 、縫類、植 本發明的水包油型乳化組合物可作為乳液、乳膏、美…ALUMINUM STARCH OCTEMYLSUC CINATE). 5〜3质量百分比。 The amount of octenyl succinate aluminum starch is preferably 〇. 5~3% by mass. It is difficult to stabilize the oil-in-water emulsion composition of the present invention after being less than 0.5% by weight or more than 3% by mass. The hardness of the oil-in-water emulsion composition of the present invention is preferably from 3 to 10 g in terms of stability and feeling of use (device: FUDOH RHE0 METER manufactured by Zhuang Leotech Co., Ltd.) pressure-sensitive shaft diameter: 10. 0 mm , sample table speed: 6cm / min, immersion: 30 delete, load 200g). When the hardness is less than 3 g, it is difficult to obtain emulsion stability, and after using more than 10 g, the feeling of use is deteriorated. In the preparation of the oil-in-water emulsion composition of the present invention, in addition to ascorbic acid_2_disodium vinegar magnesium salt, purified water, a linear saturated higher alcohol having a carbon number of 16 to 22, and xanthan gum octenyl succinic acid In addition to aluminum starch, it can also be formulated in a range that does not impair the effects of the present invention. 10 200911292 can be formulated with a non-ionic surface secret _, an age-dependent surface active surface active agent, an amphoteric surfactant, an oil agent, a premium = sex table Oxidizing agents, line absorbers, chelating agents, preservatives, anti-materials, and the like. In addition, it is also possible to formulate cosmetic ingredients such as fertility and retinol-derived extracts. , sewing, planting The oil-in-water emulsion composition of the invention can be used as an emulsion, a cream, a beauty...
關霜、紙粉底等化妝料、皮膚外用劑使用，可料醫: 品、醫藥品使用。 ’、 〔試驗例1〕 及辛烯基琥珀酸鋁澱耠的穩常彳卜 根據表1的組成，製備比較例丨〜8的水包油型乳化組合物。 分別將油相和水相加熱到85〇c，充分攪拌後，將油相添加到水相 中，用均質器以6000rpm攪拌5分鐘。然後冷卻到5〇°c，、恭力並 攪拌抗壞血酸-2-磷酸酯鎂鹽溶液。 根據以下標準，對得到的水包油型乳化組合物的經時穩定座 進行評價。 、 〇·不發生分離 x:發生分離 此外’測定製備後第二天的硬度（單位：g重）。測定硬度的 條件如下所示。 裝置：（株）Rheotech製FUDOH RHEO METER、壓敏轴直徑. 11 200911292 10. Omm、試樣台速度：6cm/min、浸入量：30mm、負荷2〇〇g 表1 比較例 1 比較·(歹！ 2 比較伤 3 比較例 4 比較伤1, 5 比較例 6 比較命, 7 比較例 8 甘油 5 5 5 5 5 5 5 5 1,2-戊二醇 1 1 1 1 1 1 1 1 黃原膠 0.1 瓜爾膠 0.1 刺槐豆膠 0.1 塔拉膠 0.1 羅望子種子多糖類 0.1 Sclerotium 膠 0.1 辛稀基破珀酸鋁澱粉 3 純淨水 35.8 35.7 35.7 35.7 35.7 35.7 35.7 32. 8 三乙基己酸甘油醋 5 5 5 5 5 5 5 5 荷荷巴種子油 7 7 7 7 7 7 7 7 矽油 SH200c-10CS 1 1 1 1 1 1 1 1 m 3 Theobroma Grandiflorum 種子油 1 1 1 1 1 1 1 1 澳洲堅果脂肪酸植物甾 醇酯 3 3 3 3 3 3 3 3 聚甘油單硬脂酸酯-10 1.5 1.5 1.5 1.5 1.5 1.5 1.5 1. 5 甘油單硬脂酸酯 0. 