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Ковальова Т.М., Половко Н.П. Фізико­хімічне та реологічне дослідження емульсійних основ з комплексним емульгатором Olivem 1000.
28.05.2014, 18:23

Резюме
Ковальова Т.М.1, Половко Н.П.2 Фізико-­хімічне та реологічне дослідження емульсійних основ з комплексним емульгатором Olivem 1000.
Досліджено фізико-хімічні та реологічні властивості емульсійних основ з використанням комплексного емульгатора для емульсій типу олія/вода Олівем 1000 рідкої, середньої та густої кремоподібної консистенції. Доведено, що Олівем 1000 дає можливість отримувати оптимальні за показниками в’язкості стабільні емульсії при концентрацій масляної фази до 30%. Вивчено вплив масової частки олійної фази на стабільність та реологічні параметри кремових основ. Досліджено зміну споживчих та реологічних характеристик кремових основ при додаванні згущувачів.
Ключові слова: емульсійні основи, реологічні дослідження.
Резюме
Ковалева Т.Н., Половко Н.П. Исследование эмульсионных основ с Olivem 1000.
Исследованы физико-химические и реологические свойства эмульсионных основ с использованием эмульгатора для прямых эмульсий Olivem 1000 жидкой, средней и густой кремообразной консистенции. Доказано, что Olivem 1000 дает возможность получать оптимальные по показателям вязкости стабильные эмульсии при концентрации масляной фазы до 30%. Изучено влияние массовой доли масляной фазы на стабильность и реологические параметры кремовых основ. Исследовано изменение потребительских и реологических характеристик кремовых основ при добавлении загустителей.
Ключевые слова: эмульгаторы, эмульсионные основы, реологические исследования.
Summary
Kovalev T.N, Polovko N.P. Physicochemical and rheological investigation of emulsion bases with Olivem 1000 complex emulsifying agent.
Studied physico-chemical and rheological properties emulsion bases with using emulsifier for emulsion direct Olivem 1000 liquid medium and thick creamy consistency. Proved that Olivem 1000 enables to obtain the optimum in terms of viscosity stable emulsions of oil phase at a concentration of 30%. The influence of the mass fraction of the oil phase on the stability and rheological properties of the cream base. The change in the consumer and rheological characteristics of the cream base by adding thickeners.
Key words: emulsifiers, emulsion base, rheological studies.

Рецензент: д.фарм.н., проф. І.І. Баранова

УДК 615.451.124.014.23

Національний фармацевтичний університет (Харків)

Национальный фармацевтический университет (Харьков)

61002, г. Харьков, ул. Пушкинская, 53

National University of Pharmacy (Kharkov) Ukraine,

61002, Kharkov, 53, str. Pushkinska

1tatyko72@gmail.com

2polovko.nat@mail.ru

Introduction. Wide range of surface-active substances for emulsion system formation induces to the search of emulsifying agents with a number of advantages and additional properties: moistening, reparative, protective, compensatory, nutritious, etc. One of the promising groups of emulsifying agents is natural products, derived from the processing of olive oil with Olivem as a joint name (manufactured by В&Т, Іtaly). Olivem 1000 favourably stands out against all of them, and in addition to its high emulsifying properties it is a reactant, which can reproduce and keep up the integrity of epidermal barrier of skin [10, 11].

Olivem 1000 can form liquid-crystalline structures, which stabilize emulsions, imitate molecular organization of intercellular lipidic matrix of corneal layer, so it can integrate into lipidic barrier of skin. More over, thanks to fatty acids, which are the part of Olivem 1000 and have physiological affinity with the fats of skin, substance can provide the transport of active pharmaceutical ingredients to deep layers of the skin, thus regulating the level of their hydration [6, 9].

Peculiarities of the structure, dermatological compatibility with skin lipids as well as moisturizing properties of Olivem 1000 make it possible to obtain stable emulsion bases promissory for the production of makeup preparations for sensitive, problem-prone skin and preparations for the correction of involutional changes of skin [8, 7].

Object of the work. Handling and investigation of model samples of the emulsions on the basis of Olivem 1000 with the aim of further production of medicinal agents and makeup preparations of different consistency on their basis.

Materials and methods of the research. For the preparation of the emulsion bases it was used the following: emulsifier oil/water Olivem 1000 – mixture of cetearyl oleate and sorbitan oleate [10], liquid petrolatum (SPhU 1.2) and purified water (SPhU 1.2), as well as hydrophilic gelling agent РапиТикс А-60/ RapiTics A-60 (sodium polyacrylate/ hydrogenated polydecene/ trideceth-6, ISP) and cetostearyl alcohol CSA, emulsifiying agent of the 2 class (SPhU 1.0, 1.2).

