CA1196867A - Non-aqueous deodorant stick composition - Google Patents

Abstract

ABSTRACT OF THE DISCLOSURE

A deodorant stick composition of the propylene glycol soap type containing essentially no water and an effective amount of an antimicrobial agent;
said product preferably being transparent and containing from about 4% to about 6% by weight of anhydrous ethanol.

Description

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A NON-A~UEOUS DEODORANT STICK C9MPOSITI0~1 This in~ention relates to anhydrous long chain fatty a~id s~ap propylene glycol based deodorant stick composition containing an effective amount of an anti-microbial compound. More particularly, it relates to clear stick compositions of the above character which are clear and have a low anhydrous alcohol content.
It has been suggested in the prior axt to prepare sodium stearate-propylene glycol based deodorant sticks which contain known antibactexial agents. A typical composition of this character is disclosed in an article by Graham Barker in Cosmetics ~nd Toil~tries, ~ol. 92, July 1977, p. 73-75. On page 73, column 1, Barker discloses a s~ick composition containing 7% sodium stearate, 10%
SDA alcohol, 58% propylene ylycol, 0.2% Irgasan*DP 300 (a bacteriostat), 19.8~ PPG-3-myristyl ether and 5% water.
It has now heen found, however~ that the deodorant effectiveness of compositions o~ this character are very significantly affected by the presence of water and to some extent, the general hy~rophillic nature of the compo-nents that make up the stick. Each of these factors tendto reduce the ability of these stick compositions to combat odor.
Another desirable feature in a deodorant stick is its clarity. Several deodorant sticks axe marketed or described in the literature as ostensibly being "clear sticks". One such product is described in the U.S. Patent to ~edeon et al 4,268,498. However, the term "clear stick"
has been used loosely in this art and has been applied to products which are not truly clear i.e. ~ransparent but also * trade mark.

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to produc:ts which are merely translucent.
It has now also been found that truly clear deodorant E~ticks can 1: e prepared if to the above described anhydrous product, a controlled quantity of anhydrous ethyl alcohol is added. This quantity is within the range o:E from about 4% by weight to about 6~ by weight based on the total weight of the stick composition.
The stick co~ositions o~ the present invention have alæo been dem~nstrated to exhibit essentially DO StaiDing in in Yitro tests. In addition~ they have been shown to have good stability at room temperature and at elevated temperature retaining their physical integrity and clarity or transparency.
It is accordingly an ob~ect of the present invention to provide a de~dorant stick composition of improved deodorant efficacyO
It is also an object of the present invention to provide a deodorant stick compc~sition o~ improved de~dorant ef.ficacy wh:Lch is also truly clear stick i. e. which is txansparent.
It is a further object of the present invention to prepare a deodorant stick composition ha~ing the characteristics described but which has ~ood stability and low staining potential.
Still a further object of the invention is to pro-vide a process ~or preparing deodorant stick compositions of the above character.
It is still an additional ol: ject of this inVention to provide prc~cesses for csntrolling odor in a subjeot by applying to the skin of such subject an e~ective amount of the deodorant stick composition set out in the above objects.
O~her and more detailed objects of this invention will be apparent ~rom the following description and claims.
- The basic backbone of the present deodorant stick compo~itions is provided by the long chain fatty acid soap. This soap is a solid under most ordinary temperatures e.g. below 2SC and is generally an alkali metal or alkali earth me~al soap; the preferred soaps being the sodium soaps.
Any of a variety of long chain fatty acids may form the acid portion of the soap employed in this in~ention.
The only limitation is that i~ forms a solid soap with the a~oresaid metals to enable it to serVe as the backbone ~or the deodorant stick. The fatty acid moiety of the soap will ordinarily be derived ~rom a long chain fatty acid having from 16 to 18 carbon ~toms. The fatty acid moiety of choice is stearic acid and the pre~erred soap is sodium stearate.
The quantity of soap that will be contained in the stick compositions of this in~ention may vaxy somewhat.
Generally, it will constitute from about 5~ to about 10%
by weight based on the total weight of the ~omposition;
with the preferred range being from about 7~ to about 9%
on the same weight basis.
Propylene glycol forms a second component of the present composition. Although this is a hydrophillic material, it appears necessary in order to form an organo-leptically acceptable deodorant stick. In any eVent, an effort is made to minimize the quantity of propylene glycol contained in the stickO Generally, the le~el o propylene glycol will constitute hetween about 20~ to about 6~ 7 70% by weight based on the total weight of the stick compo-sition with the prefexred range being from about 25% to about 40~ on the same weight basis.
Another impOEtant component of the present deodorant stick composition is the antimicrobial agent. The texm "antimicrobial agent" is used herein in its broadest sense and is intended to encompass bacteriostatic agents, bactericidal agents, antimicr~bial fragxances, antiviral agents, fungicidal agents and fungistatic agents. A
number of such agents are known in the prior art which can serve as effective deodorant agents. These include such things as hexachlorophene, trichlorocarbanili~eJ
~riclosan, Dowicil 203, usnic acid, zinc phenolsulfonate, quaternary ammonium compounds, quat~rnary ammonium saccharinate (Onyxide 3300), chlorhexidine, hydagan DEO, zinc ricinoleate, antimicrobial ~ur~ac~ants (lauricidin, Deriphat 160-C), Vitamin E, Grillocin, sodium bicarbonate, sodium polyacrylate, abietic aeid derivati~es, substituted styrene derivatives, tetra~ur~ural alcohol. The material of choice is 5-chloro-2(2,4-dichlorophenoxy)phenol.
This material is also known as Triclosan (CTFA nomenclature) and is available commercially under the trade name Irgasan DP 300 (Ciba-Geigy).
The level of antimicrobial that will be contained in the deodorant stick composition of this invention may also vary somewhat. Usually, this will be in the range of from about 0.05~ to about 5.0% ~y weight based on the total weight of the stick composition. The pxeferred range, however, is ~rom about 0.1% to a~out 0.5~ on the same weight basis.
The major portion o~ the stick composition on a weight basis will generally comprise a hydrophobic ~ehicle.

