WO2012102686A1

WO2012102686A1 - A biochemical plant protection product and plant growth regulator based on milk thistle (silybum marianum)

Info

Publication number: WO2012102686A1
Application number: PCT/TR2012/000012
Authority: WO
Inventors: Evren BULAY
Original assignee: Boyut Dis Ticaret Insaat Ve Madencilik Sanayi Anonim Sirketi
Priority date: 2011-01-24
Filing date: 2012-01-24
Publication date: 2012-08-02
Also published as: TR201100629A2

Abstract

The invention is related to a new source of plant origin to produce a biochemical plant protection product and plant growth regulator, and to a process ensuring that the relevant product is obtained from such a source. The subject-matter source of plant origin is Silybum Marianum and covers the roots, seeds, leaves and stems of the said plant. The above-written parts of the plant are dried for the product obtained from the said plant and prepared by extracts. Then they are ground as fine as possible. After being extracted by ethanol and polysorbate 80 respectively under suitable medium end conditions, a biochemical plant protection product and plant growth regulator is obtained.

Description

A BIOCHEMICAL PLANT PROTECTION PRODUCT AND PLANT GROWTH REGULATOR BASED ON MILK THISTLE (SILYBUM MARIANUM)

The invention is related to a new source of plant origin to produce a biochemical plant protection product and plant growth regulator, and to a process ensuring that the relevant product is obtained from such a source.

As a result of R&D studies related to the control methods of pests, mites, nematodes, viruses, bacteria, fungi and weeds, which cause significant agricultural losses, even to limit agricultural production in some cases, many different plant protection products have been developed in order to protect plants against harmful organisms or to prevent such organisms from being harmful, to affect life functions of plants, to eliminate undesired plants or plant sections, to control or prevent such undesired growth of plants.

The invention is related to a new source of plant origin to produce a biochemical plant protection product and plant growth regulator, and to a process ensuring that the relevant product is obtained from such a source. The subject - matter of plant origin is plant Silybum Marianum.

Silybum Marianum, also known as milk thistle plant or thistle, is a 30 to 100 cm - tall plant. Its leaves are emarginated and pricky. It is also known as thistle. Its flowers are purple while its seeds are dark colored. Its leaves, stems, flowers and seeds have been used for various purposes for years. Today, the seeds of this plant is mostly used for therapeutic purposes in liver diseases. Its seeds contain oil, starch, tannin and flavano-lignan derivative compounds.

Silybum Marianum grows commonly in Mediterraneam countries, southern Russia and northern Africa. However it is frequently found in Aegean and Marmara regions in our country. The said plant is capable of accommodating to any kind of soil, but it requires rich humus to grow to the desired tallness. To reproduce the plant, its seeds should be sown in pots at the end of spring or in fall, to be transplanted later on. In warm climate, it can grow from its self - fallen seeds as well. It can be started to grow at the beginning of spring in greenhouses or within vegetation cover.

Though only the seeds of Silybum Marianum are used in general applications, dried roots, stems and leaves of the said plant may be used in our invention together with its seeds.

The process consists of the following steps:

1 ) Subject Silybum Marianum to an organic solvent (ethanol) extraction.

2) Concentrate the obtained extract by distillation .

3) Extract the remaining raw material (Silybum Marianum) again with Polysorbate 80.

4) Remove the remaining raw material (sliybum marianum) by filtration and mix remaining liquid (filtrate) with the first extract.

5) Add other co-formulants to the mixture obtained.

Thus, a biochemical plant protection product and plant growth regulator are obtained from Silybum Marianum.

Silybum Marianum stated in Article 1 above means the seeds, dried stems, roots and leaves of the said plant. After drying, such parts are ground before extraction operation.

8 liters of ethanol should be used for 1 kg of dried and ground Silybum Marianum for the first extraction operation.

During distillation stated in the second step, at least 90 % by volume of the organic solvent should be recovered. Vacuum distillation method can be used for this operation. Then, the solvent remained in the extract should be completely removed by evaporation or spray drying method. A dried extract of 5 to 6 % may be obtained from 1 kg of Silybum Marianum, through the above- said extraction.

During extraction, denaturated ethanol may be used, that is, it is not necessary to use pure ethanol. When using denaturated ethanol, the residues with phytotoxic effects should be prevented from being concentrated in the final product. Extraction should be conducted in a continuously stirred boiler at room temperature for 3 hours as a minimum.

Before passing to the second extraction operation, ethanol residues on the material should be removed as much as possible by centrifugal or compactor and the liquid obtained meanwhile should be added to the extract before starting distillation.

Polysorbate 80 should be used for the second extraction operation. 6 liters of Polysorbate 80 should be used for 1 kg of dried Silybum Marianum powder used at the beginning of the process.

The said extraction should be performed by stirring continuously at room temperature for 4 hours as a minimum.

After the second extraction, the remaining solid substances should be removed by filtering. Residues of Polysorbate 80 on the remaining solid substances should be removed by centrifuging or pressing and the liquid obtained from here should be added to the liquid obtained from the second extraction operation.