For comparison purposes industrial samples of the creams of liquid, thick and medium consistency were used: cosmetic milk, day cream and night cream for dry and sensitive skin, «Active care» series («Біокон/Biokon», Ukraine).

Criteria and quality indices in elaboration of formulation of emulsion bases were: organoleptic and sensor properties, thermo- and colloidal stability, рН value and some rheological values [2,3,4, 5].

Determination of colloidal stability has been performed by means of centrifugation during 5 min. with 1000 s-1 revolutions frequency. Thermal stability has been determined in the condition of thermostat (ТC-80М-2) with 42,5+2,5 ºС temperature during 7 days [3]. рН determination of model samples was performed by potentiometric method at 10% water extraction from the cream at “рН 150 МИ” рН-meter (Russia). Rheological researches have been performed at “BROOKFIELD НВ DV-ΙΙ PRO” viscosimeter (USA) within the range of rate of shear 0,1 s-1 - 150 s-1 (SС4-21 spindle for 8,3 ml chamber) at 20ºС temperature [1].

Findings and discussion of them. Experimental samples have been prepared in accordance with the following technology: previously weighed out vaseline oil, Olivem 1000 (according to the formulation) have been heated double boiling up to 80-90оС. Water has been heated up to 80-90оС at the same time. Then the water has been added to oil phase and emulsified with the help of laboratory homogenizer (2000 rpm) until getting a uniform mass. Physicochemical investigations of the samples received have been conducted in 24 hours after complete chilling and structuring of the system.

The first series of experimental samples of emulsion bases has been studied with the aim of determination of concentration range of oil phase, which Olivem 1000 in 5% quantity (concentration averagely recommended by the manufacturer) can form stable emulsions [10].

The composition of model samples is given in Table 1.

Table 1

Composition of experimental samples of emulsion bases

Mass concentration of the ingredients, %

Composition

1

2

3

4

5

6

7

8

Vaseline oil

0

5,0

10,0

15,0

20,0

25,0

30,0

35,0

Olivem 1000

5,0

5,0

5,0

5,0

5,0

5,0

5,0

5,0

Purified water

up to 100,0

The results of the researches indicate that samples № 1, 2 were colloidally unstable and too liquid by its consistency, and a sample № 8 laminated during further preservation, which caused their exclusion from further researches in their initial state.

The results of the researches of physicochemical and sensor properties of stable samples are given in Table 2.

Table 2

Properties of experimental samples of emulsion bases

Quality indices

Number of a sample

№3

№4

№5

№6

№7

Thermal stability

stable

stable

stable

stable

stable

Colloidal stability

stable

stable

stable

stable

stable

Structural viscosity, Pа·s with 3 rev/min

56,3±2,8

66,5±3,3

89,6±4,5

95,3±4,7

101,0±5,1

Structural viscosity, Pа·s with 20 rev/min

1,41±0,07

1,72±0,08

2,15±0,11

2,38±0,10

2,62±0,11

рН

7,5±0,3

7,9±0,4

7,9±0,4

7,7±0,5

7,4±0,4

Organoleptic and sensor properties

Light creamy consistency, easy the apply, well spread and absorbed

Creamy consistency, well spread and absorbed

Thick creamy consistency, well spread and absorbed

Thick creamy consistency, easily spread, absorbed, leaving a fatty film

Thick cream, easily spread, absorbed, leaving a fatty film

Samples № 1,2 have been elaborated by means of introduction of РапиТикс А-60/ RapiTics A-60, which provided necessary consistent properties and colloidal stability. CSA was used as a co-emulsifier in the formulation of a sample №8, it forwarded the stability of the emulsion, but worsened sensor characteristics of a cream.

It should be noted, that the viscosity of the present series of model samples was increasing proportionally to the concentration of oil phase (Figure 1).

Figure1. Dependence of structural viscosity of model samples on oil phase concentration

Following studies have been conducted to obtain the emulsion samples of given consistency (liquid, medium and thick) on the basis of Olivem 1000. For this  purpose Olivem 1000 was used as a mono emulsifier, varying its mass concentration, and the combination with РапиТикс А-60/ RapiTics A-60 was used to obtain stable liquid emulsions. The composition of model bases is given in Table 3.