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This will ordinarily be an oily liquid which will add emolliency to the product. It will also be insoluble in water but will be soluble or dispersible in propylene glycol.
A variety of materials are known in the prior art which may be used in this invention. The materials of choice is a polyoxyproplene(3) ether of a long chain alcohol which is illustrated by PPG-3-myristyl ether (CTFA nomenclature) that is described as having the formula:
where n has an average value of 3.

Other hydrophobic emollients or combinations of emollients may also be employed as the hydrophobic vehicles of the present stick composition. These are selected for their organoleptic characteristics and their ease of removal with a surfactant such as soap. Typical emollients that are useful for the present purposes include non-polar liquids which will ordinarily take the form of a non-volatile oil. Suitable non-volatile oils for this purpose are organic oily liquids which are non-polar in character and have (a) boiling point under atmospheric pressure not lower than about 120°C and (b) a specific gravity between about 0.7 and 1.6 preferably between 0.7 and 1.2. These include such materials as liquid hydro carbons (e.g. mineral oil); fatty acid esters (e.g.
isopropyl myristate, isopropyl palmitate); branched chain fatty acid esters (2-ethyl hexyl palmitate) diesters of dicarboxylic acids (e.g. diisopropyl adipate); polyoxy alkylene glycol esters (e.g. polypropylene glycol 2000 monooleate); propylene glycol diesters of short chain fatty acids (C8-C10) (Neobee M-20); polyoxyethylene esters (polyoxyethylene (4) lauryl ether (Brij 30), polyoxyethylene fatty acids, polyoxypropylene cetyl ether (Procetyl);
higher fatty alcohols (oleyl, hexadecyl, lauryl);
silicone oils (dimethyl polysiloxane 10-1000 centistokes).
The quantity of hydrophobic ~ehicle that will be contained in the deodorant stick composition may vary from about 20% to about 70~ by weight based on the total weight o~ the composition. Best results are obtained when this component comprises between about 55% to about 65~ on the same weight basis.
As indicated above, to obtain a stick of superior clarity and transparency, one would add to the stick composition a relatively small speci~ied guantity of anhydrous ethyl alcohol. Too much or too little ethyl alcohol will a~ect the clarity o~ the stick. The quantity of alcohol added for this purpose is ~rom about 4~ to about 6~ by weight based on the total weight o~ the composition.
Aside ~rom the above described ingredients, a variety of other ingredients may be added to improve the organoleptic, the stability and emolliency characteristic of the product. The limitation put on these materials in accordnace with the present in~ention ic that they should be hydrophobic in natureO These include such things as color agents, perfumes, preservatives, c~loring, sunscreens, anticholinergics, kopical analgesics e.g. methyl nicotinate, camphor, ~enthol, methyl salicylate, eucalyptus oil, hydrocortisone, hydrocortisone acetate, anti~ungal agents, hair grooming and tinting agents, pigments to achie~e pearlescent e~fect, emollients, sur~actants, polishes and abrasives, anti-acne agents, lipstick base, anti-callus agents.
By way of example, mention may be made of the following:
coloring agents D~C YeLlow #10, FDhC ~lue ~1, D&C Yellow #11, D&C Green #6, D&C Red #17; preser~atives methyl paraben, propyl paraben.