5 0.5 0.5 0.5 0. 5 0.5 0.5 0_ 5 潜 7炒 瘅遛 抗壞血酸-2-磷酸酯鎂 鹽 6 6 6 6 6 6 6 6 檸檬酸 2 2 2 2 2 2 2 2 氫氧化鈉 1.2 1.2 1.2 1.2 1.2 1.2 1.2 1. 2 純淨水 30 30 30 30 30 30 30 30 經時穩ϊ t性室溫三日後 X 〇 X X X X X 〇 經時穩定性室溫一週後 X X X X X X X X 第二天硬度（g重） 0.3 0.7 0.6 0.3 0.6 0.3 0.7 0. 9 12 200911292 對於增粘多糖類的調配，調配黃原膠（比較例2)後，室溫下 3曰後未發生分離，但調配瓜爾膠、刺槐豆膠、塔拉膠、羅望子的 種子多糖類、Sclerotium膠的情況’室溫下3日後觀察，結果發 生了分離。因此，判斷增粘多糖類中黃原膠對提高經時穩定性有 效。此外發現，通過調配3. 〇質量％的辛烯基琥珀酸鋁澱粉（比較 例8) ’至溫下3日後不發生分離。但是，分別調配黃原膠、辛烯 基破轴酸銘澱粉時，室溫下1週後發生了分離。 〔試驗例2〕 ^遽站酸紹澱粉、i峨醇或鮫蠟醇的祐用教罢 广根據表2的組成，製備比較例9〜13、實施例卜5的水包油 1 Λ 、'且口物。分別將油相和水相加熱到85t：，充分攪拌後，將 加到水相中’料質器以__ _ 5分鐘。然後冷卻 C添加亚授拌抗壞血酸_2〜碟酸醋鎂鹽溶液。 ^艮據以下鮮’鞠崎_乳化組合彳_定性進行 汗價。 乳化穩定性 〇.不發生分離 △:微量分離 X:發生分離 析出 〇:未析此壞轉—鎂鹽 200911292 X :析出抗壞血酸-2-磷酸酯鎂鹽 對於得到的水包油型乳化组合物的發枯感，由1〇名專業評委 根據以下標準進行評分。 ~ ° 3:完全無發粘感 2 .發點感不明顯 1:有發粘感 0:有明顯的發粘感 將專業評委的評分進行平均，根據以下標準進行評價。 平均值2. 0以上 ：〇 平均值1.0以上、低於2.〇 :△Use a cosmetic such as a cream or a paper foundation or a skin external preparation. It can be used as a medicine or a medicine. </ RTI>, [Test Example 1] and octenyl succinic acid aluminum sulphate. According to the composition of Table 1, an oil-in-water emulsion composition of Comparative Example 丨8 was prepared. The oil phase and the water phase were separately heated to 85 ° C, and after thorough stirring, the oil phase was added to the water phase, and the mixture was stirred at 6000 rpm for 5 minutes with a homogenizer. Then, it was cooled to 5 ° C, and the ascorbic acid-2-phosphate magnesium salt solution was stirred and stirred. The time-dependent stable seat of the obtained oil-in-water emulsion composition was evaluated according to the following criteria. 〇·No separation occurred x: Separation occurred In addition, the hardness (unit: g weight) on the second day after preparation was measured. The conditions for determining the hardness are as follows. Device: FUDOH RHEO METER manufactured by Rheotech Co., Ltd., pressure sensitive shaft diameter. 11 200911292 10. Omm, sample table speed: 6 cm/min, immersion amount: 30 mm, load 2 〇〇 g Table 1 Comparative Example 1 Comparison · (歹2 Comparative injury 3 Comparative example 4 Comparative injury 1, 5 Comparative example 6 Comparative life, 7 Comparative example 8 Glycerin 5 5 5 5 5 5 5 5 1,2-pentanediol 1 1 1 1 1 1 1 1 Xanthan gum 0.1 guar 0.1 locust bean gum 0.1 Tara gum 0.1 tamarind seed polysaccharide 0.1 Sclerotium glue 0.1 octyl saponin aluminum starch 3 pure water 35.8 35.7 35.7 35.7 35.7 35.7 35.7 32. 