WO2008032958A1

WO2008032958A1 - Beverage composition using sea weed fusiforme and onion for the prevention of hypertension

Info

Publication number: WO2008032958A1
Application number: PCT/KR2007/004357
Authority: WO
Inventors: Kwang-Soo Kim
Original assignee: Kwang-Soo Kim
Priority date: 2006-09-11
Filing date: 2007-09-10
Publication date: 2008-03-20
Also published as: KR20060111422A; KR100758930B1

Abstract

Disclosed herein is a beverage composition for the prevention of hypertension, comprising Hizikia fusiforme and Allium cepa. The disclosed beverage composition comprises 100 parts by weight of Hizikia fusiforme, 50-80 parts by weight of Allium cepa, 1-5 parts by weight of Acanthopanax senticosus, 1-5 parts by weight of Ly ciifructus, 1-5 parts by weight of Cassia tora extract and 1-5 parts by weight of vinegar. The disclosed beverage composition shows a high an¬ giotensin I-converting enzyme that indicates anti-hypertensive activity, and thus the beverage composition is effective in preventing hypertension.

Description

BEVERAGE COMPOSITION USING SEA WEED FUSIFORME AND ONION FOR THE PREVENTION OF HYPERTENSION

Technical Field

[1] The present invention relates to a beverage composition for the prevention of hypertension, comprising Hizikia fusiforme and Allium cepa, and more particularly to a beverage composition for the prevention of hypertension, comprising Hizikia fusiforme , Allium cepa, Acanthopanax senticosus, Lyciifructus, Cassia tora extract and vinegar. Background Art

[2] Hypertension that is a vascular disease is one of typical adult diseases.

[3] With respect to hypertension, when the blood supply to the kidneys is impaired, enzyme rennin is produced, which acts on angiotensinogen to produce angiotensin I, which is then converted to angiotensin II by angiotensin-I converting enzyme (ACE). The angiotensin II causes direct vasoconstriction and accelerates the secretion of aldosterone to cause sodium and water retention, thus increasing blood pressure.

[4] ACE inhibitory activity exhibits blood pressure lowering effects by inhibiting the conversion of angiotensin I to angiotensin II.

[5] The use of ACE inhibitors having such activity enables hypertension to be effectively prevented and treated, and studies on the ACE inhibitors have recently been actively conducted.

[6] Meanwhile, Hizikia fusiforme is a seaweed belonging to the family Sargassaceae. It is known that Hizikia fusiforme is rich in minerals, including calcium, iodine and iron, and thus it prevents angiosclerosis, makes teeth healthy and promotes hair growth, when it is commonly ingested. Also, it is known to have the effect of making fetal bone strong, when it is ingested into pregnant women. In addition, it is known to have excellent effects against hyperlipidemia and arteriosclerosis.

[7] Recently, there have been many attempts to use Hizikia fusiforme, having such known effects, in food in various ways.

[8] Korean Patent Registration No. 10-0277168 (entitled "Method for preparing processed Hizikia fusiforme food and processed Hizikia fusiforme food prepared thereby") discloses processed food, such as canned Hizikia fusiforme, which is prepared by adding protein sources, such as dried anchovies and beans, to Hizikia fusiforme, adjusting the mixture to acidic pH, and sterilizing the pH-adjusted mixture at low temperature for a short time.

[9] Korean Patent Laid-Open Publication No. 1999-015783 (entitled "Method for preparing Hizikia fusiforme beverage based on Hizikia fusiforme extract") discloses a Hizikia fusiforme beverage, which is prepared by subjecting Hizikia fusiforme to water immersion, washing, extraction and separation to prepare a first extract, adding alkaline solution to the residue remaining after centrifugation, chopped the residue solution finely, extracting and separating the chopped material to prepare a second extract, mixing the extracts with each other, and adding saccharides and citric acid to the extract mixture.

[10] Allium cepa (onion) is a biennial herbaceous plant belonging to the family

Liliaceae. It is known that Allium cepa is rich in minerals, including calcium and phosphoric acid, together with various vitamins, and thus have the effect of removing harmful substances from blood. Also, it is known to have excellent effects on the prevention and treatment of hypertension.

[11] Korean Patent Laid-Open Publication No. 1996-0040210 (entitled "Method for preparing onion beverage") discloses a method for preparing an onion beverage, comprising: peeling, washing and quartering raw onion, heating the onion pieces in hot water at 80 ⁰C for 20 minutes, chopping the heated onion, stirring the chopped onion together with viscozyme to increase the enzymatic activity of the onion, pressing the stirred onion with a press, adding citron juice, citric acid, fructose, sorbitol and stevioside to the pressed onion, allowing the mixture to stand at low temperature for 2 days, filtering the supernatant through diatomaceous earth to obtain onion juice, adding lemon and vitamins to the onion juice, sterilizing and cooling the lemon-added onion juice, and sealing the cooled onion juice using a capping means.