~yl~ '7 The deodorant sticks of the invention may be pre-pared in a variety of ways. In a preferxed procedure, the formula weight of propylene glycol and sodium stearate is introduced into a stainless steel manufacturing kettle equipped with a steam jacket, a tight fitting co~er with condenser for alcohol ~umes, and an explosion proo~ propeller type mixer. The agitator is turned on and the temperature of the batch is raised to 170 to 175QF or until the sodium steaxate or soap is dissolved and a clear ~olution results.
The formula weights o~ the antimicrobial agent e.g.
Triclosan and other ingredients e.g. color, alcohol etc.
are added and the mixture is gently mixed until clear.
When the batch cools to 145 ~ 3F (62 + 2C) the fragrance is added and the mixture is gently mixed until clear.
The batch is then filled into the containers and capped immediately.
The following Examples are given to further illustrate the present invention. It is to be understood, however, that the invention is not li~ited thereto. Unless otherwise speci~ied, the percentages are ~iven as percent by weight.

Deodorant Stick (Clear? FN 1775-79 % W/W
Triclosan 0.25 Propylene glycol 27~00 Sodium stearate 8.00 PPG-3 myristyl ether (Witconol APM) 60.72 SD 40 Anhydrous alcohol 4.00 D&C Yellow #10 (1~) 0.03 ~ . In a suitable container combine propylene glycol and sodium stea~ate. Vnder gentle agitation, heat to i7 165-170F and mix until clear solution is obtained.

2. Add PPG-3 myristyl ether, color solutions, Triclosan, cool to 130-140F, add alcohol. ~ently mix until clear.

3. Pour into containers at 142-149 F (61 -65 C) and cap immediately. Note: use gentle agitation in order not to entrap air in the product.
To determine the in vivo deodorant activity of the deodorant stick FN 1775-79, the experiments described below were carried out. In this case, a comparison was made between underarms treated with stick FN 1775-79 and untreated underarms. Ten adults (8 males, 2 females) were used in the study.
Method Prior to initial product application both axillae were washed with soap and water. The test products were then applied to one axilla and the other remained untreated.
This was repeated 24 hours later.
Odor evaluations ollowed by washing and product applicathons were made at 24 hours on the second, the third and the fourth days of the study. Additional observations were made at 6 houxs on the third and fourth day.
Three judges were used for the study. An odor scale of 0-8 was employed for these observations with O
indicating the absence of detectable odor and 8 ~ery strong odor.
Data was e~aluated separately a~ each time period.
A summary of the average odor scores is ~iven in Table I.
The results of the statistical analysis are summarized as follows:
Six Hours after Treatment: The pxoduct FN 1775-~9 was significantly effective (.~1 le~el) in reducing odor.

The level of effectiveness did not dif~er significantly between days or among judges.
~ The product FN 1775-79 was significantly effec~i~e (.01 level) in reducing odor.
The level of effectiveness did not differ signi~icantly among days or judges.
TABLE I
Avera~e Odor Scores for all Three J~d~es Combined Day 2 10(hrs.) V-T
Time T U U-T T
24 3.60 5.73 2.13 .37 Day 3 6 2.50 6.10 3.60 .59 24 2.70 4.73 2.03 .43 ~ 2.80 5.53 2.73 .49 24 2.60 5. 33 2. 73 . 51 ~ P value 6 2.65 5.82 3.17 .54 ~ .001 24 20 97 5. 27 2.30 .44 ~.001 The following Examples are given in tabular form.
These sticks were prepared using a process similar to ~hat described in Example 1.