8 triethylhexanoic acid vinegar 5 5 5 5 5 5 5 5 Jojoba Seed Oil 7 7 7 7 7 7 7 7 Emu Oil SH200c-10CS 1 1 1 1 1 1 1 1 m 3 Theobroma Grandiflorum Seed Oil 1 1 1 1 1 1 1 1 Macadamia Fatty Acid Phytosterol ester 3 3 3 3 3 3 3 3 Polyglycerol monostearate-10 1.5 1.5 1.5 1.5 1.5 1.5 1.5 1. 5 Glycerol monostearate 0. 5 0.5 0.5 0.5 0. 5 0.5 0.5 0_ 5 7 stir-fry ascorbate-2-phosphate magnesium salt 6 6 6 6 6 6 6 6 citric acid 2 2 2 2 2 2 2 2 Sodium hydroxide 1.2 1.2 1.2 1.2 1.2 1.2 1.2 1. 2 Purified water 30 30 30 30 30 30 30 30 Stable at room temperature t after room temperature for three days after X 〇 XXXXX 〇 Stability at room temperature after one week XXXXXXXX Hardness (g weight) on the second day 0.3 0.7 0.6 0.3 0.6 0.3 0.7 0. 9 12 200911292 For the formulation of polysaccharides, after the preparation of xanthan gum (Comparative Example 2), no separation occurred after 3 室温 at room temperature. However, the condition of guar gum, locust bean gum, tara gum, tamarind seed polysaccharides, and Sclerotium gum was observed. After 3 days at room temperature, the results were separated. Therefore, it was judged that xanthan gum was added to the polysaccharides. Improve stability over time. Further, it was found that no separation occurred after 3 days from the temperature of 3. 〇 mass% of octenyl succinate aluminum starch (Comparative Example 8). However, when xanthan gum and octene-based sclerosin-like starch were separately formulated, separation occurred one week after room temperature. [Test Example 2] ^The application of the acid-salting starch, the i-anol or the decyl alcohol in the station was carried out according to the composition of Table 2, and the oil-in-water 1 13 , ' of Comparative Examples 9 to 13 and Example 5 were prepared. And the mouth. The oil and water phases were separately heated to 85 t: and, after thorough agitation, were added to the aqueous phase ' massor for __ _ 5 minutes. Then, the C is added to the sub-mixed ascorbic acid-2~disc magnesium sulfate solution. ^ According to the following fresh '鞠崎_emulsified combination 彳 _ _ qualitative sweat price. Emulsification stability 〇. No separation occurred △: Micro-separation X: Separation and precipitation occurred 〇: No decomposition was observed - Magnesium salt 200911292 X: Precipitated ascorbic acid-2-phosphate magnesium salt for the obtained oil-in-water emulsion composition A sense of dryness was scored by a panel of professional judges based on the following criteria. ~ ° 3: No stickiness at all 2. No feeling of hair is noticeable 1: There is a feeling of stickiness 0: There is a noticeable stickiness. The scores of professional judges are averaged and evaluated according to the following criteria. The average value is 2.0 or more: 〇 The average value is 1.0 or more and less than 2. 〇 : △
