DK146112B - INSECTICID AGENT FOR USE IN THE FORM OF SHAMPOO - Google Patents

Description

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DIRECTORATE OF THE PATENT AND TRADEMARKET SYSTEM

(21) Patent Application No. 5175/77 (51) Int.CI.3: A 01 N 65/00 (22) Filing Date: 22 Nov 1977 (41) Aim. available: 23 May] 1978 (44) Submitted: 04 Jul983 (86) International Application No: - (30) Priority: 22 Nov 1976 FR 7635121 (71) Applicant: 'S.E.R.T.O.G .; 92200 Neuilly sur Seine, FR.

(72) Inventor: Pierre Muvln; FR, Pierre 'Moreau; FR.

(74) Agent: Hotman-Bang & Boutard_ (54) Insecticidal agent for use in the form of shampoo

The present invention relates to an insecticidal agent for protection against insects and for use in the form of shampoos and particularly intended for eradication and protection against particularly resistant O insects such as lice and fleas.

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Various compounds are known which are capable of destroying this type of insect, such as DDT, hexaehlorocyclohexane or lindane.

“However, these products generally always appear in the form of powders, and their increased toxicity makes them dangerous to use in direct contact with mammalian skin.

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If you take the example of lice and fleas, then these land plagues mainly attack young individuals (children, puppies, kittens) and thus individuals who are particularly sensitive to toxic substances.

On the other hand, certain acidic compounds in liquid form, such as acetic acid, are known to be effective against insects and parasites, especially when these substances are used in solution with a pH close to 2.

However, the liquid products at these pH values noticeably attack the skin of the individuals, so that they have to be used in more dilute solution, which greatly reduces their effect.

From the disclosures of British Patent Nos. 1,001,681 and German Patents Nos. 266,809 and 346,596, it is known to use organic acids such as e.g. acetic acid, valeric acid and phenylacetic acid for protection against insects including in hair care products.

From the disclosures of German Patent No. 834,583, British Pat.

1 001 681 and French usage pattern No. 2 268 513, the use of extracts and essences is known, and the use of natural and / or synthetic camphor is known e.g. from the specification to Belgian Patent No. 491 727.

However, it has been found that in the combination of a wetting agent such as sodium, ammonium or triethanolamine lauric sulfate, preferably sodium lauryl sulfate, at a high concentration, 2-6 volume of acetic acid and 0.5 - 3 volume volume. % natural or synthetic plant extract selected from extracts or essences of cloves, lavender, peppermint, marjoram (origanum L.), rosemary, lime, juniper, lemon, citronella, thyme, pear apple (Datura stramonium), pine, pyrethrum, pyrethrin and the essentials oils from real cinnamon bark or cinnamon leaves obtain a remedy in the form of a so-called shampoo that can be used to kill insects, especially lice, both on humans and animals as well as on lifeless surfaces.

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This shampoo treatment will thus prevent re-infection with the parasites concerned.

The insecticidal agent in question is therefore peculiar to the part of claim 1.

In addition, an insect repellent and wound healing compound, such as natural or synthetic camphor, may be added in volume ratios of between 0.5 and 5%, preferably between 0.5 and 1.5 °.

In order to better understand the benefits and judge the value of the effect of the compositions of the invention, examples of the preparation of mixtures as well as their corresponding use in the main fields of application and the associated treatment methods will be described below.

With each formulation it will be seen that the content of wetting agent is important.

Indeed, it has been surprisingly found that the insecticidal effect of the acetic acid is greatly increased by the addition of wetting agents such as sodium, ammonium or triethanolammonium lauryl sulfate, the classical cation bases or such nonionic compounds commonly used in the field of shampoos. and that the products thus formed have proved remarkably stable.

This observation can be verified by the following tests carried out on moth beetles, ants, eagles, lice and fleas: The products prepared according to the descriptions in the following examples are diluted to triple, then a few drops are applied to each insect, which is held between coverslips so that the insect body is approximately 3/4 impregnated.

It then measures the time needed for the insect to no longer exhibit movement. This time is compared with that obtained with an aqueous acetic acid solution of similar pH.

The results obtained show that the times are on average from 2 to 5 times less using shampoo than is the case with pure acetic acid (20 - 50 seconds instead of 1-3 minutes).

EXAMPLE 1

Hygienic shampoo effective_mod_lus for adults and children

The stated volume ratios are volume ratios.

Wetting agent "Texapon'®N 40 (HENKEL) 75 to 95¾

Synthetic camphor 0.5 to 1.5¾

Citronella 0.5 to 1.5¾

Acetic acid 5 to 6¾ pH 1.8 to 3.5

The procedure for producing the stable shampoo is as follows:

A solution of the wetting agent "ΤΕΧΑΡ0Ν" ® is prepared which is diluted to 30¾ with water using a container equipped with a slow stirrer.