As a final operation, the first and second extracts obtained should be filtered separately, mixed together with suitable co-formulant, completed to 10 liters (by adding distilled water), bottled and made ready for consumption.

The above-said invention is a proses generally related to the manufacture of biochemical agricultural pesticides and plant growth regulators. The said invention is a plant protection product and plant growth regulator, prepared with the extracts specially obtained from Silybum Marianum. Silybum Marianum, used in this invention covers the roots, seeds, leaves and stems of the said plant. Before preparing the powder to be subject to the extraction operation, the above-mentioned parts of the plant should be dried and then should be ground as fine as possible.

Two examples of the application of the product, which is our invention, to the industry are given below. Our examples show the importance of our invented product, both as a plant protection product and plant growth regulator, in growing greenhouse tomatoes.

Our final product will be referred to as Silymar herein after in the following examples. Example 1 : Application as a biochemical plant protection product:

Powdery Mildew in greenhouse tomatoes.

Application of Silymar: After symptoms have been seen, total 4 application at 7-day intervals.

Application of TOPAS 100 EC: After symptoms have been seen, total 2 applications at 14-day interval.

Character Recurrence Disease Disease % Effect %

Index

Silymar 1 0,360 7,20 61 ,29

25 ml/100L water 2 0,310 6,20 70,19

3 0,300 6,00 66,29

4 0,390 7,80 67,23

AVERAGE 0,340 6,80 66,25

AVERAGE 0,263 5,45 73,97

Silymar 1 0,100 2,00 89,25

100 ml/100L water 2 0,160 3,20 84,62

3 0,100 2,00 88,76

4 0,160 3,20 86,55

AVERAGE 0,130 2,60 87,30 TOPAS 100 EC 1 0,150 3,00 83,37

(Penconazole 100 2 0,140 2,80 86,54

g/1 L) 3 0,1 10 2,20 87,64

25 ml/100L Water 4 0,210 4,20 82,35

AVERAGE 0,153 3,05 85,10

Control 1 0,930 22,60

2 1 ,040 25,80

3 0,890 24,80

4 1 ,190 27,80

AVERAGE 1 ,013 25,25

Example 2 : Usage as a biochemical plant growth regulator.

Fertilization program in greenhouse tomatoes:

Comparison between the results of a standard fertilization program and a fertilizer + Silymar mixture fertilization program.

A dose of 50 mL Silymar / 100 L water was added to the standard foliar fertilizer applications and the difference from those fertilizers used by itself was observed.

Season-end comparison between yields (kg per decare).

Producer standard (foliar fertilizer used by itself): 12400 kg / da Producer standard + Silymar (adding Silymar to every foliar fertilizer application): 14800 kg / da.

This shows a yield increase of about 20 %, which is very important for the producer.

Claims

1. The invention is related to a new source of plant origin to produce a biochemical plant protection product and plant growth regulator, and to a process ensuring that the relevant product is obtained from such a source, whose characteristic is that the said source of plant origin is Silybum Marianum and the subject - matter product is obtained from the said plant by the following operations in order:

- Subject the said Silybum Marianum to an organic solvent extraction,

- Concentrate the obtained extract,

- Post-extraction, subject the remaining Silybum Marianum again to an extraction operation with Polysorbate 80,

- Remove solid substance from the second extract and mix the remaining liquid with the first extract, after filtration

- Add other co-formulant to the mixture obtained.

2. The process according to Claim 1 and it is characterized in that, while subjecting Silybum Marianum to an organic solvent extraction, which is the first step of the process, the organic solvent should be ethanol and for such an extraction operation, 8 liters of ethanol should be used for 1 kg of dried Silybum Marianum consisting of fine ground of seeds, roots and leaves of dried Silybum Marianum.

3. The process according to Claims 1 and 2 and it is characterized in that, in the second step of the process related to obtaining the subject-matter product, the extraction obtained in the first step should be concentrated in a continuously stirred boiler at room temperature for 3 hours as a minimum, by distillation method and that at least 90 % o fthe organic solvent by volume should be recovered.

4. The process according to Claims 1 to 3 and it is characterized in that, in the second stage extraction operation

- Polysorbate 80 should be used as an organic solvent at this stage, - Before passing to the second extraction operation, ethanol residues on the material should be removed as much as possible by centrifugal or compactor,

- Silybum Marianum remaining from the first extraction should be subject to an extraction operation with Polysorbate 80, by continuosly stirring at room temperature for 4 hours as a minimum,

- 6 liters of Polysorbate 80 should be used for 1 kg of dried Silybum Marianum powder used at the beginning of the process.

5. The process according to Claims 1 to 4 and it is characterized in that, in mixing the obtained extract after filtering, with the first extract

- Solid substances remaining from the second stage extraction operation should be filtered and removed,

- Polysorbate 80 remaining on solid substance residues should be removed by centrifuging or pressing,

- The liquid obtained should be added to the liquid obtained from the second extraction operation.

6. The process according to Claims 1 to 4 and it is characterized in that, in the final operation for the process to produce a biochemical plant protection product plant growth regulator, the mixture obtained from the first and second extracts are filtered separately and mixed with suitable co-formulant, and then should be packed.