平均值低於1.0 ： X 此外，測定製造後第二天的硬度（單位：g重），測定硬度的 條件如下所示。 裝置：（株）Rheotech 製 FUDOH RHEO METE1R、壓敏軸直押· • 〇酿、5式樣台速度：6cm/min、浸入量：30mm、負荷2〇〇。 § 0 14 200911292 表2 交例 9 交例 10 财交例 11 交例 12 交例 13 tbfe例 14 實施例 1 實施例 2 tim 3 雜例 4 cm 5 甘油 5 5 5 5 5 5 5 5 5 5 1,2-戊二醇 1 1 1 1 1 1 1 1 1 1 黃原膠 0.1 0.1 0.5 0.1 0.1 0.1 辛烯基琥珀酸鋁澱粉 3 3 3 3 3 2 純淨水 38 37. 9 36.5 35 34.9 33.5 36 33.4 34.9 36 mr 三（辛酸/癸酸/十四 烷酸/硬脂酸）甘油酯 1 1 1 1 1 1 1 1 1 1 月桂酰谷氨酸二（植 物甾醇/辛基月桂醇) 酯 2.5 2.5 2.5 2.5 2.5 2.5 2.5 2.5 2.5 2.5 荷荷巴種子油 5 5 5 5 5 5 5 5 5 5 矽油 SH200C-10CS 1.5 1.5 1.5 1.5 1.5 1. 5 1.5 1.5 1.5 1.5 鯨蠟醇2-乙基己酸 酯 3 3 3 3 3 3 3 3 3 3 山*%醇 1.5 1.5 1.5 1.5 2.5 聚山梨醇酯60 2 2 2 2 2 2 2 2 2 2 鯨蠟醇 2.5 聚甘油單硬脂酸醋 -10 0.7 0.7 0.7 0.7 0.7 0. 7 0.7 0.7 0.7 0.7 甘油單硬脂酸酯 1.1 1.1 1.1 1.1 1.1 1. 1 1.1 1.1 1.1 1.1 龄iS 抗壞血酸-2-磷酸酯 鎂鹽 6 6 6 6 6 6 6 6 6 6 檸檬酸 2 2 2 2 2 2 2 2 2 2 氫氧化納 1.2 1.2 1.2 1.2 1.2 1.2 1.2 1.2 1.2 1.2 純淨水 30 30 30 30 30 30 30 30 30 30 乳化穩定性5°C 6個月後 X X X X X X Δ 〇 〇 〇 乳化穩定性室溫6個月後 X X X X X X Δ 〇 〇 〇 乳化穩定性40°C 6個月後 X X X X X X Δ 〇 〇 〇 析出5°C 6個月後 — — — — — — 〇 〇 〇 〇 析出室溫6個月後 — — — — — — 〇 〇 〇 〇 析出40°C 6個月後 — — 一 — — — 〇 〇 〇 〇 發粘感 — — — — — — Δ 〇 〇 〇 第二天硬度（g重） 0.4 0.5 1.2 0.7 0.9 5.4 5.5 5.5 6.0 5.5 15 200911292 不論是分解獨娜黃麟、山蝓醇、辛雜琥雜域粉 時（比較例10〜丨2)，還是組合雛黃原踢、辛稀基號輸呂殿粉 時（比車乂例13)，或是組合調配辛婦基號轴酸铭殿粉和山喻醇時 (比較例14)，水包油型乳化組合物6個月都會發生分離，但調配 有黃原膠、山喻醇（或録_)、辛婦基琥爾細粉這3種化合 物的實施例2〜4 ’在5t〜耽下’水包油魏化組合物不發生口 分離’是穩㈣。組合調配黃原膠和山喻醇的實施例丄的水包油 型乳化組合物6個月微量分離。 〔試驗例3〕 水的調配量的分;^ 根據表3的組成，製備比較例15、實施例5〜9的水包油乳化 型組合物。分麟油姊水相加熱至85〇c，充分勝後，將油相 添加到水相巾，簡質如6麵_獅5分鐘。然後冷卻至 50C，添加並攪拌抗壞血酸_2_磷酸酯鎂鹽溶液。 根據以下標準’對得到的水包油型乳化組合物的歉性進行 評價。 乳化穩定性 〇：不發生分離 △:微量分離 X:發生分離 析出 16 200911292 〇：未析出抗壞血酸-2-磷酸酯鎂鹽 X .析出抗壞血酸-2-麟酸酯鎂鹽 由10名專業評委 對於得到的水包油型乳化組合物的發柏感， 根據以下標準進行評分。 3:完全無發粘感 2:發粘感不明顯 1:有發粘感 f 0:有明顯的發粘感 將專業評委鱗分進行平均，根據以下標準進行評價 平均值2. 0以上 ：◦ 平均值1. 0以上、低於2. 〇 : △The average value was less than 1.0 : X In addition, the hardness (unit: g weight) on the second day after the production was measured, and the conditions for measuring the hardness were as follows. Device: Rheotech Co., Ltd. FUDOH RHEO METE1R, pressure sensitive shaft directing • Brewing, 5-type table speed: 6 cm/min, immersion: 30 mm, load 2 〇〇. § 0 14 200911292 Table 2 Example 9 Example 10 Financial Example 11 Example 12 Example 13 tbfe Example 14 Example 1 Example 2 tim 3 Example 4 cm 5 Glycerin 5 5 5 5 5 5 5 5 5 5 1 , 2-pentanediol 1 1 1 1 1 1 1 1 1 1 xanthan gum 0.1 0.1 0.5 0.1 0.1 0.1 octenyl succinate aluminum starch 3 3 3 3 3 2 purified water 38 37. 