The synthetic camphor and citronella oil are then added in the above quantities and await complete dissolution.

It is then slowly added by means of a decant funnel technical acetic acid, monitoring the pH, e.g. using a pH meter.

The addition of acetic acid is stopped when the pH is close to 3 and the stirring is stopped after 5 minutes.

Test 1: 5 146112

Two children aged 11 and 13, respectively, were treated whose hair contained a substantial accumulation of adult lice and lice eggs, using a shampoo containing 1¾ synthetic camphor, 1 ί ci-tronella oil, 5% acetic acid and 93¾ "TEXAPON" diluted to 30¾ (pH adjusted to 3).

A wash using this shampoo was performed one morning at. 9. The shampoo was used with effect for 15 minutes, after which a water wash was performed.

Examination of the head showed that there were no longer any adult lice and that the amount of lice eggs had decreased.

A new shampoo wash was performed 2, 4 and 6 days later, which meant that no adult lice could be observed, the number of lice eggs was in regular decline.

Re-washing was performed every week. After 3 weeks the lice eggs had completely disappeared.

Test 2:

A young girl of 15 years old had become aware at bathing that lice were swimming around beside her. She was treated every night with a powder containing 0.8¾ of lindane, covered with a cap overnight and then washed with a regular shampoo each morning and saved with a close comb. After 5 days, lice eggs were still present in the hair.

A single shampoo treatment with the product described in Test 1 was sufficient to rid the hair of all parasites and thereby cease the cumbersome and unpleasant treatment.

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Test 3: 6

A little girl of 5 years had lice eggs and had been treated every night for 3 weeks with a powder based on 0.4¾ lindane and 10? » DDT.

She kept these insecticides in her hair overnight using a cap and received a regular shampoo treatment in the morning followed by a close-comb rescue.

This little blonde girl had a particularly fine hair, and the numerous lice eggs were very well stuck in her hair.

An initial treatment with the product mentioned in test 1 yielded only a partial result. Two more treatments were needed with the product to achieve complete removal of the lice eggs.

EXAMPLE 2

Treatment_of_lopper, lice and_blood mites in dogs

A shampoo prepared as in Example 1 was used containing 6¾ acetic acid, 1.5¾ citronella oil and 1.5¾ clove oil and 91¾ "TEXAPON" diluted to 30¾ (pH adjusted to 2).

An adult badger dog treated with fleas was treated.

A wash with a shampoo formulated for veterinary use was performed as indicated above one morning at. 8. At 12 o'clock the dog had no more fleas and was not re-infested within 3 days despite unfavorable surroundings.

A maintenance treatment which consisted of atomizing a liquid composed of a solution of thyme extract 25 µl. vinegar 73¾ and citronella oil 2¾ avoided any return of parasites until the environment (rooms and textiles) could be completely disinfected.

In general, the method of application of the products according to the invention can be described as follows: A shampoo treatment of the parts to be treated is carried out by means of the mixtures described above, the products are allowed to operate for a period of time which is usually between 1 and 10. minutes for living beings and between 6 and 20 minutes for objects.

Rinse thoroughly, which flushes the acetic acid as well as the insects and parasites.

After washing, it is found that products that are repellent to the insects have remained in sufficient quantity to protect against new infections.

However, in many cases, one is interested in continuing the treatment with consecutive but separate washing treatments until the larvae have completely disappeared, as well as in applying a maintenance treatment consisting of spraying or atomizing various essences of insecticidal or parasitic killing products. , as indicated above, with or without camphor, but preferably without acetic acid, viz. citronella oil, clove oil, lavender oil, peppermint oil, marjoram oil, rosemary oil, linden oil, juniper oil, lemon oil, thyme oil, baby apple oil (Datura stramonium), pyrethrum extract or real cinnamon oil.

These sprays permanently protect the treated surfaces between each shampoo treatment.

In addition, the insecticide effect of a shampoo similar to that used in Test 1 of Example 1 has been tested compared to a powdered lindane mixture containing 1.5% by weight as follows:. 8 1. Test on adult lice; In a small bowl, place 5 cm 2 of pure shampoo, then put down 5 lice (pediculus humanus). Death occurs immediately. After being convinced of this result, they performed a second experiment, leaving the lice in the shampoo for only 10 seconds, then removing them with a wooden stick. They were placed under a magnifying glass and found that the lice were completely dead.

Similarly, food shampoo diluted to 50% was then continued to 25% for the purpose of approaching application concentrations, which vary between 25 and 100%.

The killing of the lice is slower with these two dilutions, and the attempt to remove the lice shows that after 30 seconds the lice do not return to life.

The same experiments have been performed on the pharyngeal phthirius pubis with the same mortality rate of 100 after 30 seconds. These experiments have been repeated in comparison with a powdered linden mixture containing 1.5%.

