Formulation and Evaluation of Grape Seed Oil (Vitis Vinifera, L) Facial Cream with Variations in The Concentration of Stearic Acid as an Emulsifier

Ageing is a complex biological process resulting from intrinsic ageing and extrinsic ageing. The most influential factor in ageing is free radicals because they can cause oxidative stress, which plays an essential role in the ageing process. Oligomeric proanthocyanidins (OPC) in grapeseed oil have the highest antioxidant effect against free radicals. These antioxidants are used in cosmetic products to maximize the treatment of ageing. This study aims to optimize the formula for grape seed oil cream by varying the concentration of stearic acid as an emulsifier. Grape seed oil is formulated into cream preparations which are divided into three formulas, namely formula one (F1), which uses 10% stearic acid concentration, formula two (F2) 12% stearic acid concentration, and formula three (F3) 14% stearic acid concentration. Determination of optimum stability and formula is obtained from the evaluation of cream preparations, including organoleptic, physical homogeneity, pH, dispersion, viscosity, and emulsion type tests. The results showed that the concentration of stearic acid emulsifiers affected the spreadability and viscosity. And does not affect the pH, homogeneity, and type of emulsion. Formulation and Evaluation of Grape Seed Oil (Vitis Vinifera, L) Facial Cream with Variations in The Concentration of Stearic Acid as an Emulsifier (Supriadi, et al.)


Introduction
Ageing is a complex biological process due to intrinsic factors (from within the body, such as genetics) and extrinsic factors (from the environment). Extraneous factors that play the most role in ageing are free radicals. Free radicals can majorly impact the ageing process because they can cause oxidative stress [1]. Psychosocial effects have created a demand to fight ageing on the skin, one of which is anti-ageing cosmeceutical products. Anti-ageing products used to fight age caused by free radicals contain antioxidants as their active ingredients [2].
Antioxidants from grapes (Vitis vinifera, L) are considered a good source of antioxidants. It mainly due to oligomeric proanthocyanidins (OPC) in grapeseed oil.
Wine is a commodity that provides added value. It can be consumed as fresh fruit, grape juice, drinks (wine), raisins, and others [3]. Grapes contain various vitamins and minerals, such as calcium, magnesium, potassium, vitamins B1, B2, B3, B5, B6, and C and contain flavonoid compounds. The skin of grapes is rich in resveratrol, a substance that can delay the appearance of wrinkles on the skin. Research on the use of red grape juice (Vitis vinifera L.) in cream preparations showed that red grape juice with a concentration of 3% was able to reduce evaporation of water from the skin by 9.79% -10.68 [4].
Grapeseed oil contains antioxidants that are beneficial in treating the skin. The antioxidants contained in it are vitamin E and oligomeric proanthocyanidins (OPC). This OPC serves to ward off free radicals that damage skin tissue. OPC can repair collagen damaged by free radicals, thus preventing wrinkles on the skin. The content of vitamin E in grape seed oil is also beneficial for the skin, where vitamin E helps moisturize the skin, improve skin elasticity and reduce the appearance of wrinkles [5].
The presence of antioxidant activity in grape seed oil can be used to properly utilize grape seed waste and potentially make cosmetics for skin care, for example, on facial skin.
Currently, the use of cosmetics is increasing, especially with antioxidants that prevent premature ageing and neutralize free radicals on the skin [6]. Based on its ability as an antioxidant, grapeseed oil can be formulated in the form of cream preparations. Creams in the form of antioxidants protect the skin from environmental influences (sun exposure and pollution) by inhibiting skin damage and premature ageing [7].
Cream preparations are widely chosen as topical preparations because they are easy to use, formulate and function as good protectors, comfortable, and evenly distributed to the skin [8]. Many patients and doctors prefer creams over ointments because creams are easier to spread and clean [9]. The type of cream is divided into two: the type of cream in oil in water (W/A) and water in oil (W/W). Oil (W/M) is more accessible to wash with water and is not slippery when applied to the skin, such as on the face and is indicated for cosmetics [10]. Stearic P-ISSN 2962-5769 • E-ISSN 2962-0007 acid has an essential role in cream formulations, namely as an emulsifier with a concentration of 1-20%. The use of stearic acid in oil-in-water (W/W) cream-type formulations [11].
Based on the above explanation, a cream formulation for the face with type M/A was made, which contains the active substance of grape seed oil as an antioxidant. This grape seed oil W/A cream formula uses stearic acid emulsifier concentration with several variations, and the cream formula is good and physically stable.
The type of research conducted is experimental research. Several steps were carried out. It included searching for grapeseed oil samples, formulation of grape seed oil cream, physical evaluation of the finished cream including organoleptic testing, testing pH, viscosity, homogeneity, spreadability and emulsion type. The manufacture of grapeseed oil is carried out by Lansida Herbal Technology, Yogyakarta, Central Java.