9 36.5 35 34.9 33.5 36 33.4 34.9 36 mr Tris(octanoic acid/capric acid/tetradecanoic acid/stearic acid) glyceride 1 1 1 1 1 1 1 1 1 1 Lauroyl glutamic acid di(phytosterol/octyl lauryl alcohol) ester 2.5 2.5 2.5 2.5 2.5 2.5 2.5 2.5 2.5 2.5 Jojoba seed oil 5 5 5 5 5 5 5 5 5 5 Emu oil SH200C-10CS 1.5 1.5 1.5 1.5 1.5 1. 5 1.5 1.5 1.5 1.5 Cetyl alcohol 2-ethylhexanoate 3 3 3 3 3 3 3 3 3 3 Hill*% alcohol 1.5 1.5 1.5 1.5 2.5 Polysorbate 60 2 2 2 2 2 2 2 2 2 2 Cetyl alcohol 2.5 Polyglycerol monostearate-10 0.7 0.7 0.7 0.7 0.7 0. 7 0.7 0.7 0.7 0.7 Glycerol monostearate 1.1 1.1 1.1 1.1 1.1 1. 1 1.1 1.1 1.1 1.1 Age iS Ascorbic acid-2-phosphate magnesium salt 6 6 6 6 6 6 6 6 6 6 Citric acid 2 2 2 2 2 2 2 2 2 2 sodium hydroxide 1. 2 1.2 1.2 1.2 1.2 1.2 1.2 1.2 1.2 1.2 Purified water 30 30 30 30 30 30 30 30 30 30 Emulsification stability 5 ° C After 6 months XXXXXX Δ 〇〇〇 Emulsification stability Room temperature 6 months later XXXXXX Δ 〇〇 〇Emulsification stability 40 °C After 6 months XXXXXX Δ 〇〇〇5°C after 6 months — — — — — — 〇〇〇〇 室温 室温 室温 6 6 6 6 6 6 6 6 6 6 6 6 6 6 6 6 6 6 6 6 6 6 6 6 6 After decomposing 40 ° C for 6 months — — — — — — — — — — — — — — — — — — — — — — — — — — — — — — — — — — — — — — — — — — — — — — — — — — — — — — — — — — — — — 15 200911292 Whether it is the decomposition of Dina Huanglin, Hawthorn alcohol, Xinzao miscellaneous powder (Comparative example 10~丨2), or combination of the original Huangyuan kick, Xindi base number lost Lu Dian powder (than the rut In the case of Example 13), or when the combination of Xiningji Axis Acid Mingtang Powder and Shanyu Alcohol (Comparative Example 14), the oil-in-water emulsion composition will be separated in 6 months, but the yellow gum and the mountain are blended. Example 2~4 'in 5t~耽' of the three compounds of the alcohol (or _) and the sylvestre The oil-in-water Weihua composition does not undergo oral separation, which is stable (4). The oil-in-water emulsion composition of Example 调, which was combined with xanthan gum and yam, was subjected to 6-month micro-separation. [Test Example 3] The amount of water to be blended; ^ The oil-in-water emulsion composition of Comparative Example 15 and Examples 5 to 9 was prepared according to the composition of Table 3. The water phase of Linlin Oil is heated to 85〇c. After