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Ex. 2 Ex. 3 Ex. 4 FN 1775-60 ~N 1775-~1FN 1775-62 g6 W/W % W/W % W/W

Triclosan -- -- 0.25 Propylene glycol ~ 27.00 Sodium stearate -- -- 8. 00 PPG- 3 Myri styl ether ~ 56. 75 Absolul:e alcohol 6 . 00 12. 00 4 . 00 D~C Yellow #10 (1% sol. ) _ __ __ FD~C Blue # 1 (1~6 sol. ) ---- --~ 1. 50 Stearyl alcohol38. 00 35. 50 --Zinc phenolsulfonate 2. 50 5. 00 --G-2162 2. 00 2. 00 --Ionol CP 0.05 0.05 --Volatile Silicone F-251 48. 95 45. 45 --Perfume 604. 453 (firm) 2. 50 -_ 2. S0 __ 100.00 100.00 100.00 Notes:
1 Polyoxyethylene(25)propylene glycol stearate 2 Butylated hydroxytoluene To determine the in vi~o deodorant activity of the .
clear deodorant stick FN 1775-62, the experiments described below were carried out. In this case, a comparison was made bçtween underarms treated with stick FN 1775-62 and untreated underarms. Twelve adult subjects (10 males and 2 females) were used in the experiment.

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~36~i7 Method:
Following a control (or 24 hr.) evaluation, both axillae were washed with soap and water. The test product was then applied to one axilla and the other remained untreated. Odor evaluations were made at 2, 6 and 24 hours later. The same procedure was repeated the second day.
Four judges were used for the study. An odox scale of 0-8 was employed for these observations with 0 indicating the absence of detectahle odor and 8 very strong odor.
The protocol called for fourteen subjects. One subject was absent and another had consistently low odor scores throughout the whole study period. Therefore, only twelve subjects were used in the analyses.
Data was evaluated separately at each time period.
A summary of the average odor scores is given in Table II.
The results of statistical analysis are summarized below.
Before Treatment: Before pre-treatment wash, there was no significant difference (P-.49) between the average odor scores of the two axillae for the panelists.
Two Hours after Treatment: The product was significantly effective (P ~.01) in reducing odor. The level of effective-ness did not differ significantly between days or among judges.
Six Hours after Treatment: The product was significantly effective (P ~D 01) in reducing odor. The level of effecti~e-ness did not differ significantly between days or among judges.

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- ~2 Twent -four Hours after l'reatment: There was no signifi-cant di~ference (P-.08) between the average treated odor score and the average untreated odor score. The level of effectiveness did not differ significantly between days or among judges.

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~ W/W
Hydrocortisone 0.50 Propylene glycol27.00 PPG-3 Myristyl ether60.43 ~bsolute alcohol 4.00 Cocoline Brown (1% Aq. Sol.) 0.07 Sodium stearate 8.00 100. 00 _26 % W/W
Irgasan DP 300 0.20 Propylene ylycol27.00 Sodium stearate 8.00 Procetyl AWS 60.80 Absolute alcohol 4.00 ~
To test the affect of the presence of rela~ively large quantities of water on the deodorant activity of compositions of the present in~ention, the followin~
compositions were prepared and designated as formulas BK 1778-24 and BK 1778-25 respecti~ely. BK 1778-25 differs from BK 1778-24 only in the fact that the former contains the antibacterial TriclosanO