A. Making Procedure
Weigh all the ingredients that will be used in making the cream. Enter the components included in the oil phase (grapeseed oil, stearic acid, cetyl alcohol, stearyl alcohol) into a cup and then heat in a water bath, stir until homogeneous with stirring until it reaches a temperature of 70-75°. Then enter the propyl paraben and methyl paraben into the oil phase and stir until homogeneous. The solubility of propyl paraben and methyl paraben is very slightly soluble in water, in 3.5 parts of ethanol (95%), in 3 parts of acetone, and 140 parts of glycerol, and 40 parts of fatty oils, easily soluble in alkaline hydroxide solutions. Melting Temperature 95° to 98° [12].
Mix the aqueous phase (glycerin, triethanolamine and hot aquadest) with heating until the temperature reaches 70-75°. Then mix the two phases, namely the oil phase and the water phase, into a hot mortar. Stir until a good cream preparation is formed (see Table 1).

Formulation and Evaluation of Grape Seed Oil (Vitis Vinifera, L) Facial Cream with Variations in
The Concentration of Stearic Acid as an Emulsifier (

B. Preparation Evaluation
Physical evaluation test of the preparation was carried out for 28 days on days 0, 7, 14, 21 and 28. It included organoleptic observation, viscosity testing, pH measurement, homogeneity testing, spreading power testing and cream type testing. Organoleptic observations of cream preparations include observations of the colour, texture, and odour of cream preparations [13]. Measurement of pH using a pH indicator. Weighed as much as 0.5 g and dissolved in 50 mL of distilled water, then measured the pH. The tolerance for cream pH ranges from 4.0 to 8 (SNI 16-4399-1996). Viscosity measurements were carried out using a viscometer (Brookfield). The preparation is stored in a 100 ml glass beaker as much as 100 grams, then attached to a spindle size four, and the rotor was run at a speed of 100 rpm; after showing a stable number, read and record the results [11]. Homogeneity testing is done by taking 1 gram of cream on the top, middle and bottom, then applying it to a piece of transparent glass (object glass). Observe if there are coarse grains visually [12].
Cream weighing 1 gram was placed in the middle of a round glass scale. On top of the cream is placed another round glass and ballast. So, the round glass and ballast weight is 150 grams, left for 1 minute. Then the diameter of the distribution was recorded [12]. The dispersion requirement for topical preparations is about 5-7 cm [14]. Good dispersion causes the contact between the drug and the skin to be broad so that the absorption of the drug into the skin takes place quickly.
The type of emulsion preparation was determined by placing a certain amount of preparation on an object glass, adding one drop of methyl blue, and stirring with a stirring rod.
If the methyl blue is evenly distributed, the preparation has an o/w emulsion type, but if only blue spots are present, the preparation has a w/o emulsion type [15]. P-ISSN 2962-5769 • E-ISSN 2962-0007

C. Statistic analysis
Analysis of research data using SPSS 21.0. From the results of the research on pH, dispersibility and viscosity, analysis was carried out using the Shapiro-Wilk test to state that the data were normally distributed. If the data is not normally distributed, statistical analysis using the Kruskal-Wallis test is used to determine the effect of variations in the concentration of stearic acid on grape seed oil cream preparations. Meanwhile, the organoleptic test results' data, homogeneity and emulsion type were analyzed descriptively.

Results
The manufacture of grapeseed oil is carried out by Lansida Herbal Technology, Yogyakarta, Central Java. The cream was made using grapeseed oil as the active ingredient and several other ingredients according to a predetermined formula. The prepared cream was evaluated by organoleptic, pH, spreadability, homogeneity, viscosity, and emulsion type tests.
The physical evaluation of cream preparations aims to determine the effect of variations in stearic acid concentration on the physical properties of the preparation. It includes cream organoleptic, pH, dispersibility, homogeneity, viscosity, and cream type tests.
The organoleptic examination includes the shape, colour and odour of the cream. The results of the organoleptic test can be seen in Table 2. The purpose of testing the pH of this cream preparation is to determine whether the cream has met the pH requirements for topical preparations, which are between 4.5-7.5. pH preparations that are too acidic can irritate the skin, while if the pH value is too alkaline, it can make the skin dry and scaly [16]. The pH test is carried out using pH indicator paper. The results of the pH measurement test can be seen in Table 3.