the victory, the oil phase is added to the water phase towel, which is as simple as 6 faces _ lion for 5 minutes. Then, it was cooled to 50 C, and the ascorbic acid-2-phosphate magnesium salt solution was added and stirred. The apology of the obtained oil-in-water emulsion composition was evaluated according to the following criteria. Emulsification stability 〇: No separation occurs △: Micro-separation X: Separation and precipitation occurred 16 200911292 〇: Ascorbate-2-phosphate magnesium salt was not precipitated X. Ascorbate-2-Lactate magnesium salt was precipitated by 10 professional judges The sensation of the oil-in-water emulsion composition was scored according to the following criteria. 3: No stickiness 2: Sticky feeling is not obvious 1: There is sticky feeling f 0: There is a clear sticky feeling. The professional judges scales are averaged, and the average value is evaluated according to the following criteria: 2.0 or more: ◦ The average value is 1.0 or more and less than 2. 〇: △
平均值低於1.0 : X 此外’測定製造後第二天的硬度（單位·· g重），剛定硬声的 條件如下所示。 裝置：（株）Rheotech製FUDOH RHEO METER、壓敏輪直押 10. Omm、試樣台速度：6cm/min、浸入量：30mm、負荷加如。 17 200911292 表3 比較例 15 實施例 5 實施例 6 實施例 7 實施例 8 實施例 9 甘油 5 5 5 5 5 2 1, 2-戊二醇 1 1 2 2 1 1 黃原膠 0.1 0.1 0.05 0.2 0.2 0.1 辛烯基破珀酸鋁澱粉 3 3 3 3 3 0.5 純淨水 25.4 30.4 29.75 28.6 39.8 34.3 三（辛酸/癸酸/十四烷酸/ 硬脂酸）甘油酯 4 4 5 5 1 1 澳洲堅果脂肪酸植物甾醇 酯 3 3 月桂酰谷氨酸二（植物甾 醇/辛基月桂醇）酯 2.5 2.5 2.5 1 mr 荷荷巴種子油 10 5 5 5 5 2.5 矽油 SH200c-10CS 1.5 1.5 1 1 1.5 0.5 鯨蠟醇2-乙基己酸酯 3 3 3 2 山蝓醇 1.5 1.5 3 4 1.5 0.5 聚山梨醇酯60 2 2 2 2 2 1.2 聚甘油單硬脂酸酯-10 0.7 0.7 1.5 1.5 0.7 0.5 甘油單硬脂酸酯 1.1 1.1 0.5 0.5 1.1 0.6 f挺 抗壞血酸-2-磷酸酯鎂鹽 6 6 6 6 5 8 7钕 檸檬酸 2 2 2 2 1.7 2.7 氫氧化納 1.2 1.2 1.2 1.2 1 1.6 純淨水 30 30 30 30 25 40 乳化穩定性5°C 6個月後 〇 〇 〇 〇 〇 〇 乳化穩定性室溫6個月後 〇 〇 〇 〇 〇 〇 乳化穩定性40°C 6個月後 〇 〇 〇 〇 〇 〇 析出5°C 6個月後 X 〇 〇 〇 〇 〇 析出室溫6個月後 X 〇 〇 〇 〇 〇 析出40°C 6個月後 X 〇 〇 〇 〇 〇 發粘感 〇 〇 〇 〇 〇 〇 第二天硬度（g重） 5.8 5.5 6.0 6.3 6.0 3.8 18 200911292 相對於6質量％的抗壞血酸-2-碟酸酯鎂鹽，只調配56. 48質 量％ (25.4質量％ + 30質量«的純淨水’純淨水的調配量低於抗 壞血酸-2-磷酸酯鎂鹽的調配量的10倍量的比較例15，6個月析 出抗壞jk酸-2-璃酸酯鎂鹽。但是，相對於6質量％的抗壞血酸-2-磷酸酯鎂鹽，調配60.4質量％(30.4質量％ + 30質量％)的純淨水， 純淨水的調配量為抗壞血酸-2-磷酸酯鎂鹽的調配量的1〇倍量以 上的實施例5，6個月不發生分離，是穩定的。所以爲了維持本 發明的水包油型乳化組合物的穩定性，必須調配抗壞血酸-2-磷酸 酯鎂鹽的調配量的1〇倍量的純淨水。如實施例6〜9所示，能夠 得到調配5〜8質量％的抗壞血酸-2-磷酸酯鎂鹽的穩定的水包油塑 乳化組合物。 