-- .15 Ingredients ~
Water, deionized21.72 Propylene glycol66.00 Sorbitol solution, 70~ 5.00 Sodium stearate, C-7 (Witco) 7.00 Color D&C Yellow ~10 (1.0% sol.) 0.13 Color FD~C Blue #l (0.1% sol.) 0.15 ~00. 00 Ingredients % W/W
Water, deionized21.47 Propylene glycol66.00 Sorbitol solution, 70~ 5.00 Sodium stearate, C-7 (Witco) 7.00 Triclosan (Irgasan DP 300 Ciba) 0.25 Color D&C Yellow ~10 (1.0% sol.) 0.13 Color FD&C ~lue # 1 (0.1% sol.~ 0.15 100. 00 Materials: ~. Deodorant stick (BK 1778-25) B. Deodorant stick (BK 1778-24) ~ethod:
Following a control (or 24 hr.) evaluation, both axillae were washed with soap and water. Test products were applied according to a randomly pre-assigned product-axilla allocation. Odor evaluations were made at 2, 6 and 24 hours later. The same procedure was repeated the second day.

i'7 Four judges were used for the study. An odor scale of 0-8 was employed ~or these observations with 0 indicating the absence of detectable odor and 8 very strong odor.
Data was evaluated separately at each time period.
A summary of the average odor ~cores i~ given in Table IIlo The results of statistical analysis are summarized below.
Before Trea~ment: Before pre-treatmen~ wash, the difference between the average odor scores o~ ~he A ~ B axillae differed significantly (P=.04) among judges. The difference of these two average odor scores were rated significant at the P-values of .86, .04, .06, and .35 by the four judges respectively.
Two Hours af ~ : There was r.o significant differ-ence (P=.88) between the average odor scor~s of the two products. The B-A values did not differ significantly (.05 level) between days or among judges.
~ : There was no significant differ-ence (P=.81) betwaen the average odor scores of the two productsO The B-A values did not differ significantly (.05 level) between days or among judges.
~ tment: There was hO significant difference (P=.16) between the average odor scores of the two products. The B~A values did not differ significantly (.05 level~ between days or among judges.

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It is clear rom the above that there is no significant difference between in vivo deodorant activity of BK 177B-25 (containing .25~ Triclosan) and BK 1778-24.
Each of these compositions are previously indicated as containing significant ~uantities of water. In contrast to this, in the comparisons given above between the comparable composition of this invention with and without the antibacterial agents, a significant difference in deodorant activity was recorded.
To examine the staining potential for a product representative of the present invention, the stick having the following foxmula and identified as "Code 21" was prepared.

Ingredients % W/W
Triclosan .25 Fragrance 2.50 Propylene glycol 27.00 Sodium stearate 8.00 Polypropylene glycol (3)myristyl ether56.75 Absolute alcohol 4~00 FD&C ~lue #l (.1% sol.) 1.50 ___ 100. 00 The staining potential of this product was avaluated on white cotton T-shirts and blue cotton fabrics.

~6~i'7 ~ 19 -Procedure:
"Hanes" 100% cotton white T-shirts ~nd 100% cotton blue fabric were cut into 6~' x 8" swatches. Test materials were applied e~enly onto each of two 1" x 6" ~trips across the fabric. One gram of li~uid product was pipetted and 0.5 gram o~ solid stick product was spread onto each strip.
Aerosol product was ~pplied by dispensing 1.2 grams of the aerosol can's content onto each strip from a distance of four to six inches. This corresponds to a 2 second spray at a spray rate o 0.6g/sec.
Swatches were placed at 100 F and 80-85% R.H. for 18-24 hours and laundered in a Sears Kenmore ~ea~y Duty Washer, Model #299~1 set at Warm Wash/Warm Rinse (105F
water), wash and 2nd rinse, cotton white settings. The detergent ~anufacturer's directions were followed as closely as possible, which were consistent with AATCC test method 124-1978. On the average, 85 grams (1 cup) of TIDE*detergent were added to a 1.7-2.0 Kg load and 19 gallons (medium setting) o~ water. Depending on load size, the amount of water (machine setting) and amount of de~ergent used was varied to insure AATCC test conditions:
(4.4-4.7 g detergent/gallon ~f wa~er, 42-54 g detergent/
Kg load).
Swatches were dried in a Sears Kenmore Automatic Dryer set at automatic cycle, cotton sturdy setting.
Samples were e~aluated visually for stains by at least two judges. The coding system for degree of stain in this study was as follows:

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Degree of Numerical Stain Value Comments None 0 No stain ohservable Very slight 0.5 Barely perceptible Very slight to Average of very slight slight 0.75 & slight Slight 1.0 Obvious, undesirable but acceptable Slight to moderate 1.5 Borderline, acceptable Moderate 2.0 Unacceptable Moderate to heavy 2.5 Unacceptable Heavy 3.0 Unacceptable In this study, a series of products including product Code 21 were evaluated. The results of these tests are summarized in Tables IV and ~ below.