Formulation and Evaluation of Grape Seed Oil (Vitis Vinifera, L) Facial Cream with Variations in
The Concentration of Stearic Acid as an Emulsifier (Supriadi, et al.) 25 The homogeneity test determines the mixture of cream preparation ingredients [17].
In this evaluation, the homogeneity test of the cream was carried out visually by observing the colour of the cream and the presence or absence of parts that were not well mixed. The results showed that the cream preparation with stearic acid emulsifier met the homogeneity requirement. That is, no coarse particles were seen. The condition for the preparation of the cream is that if it is applied to a piece of glass, no separation between the components make up the emulsion. The results of the homogeneity test can be seen in Table 4.  The cream's spreadability was evaluated to determine the extent of the spread of the cream when applied to skin. So, the ease of laying the preparation to the skin could be seen.
The dispersion surface produced by increasing the loading is intended to describe the dispersion characteristics. The resulting surface area is directly proportional to the increase in the added load [18]. The dispersion requirement for topical preparations is about 5-7 cm [14].
The results of the dispersion test can be seen in Table 5. A viscosity test is carried out to determine the viscosity level of the resulting preparation. Viscosity is a statement of a liquid to flow. The higher the viscosity, the more P -ISSN 2962-5769 • E-ISSN 2962-0007 difficult it is to flow/ the greater the resistance [9]. The viscosity required by SNI 16-4399-1996 is 2.000cp-50.000cp. Viscosity test results can be seen in Table 6.  [15]. The results of the emulsion type test can be seen in Table 7.

Discussion
The manufacture of grapeseed oil is carried out by Lansida Herbal Technology, Yogyakarta, Central Java. Cream manufacture is divided into three formulas, where each formula differs only in adding the emulsifier concentration. In the first formula (F1), the added formula was stearic acid as much as 10% of the total formula. In the second formulation (F2), the emulsifier was added to 12% of the complete formula. And the third formula (F3) emulsifier added is 14% of the total formula. The procedure for making cream begins with heating the mortar and stamper by inserting hot water into the mortar and stamper, which is then allowed to stand for a while until the mortar is prepared for the mixing process of the two phases.

Formulation and Evaluation of Grape Seed Oil (Vitis Vinifera, L) Facial Cream with Variations in
The Concentration of Stearic Acid as an Emulsifier (Supriadi, et al.) 27 The melting of the oil phase, namely 5% grapeseed oil, 10% stearic acid (F1), 12% stearic acid (F2), 14% stearic acid (F3), 1% cetyl alcohol, 1% stearyl alcohol was carried out on a water bath at a temperature of ± 70˚C. Heating is carried out at a temperature of ± 70˚C because this temperature is the highest melting point for melting materials in the oil phase, Melting Temperature 95° C to 98°C [12].
At the same time, in the aqueous phase, 2% triethanolamine functioning emulsifier, and 10% glycerin which functions as a humectant and emollient, were mixed into distilled water at a temperature of ± 70˚C until all ingredients were dissolved. Added methylparaben stir until homogeneous. Mixing the oil and water phases is carried out at the same temperature of ± 70˚C to avoid separation between the two steps. Then the two phases are combined in a hot mortar and stirred using a stamper until a creamy mass is formed. After the cream mass is created, the preparation is put into a cream container.
The finished cream preparation was stored at room temperature. Physical evaluation included organoleptic observation, pH measurement, viscosity testing, homogeneity testing, spreadability and emulsion type. Physical evaluation of cream preparations aims to determine the effect of variations in stearic acid concentration on the physical properties of the preparation. It includes cream organoleptic, pH, dispersibility, homogeneity, viscosity, and cream type tests.
The organoleptic observations of F1, F2 and F3 creams on day 0 showed that the cream was white, odourless, and soft (Table 2). In F1, the cream did not change in colour, smell or texture after 28 days of storage. While in F2 and F3, the texture varies to become thick and solid on the 14th day of storage until the 28th day. It is influenced by the high viscosity of the cream preparation, which affects the viscosity of the preparation.
The pH value of cream F1, F2 and F3 on the 0th day in a row was 7. On the 7th day of storage, F1, F2 and F3 decreased the pH to 6 (  Table 5 expresses the results of evaluating the spreadability of grape seed oil cream.
Each formula shows a different spreadability when given a load of 150 g above the coverslip of the cream preparation. There was a decrease in dispersion until the 28th day of storage. F1 has a higher dispersion value than F2 and F3. It shows that the greater the concentration of stearic acid, the smaller the spread area produced due to an increase in viscosity. The wider the spread area created by a cream, the cream will have a better spreading ability when applied. However, the results showed that F1 did not meet the dispersion test requirements, while F2 and F3 met the criteria for the dispersion test.
From the results of the evaluation of the viscosity of the three formulas,

Conflict of Interest
We declare that there is no conflict of interest.