【圖式簡單說明】 ^ 【主要元件符號說明】 19The average value is less than 1.0 : X In addition, the hardness (unit··g weight) on the second day after manufacture is measured, and the conditions for the hard sound are as follows. Device: FUDOH RHEO METER manufactured by Rheotech Co., Ltd., pressure sensitive wheel, 10. Omm, sample table speed: 6 cm/min, immersion amount: 30 mm, load plus. 17 200911292 Table 3 Comparative Example 15 Example 5 Example 6 Example 7 Example 8 Example 9 Glycerin 5 5 5 5 5 2 1, 2-Pentanediol 1 1 2 2 1 1 Xanthan gum 0.1 0.1 0.05 0.2 0.2 0.1 octenyl saponin aluminum starch 3 3 3 3 3 0.5 purified water 25.4 30.4 29.75 28.6 39.8 34.3 tris(octanoic acid/capric acid/tetradecanoic acid/stearic acid) glyceride 4 4 5 5 1 1 macadamia fatty acid Phytosterol ester 3 3 lauroyl glutamic acid bis (phytosterol / octyl lauryl alcohol) ester 2.5 2.5 2.5 1 mr jojoba seed oil 10 5 5 5 5 2.5 eucalyptus oil SH200c-10CS 1.5 1.5 1 1 1.5 0.5 cetyl alcohol 2-ethylhexanoate 3 3 3 2 behenyl alcohol 1.5 1.5 3 4 1.5 0.5 Polysorbate 60 2 2 2 2 2 1.2 Polyglycerol monostearate-10 0.7 0.7 1.5 1.5 0.7 0.5 Glycerol monostearyl Acid ester 1.1 1.1 0.5 0.5 1.1 0.6 f very ascorbic acid-2-phosphate magnesium salt 6 6 6 6 5 8 7 citric acid 2 2 2 2 1.7 2.7 sodium hydroxide 1.2 1.2 1.2 1.2 1 1.6 pure water 30 30 30 30 25 40 Emulsification stability 5 ° C After 6 months, emulsification stability, room temperature after 6 months 〇〇〇〇 〇〇Emulsification stability 40°C After 6 months, 5°C is decanted. After 6 months, X 〇〇〇〇〇 is precipitated at room temperature for 6 months and X 〇〇〇〇〇 is precipitated at 40°C. After a month, X 粘 粘 粘 〇〇〇〇〇〇 〇〇〇〇〇〇 〇〇〇〇〇〇 〇〇〇〇〇〇 〇〇〇〇〇〇 5.8 5.8 5.8 5.5 6.0 6.0 6.0 6.0 6.0 6.0 6.0 6.0 6.0 6.0 5.5 Only the blending amount of 56.48 mass% (25.4 mass% + 30 mass «pure water' pure water is less than 10 times the amount of the ascorbate-2-phosphate magnesium salt, and the precipitation is 6 months. Anti-defective jk-acidic acid-magnesium salt. However, 60.4% by mass (30.4% by mass + 30% by mass) of pure water, pure water is blended with respect to 6 mass% of ascorbic acid-2-phosphate magnesium salt. In Example 5, which was a compounding amount of the amount of the ascorbic acid-2-phosphate magnesium salt, the amount of the compound was not more than 6 months, and was stable. Therefore, in order to maintain the stability of the oil-in-water emulsion composition of the present invention, it is necessary to mix 1 liter of pure water of the amount of the ascorbyl-2-phosphate magnesium salt. As shown in Examples 6 to 9, a stable oil-in-water emulsified composition containing 5 to 8 mass% of ascorbic acid-2-phosphate magnesium salt can be obtained. [Simple description of the figure] ^ [Explanation of main component symbols] 19