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TAB (cont'd) (a) Observed data translated into numerical scores 0 = No stain 1 = Slight s~ain, ac~eptable (observable bu~
not objectionable) 2 - Moderate stain (unacceptable) 3 = Heavy stain (unacceptable) All stains are either yellow or yellow and gray, unless indicated:
~G~ Stain is green and yellow (P) Stain is pink Conclusiono For the Code 21 product, the residue buildup was nil and the product is not fabric staining.

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DEGREE OF STAINING (NUMERICAL) ( ) BLUE SWATCHES WITHOUT SEBUM TREATME:Nl' , DAY OF TEST

1.0 1.0 1.0 1.0 1.0 2 0.75 1.0 1~0 1.0 1.0 3 0O5 0.5 1.0 0.5 1.0 7 ~.5 0 0 0 0 12 0 1.0 1.5 1.0 2.0 14 o 2.0 2.~ 1.5 2.0 ~0 16 17 ~.o 2.0 1.5 __ 1~ o 0 0.5 0 0 19 0 0.75 0~5 1.0 0.5 0 0 ~ 0 --.
(a) Observed data translated into numerical scores:
0 = No stain 1 = Slight stain, acceptable (observable but not objectionable) 2 = Moderate stain (unacceptable) 3 = Hea~y stain (unacceptable) ~11 stains are dark oii. stains Conclusion: Code 21 produced acceptably low levels of stain on all fabrics tested.

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~ 24 -Although the invention has been described with reference to specific forms thereof, it will be understood that many changes and modifications may be made without departing from the spirit of this invention.

Claims (7)

1. A non-aqueous transparent deodorant stick composition containing sodium stearate, propylene glycol and at least one antimicrobial agent which functions only as a deodorizing agent;
said stick containing essentially no water; said stick also containing anhydrous ethanol in the range of from about 4% to about 6% by weight based on the total weight of said stick composition; said sodium stearate and propylene glycol being present in sufficient amounts to maintain the physical integrity of said stick; the level of said anhydrous ethanol in said stick serving to insure the clarity and the trans-parency of said stick.

2. A deodorant stick composition according to claim 1 in which said antimicrobial agent is selected from the group consisting of hexachlorophene, trichlorocarbanilide, Triclosan*
Dowicil* 200, usnic acid, zinc phenolsulfonate, quarternary ammonium compounds, chlorhexidine, Hydagan* DEO, zinc ricin-oleate, antimicrobial surfactants, Vitamin E, Grillocin* , sodium bicarbonate, sodium polyacrylate, abietic acid deriva-tives, substituted styrene derivatives and tetrafurfural alcohol.

3. A deodorant stick composition according to claim 2 including an emollient.

4. A deodorant stick composition according to claim 3 in which said emollient is PPG-3 myristyl ether.

5. A deodorant stick composition according to claim 1 or 3 containing Triclosan*.

6. A clear non-aqueous deodorant stick composition having a low anhydrous alcohol content and containing sodium stearate, propylene glycol, PPG-3 myristyl ether and Triclosan*;
said ingredients being present in said stick composition within the following range of weight percentages based on the total weight of said stick composition:

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Triclosan* from about .05% to about 5%
propylene glycol from about 20.0% to about 70%
sodium stearate from about 5.0% to about 10.0%
PPG-3 myristyl ether from about 20.0% to about 70.0%
anhydrous ethanol from about 4% to about 6%.

7. A clear non-aqueous deodorant stick composi-tion having a low anhydrous alcohol content and containing sodium stearate, propylene glycol, PPG-3 myristyl ether and Triclosan*; said ingredients being present in said stick composition within the following range of weight percentages based on the total weight of said stick composition:
Triclosan* from about .10% to about 0.50%
propylene glycol from about 25.0% to about 40.0 sodium stearate from about 7.0% to about 9.0%
PPG-3 myristyl ether from about 55.0% to about 65.0%
anhydrous ethanol from about 4% to about 6%.

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