Table 3

Composition of experimental samples of model bases

Mass concentration of ingredients, %

Composition

1

2

3

4

5

6

7

8

9

10

11

12

13

Vaseline oil

0

0

3,0

3,0

3,0

5,0

5,0

5,0

8,0

8,0

8,0

10,0

10,0

Olivem 1000

5,0

8,0

3,0

5,0

8,0

3,0

5,0

8,0

3,0

5,0

8,0

3,0

5,0

РапиТикс А-60/ RapiTics A-60

0,3

 

0,3

0,3

 

0,3

 

 

 

 

 

 

 

Purified water

Up to 100,0

Composition

14

15

16

17

18

19

20

21

22

23

24

25

26

Vaseline oil

10,0

15,0

15,0

15,0

20,0

20,0

20,0

25,0

25,0

25,0

30,0

30,0

30,0

Olivem 1000

8,0

3,0

5,0

8,0

3,0

5,0

8,0

3,0

5,0

8,0

3,0

5,0

8,0

Purified water

Up to 100,0

 

It is noted, that the increase in stability and viscosity of a cream is forwarded by introduction of gelling agents, particularly РапиТикс А-60/ RapiTics A-60. Thus, the introduction of it to the composition of emulsion bases with minimal mass concentration of oil phase (up to 5%) in the 0,3% concentration, recommended by the manufacturer, results in formation of stable emulsions, that makes it reasonable to perform additional researches with other gelling agents.

In turn the concentration 20% and more of vaseline oil worsens tactile sensation during cream application and reduces to its stickness. But the use of the emulsifier of the 2 class and a structure-forming agent – cetostearyl alcohol in the ratio of 7:3 to the creams with high content of vaseline oil increases the indices of viscosity, provides stability and improves consumer characteristics of the creams studied.

It has been found experimentally that the increase in emulsifier content promotes the increase of indices of viscosity of the samples. Thus, a stable sample has been obtained which contains 8% of Olivem 1000 without Vaseline oil of creamy consistency (so-called oil-free mixture), which however had unsatisfactory tactile characteristics. Thanks to a small quantity of oil and to the presence of РапиТикс А-60/ RapiTics A-60 the samples №3, 4, 6 had satisfactory tactile characteristics and the consistency of a liquid cream. The samples №7, 9, 12, where the mass concentration of oil has been increased, were also stable and had the consistency of a liquid cream. The samples № 15, 18, 21, 24 were colloidal and thermally unstable so they have been excluded from further investigations. The samples № 10, 13, 16, 19, 22, 25 were stable and had a creamy consistency. The samples №5, 8, 11, 14, 17, 20, 23, 26 were also stable and had thick creamy consistency.

The samples № 7, 13, 16, 19, 22, 25 were liable to rheological investigations, the most precisely meeting the requirements of regulatory documents on cosmetic creams as for organoleptic, physicochemical and sensor properties [3].

Basing on the results of the investigation of structural and mechanical properties of experimental samples complete rheograms on the dependence of rate of shear (Dr) on shear stress (tr) under 20 ºС temperature were built (Figure 2).

Given rheorgams as well as structural and mechanical properties of model compositions examined were close to industrial samples of creams of liquid and medium consistency. To obtain thick creams for decreasing of the amount of oil phase and  Olivem 1000 it is reasonable to combine it with CSA in a 7:3 ratio. Such a ratio of emulsifiers is based on the calculation of hydrophilic-lipophilic balance of the system.

Figure 2 . Rheogram of the dependence of rate of shear (Dr) on shear stress (t), where 7, 13, 16,19, 22, 25 – are model samples of emulsion bases, А – comparison sample (cream of a medium consistency), В – comparison sample (cream of a liquid consistency)

The presence of hysteresis loops on the rheograms of flow indicates adequate thixotropy of samples examined: the structure can fail under high shear stress, but it gradually recovers after the drop of shear stress. Model samples also had good consumer characteristics. The results of the researches make it possible to continue the study of the samples obtained for physicochemical stability in the process of preservation.

Conclusions:

Model samples of emulsion bases Olivem 1000 of liqiud, medium and thick creamy consistency has been designed. It has been found, that Olivem 1000 makes it possible to obtain stable emulsions optimal by viscosity indices with oil phase concentration up to 30%.

Optimal mass concentration of Olivem 1000 for emulsions different by concentration has been determined: liquid – up to 3%; creamy consistency – 4-5%, thick – 6-8%.

Flexible and viscid as well as thixotropic properties of model samples of emulsion bases confirmed by good ability to spread and satisfactory sensor characteristics have been studied.

The influence of mass concentration of oil phase on the stability and rheological parameters of cream bases has been studied.

The change of consumer and rheological characteristics of cream bases adding РапиТикс А-60/ RapiTics A-60 gelling agent and CSA emulsifier has been examined.

Physicochemical and rheological investigations done indicate the prospectivity of the use of Olivem 1000 emulsifier in order to obtain emulsion bases of different consistency and to form medicinal and makeup preparations on their basis.

Література

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