The following table summarizes the results found, using a shampoo formulation R.S. 206 consisting of (by weight):

Acetic acid 4.54%

Camphor 0.76%

NaCl 0.20%

Citronella 0.76% "Texapon" ® 35.00%

Water 58.74% 100.00% 9 U6112

Experiments with pediculus humanus adult individuals:

After 10 After 30 After 2 Mortality Percentage_seconds_seconds_hours R.S. 206 pure 100 * 100¾ 100¾ R.S. 206 diluted to 50¾ 20¾ 100¾ 100¾ R.S. 206 - diluted to 25¾ 0¾ 100¾ 100¾

Lindan powder with 1.5¾ 0¾ 0¾ 50¾

The same experiment has been conducted with adult individuals of phthirius pubis with identical results.

EXAMPLE 3

Various formulations were tested on flies and lice. When testing on flies, 10 flies were placed in a box of dimensions 20 x 15 x 10 cm and made of mosquito net over small pieces of wood. Ca. 0.5 cm 2 was sprayed on the flies. The number of killed flies was calculated after 2 hours.

When testing on lice, 10 lice were placed on a glass plate (so-called Petri plate) and they remained for a period of approx. 10 seconds covered with a drop of the liquid to be tested and then rinsed with water using a pipette. The lice killed after 2 hours were counted.

The formulations tested had the following composition:

Formulation 1.1: Acetic acid: 4.5 *, the rest water.

Formulation 1.2: "Texapon" ® extract N 40 diluted to 30? 0 concentration: 94 *, water: 6¾.

Formulation 1.3: Citronella extract: 1.5 *, the rest water.

Formulation 1.4: Acetic acid: 4.5 µl, citronella extract: 1.5¾, the rest water.

Formulation 1.5: Acetic acid: 4.5 *, citronella extract: 1.5 *, "Texapon" ® extract N 40 diluted to 30 * concentration: 94 *; pH adjusted to 2.7.

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Formulation 1.7: Analogous to Formulation 1.6, however, the pH was raised to 5.5 by the addition of sodium hydroxide.

Formulation 1.8: Acetic acid: 9S, citronella: 1.5? Ό, the remainder consisting of "Texapon" ® extract N 40 diluted to 30Sa concentration; pH = 1.

In tolerance testing, a small amount of each test formulation was applied to the skin of a rabbit or human. Regarding the rabbit, pink staining or sensitivity reaction was observed after application, rating the pink stain or sensitivity as either "medium" or "poor". With respect to tolerance of the tested formulations on human skin, the arm was used, and there was a slight burning sensation in connection with formulation 1.8.

The following table describes the tests described above.

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In this clinical trial, a formulation designated as R.S. 208 having the following composition:

Acetic acid 4.57 g

Sodium Chloride 4.87 g of "Texapon" N 40 36.55 g

Marjoram oil (origanum) 0.76 g of purified water up to 100 g

The shampoo in question was used in the treatment of 14 different families in an average urban settlement, with one or more of the family members, especially among the children, being attacked by lice.

In all cases, the use of shampoo according to the previously stated guidelines led to the discontinuation of the infection and no adverse effects were noted, as the irritation was limited to a few accidental eye springs which were quickly remedied using clean water.

The product obtained has been found to be more active than a 1.5 Lind Lindan blend.

Lindan mixtures of 0.4 and 0.8¾ have an effect insufficient to be used as a basis of comparison.

In addition, the bacteriostatic effect of products of the invention has been found, and this has been done, although they do not contain any of the commonly used bactericidal compounds, such as methyl paraoxybenzoate, but various experiments have shown that no bacteria develop in the products in the pure state or diluted to 50¾.

The study carried out to find that the mixture was free of bacteria has been continued in view of the interesting results obtained.

The study method used was as follows with shampoo prepared analogously to Example 1: 1. Inoculation on plain gelatin 2. Incubation in oven at 37 ° C for 48 hours and then for 7 days. results:

After 48 hours After 7 days

Shampoo, clean 0 colonies 0 colonies

Shampoo, diluted to 50% 0 colonies 0 colonies

After inoculation with Escherichia coli:

Shampoo, clean 0 colonies 0 colonies

Shampoo, diluted to 50% 0 colonies 0 colonies

The toxicities observed can vary considerably, which is reinforced by the fact that acetic acid associated synergistically with a wetting agent gives this an increased insecticidal ability, although the toxicity remains within limits fully compatible with the use of the product in contact with sensitive skin layers.

The oral toxicity determined by administering shampoo prepared in accordance with Example 1 to male mice of the species River and having a mean body weight of 25 g shows a maximum tolerated dose of 24 ml / kg and for the lethal dose 100 a value of 40 ml / kg.

The results obtained do not allow the calculation of a light dose 50.

In comparison, the lethal dose 50 for lindane as determined by aqueous mixtures administered orally to mice is approx. 300 mg / kg.