[12] However, studies on beverage compositions, which contain, as a main component,

Hizikia fusiforme ox Allium cepa, known to have an excellent effect against arteriosclerosis, hypertension and the like as described above, and which have a better taste and flavor and, at the same time, shows an excellent effect on the prevention of hypertension, are still insufficient. Disclosure of Invention Technical Problem

[13] It is an object of the present invention to provide a beverage composition for the prevention of hypertension, which comprises, as main components, Hizikia fusiforme and Allium cepa, which are natural plants known to have a good effect against hypertension, as well as a preparation method thereof. Technical Solution

[14] To achieve the above object, the present invention provides a beverage composition for the prevention of hypertension, comprising 100 parts by weight of Hizikia fusiforme, 50-80 parts by weight of Allium cepa, 1-5 parts by weight of Acanthopanax senticosus, 1-5 parts by weight of Ly ciifructus, 1-5 parts by weight of Cassia tora extract and 1-5 parts by weight of vinegar.

[15] The beverage composition of the present invention is prepared through a method comprising the steps of: (1) preparing materials; (2) mixing 100 parts by weight of Hizikia fusiforme with 50-80 parts by weight of Allium cepa, 1-5 parts by weight of Acanthopanax senticosus and 1-5 parts by weight of Ly cii fructus; (3) adding loess water to the mixture in an amount of 6 liters per kg of Hizikia fusiforme, heating the mixture solution to 100 ⁰C and additionally heating the heated mixture solution for 1-2 hours; (4) filtering the heated mixture of step (3); (5) heating loess water, adding the heated loess water to Cassia tora in an amount of 2 liters per 10 g of Cassia tora, extracting the Cassia tora in the heated loess water for 10-20 minutes, and then filtering the extract, thus preparing Cassia tora extract; and (6) adding, based on 100 parts by weight of the Hizikia fusiforme of step (2), 1-5 parts by weight of the Cassia tora extract and 1-5 parts by weight of vinegar to the filtrate of step (4).

[16] The present inventors have conducted many studies to develop a beverage composition which can be conveniently drunk for the purpose of preventing hypertension and, as a result, have found that a beverage composition prepared using Hizikia fusiforme and Allium cepa has an excellent activity of inhibiting the angiotensin I-converting enzyme.

[17] Hizikia fusiforme used in the present invention is a seaweed belonging to the family Sargassaceae, and is rich in minerals, including calcium, iodine and iron. The dietary fiber content thereof is 2.5-fold higher than that of cucumbers and is higher than that of apples or pears. Recently, it was known to have an effect against effects against hyperlipidemia and arteriosclerosis.

[18] Allium cepa used in the present invention is a biennial herbaceous plant of the family Liliaceae. It is known that Allium cepa is rich in minerals, including calcium and phosphoric acid, together with various vitamins, and thus has the effect of removing harmful substances from blood.

[19] Also, it is known that Allium cepa removes unnecessary fat and cholesterol from blood, lowers the viscosity of blood to make blood non-sticky, runnable and clear, has an excellent effect of lowering blood pressure, and thus shows excellent effects on the prevention and treatment of hypertension.

[20] The present inventors have prepared a beverage composition for the prevention of hypertension using Hizikia fusiforme and Allium cepα, known to have an excellent anti-hypertension activity as described above, together with herbal medicinal materials, which are compatible with Hizikia fusiforme and Allium cepa to improve the taste and flavor of the composition and can further increase the anti-hypertension activity of the composition, thereby completing the present invention.

[21] Specifically, the Chinese medicinal materials used together with Hizikia fusiforme and Allium cepa in the present invention are Acanthopanax senticosus, Lycii fructus and Cassia tora.

[22] Acanthopanax senticosus contains anthoside B. D (lignan glycoside) as a main component, water-soluble glycosides serving to increase immunogenicity, together with various glycosides, and is rich in vitamins, such as vitamins B and C, and minerals, such as cobalt and manganese. Also, it is known to have excellent pharmacological effects such as a cardiotonic effect.

[23] Lycii fructus is the fruit of Lycium chinense, which contains proteins, fats, saccharides, calcium, phosphorus, iron, betaine, rutin, vitamins A, Bl, B2 and C, etc. It is known that Lycii fructus is rapidly absorbed in vivo, is used as a tonic or an antipyretic in Chinese medicine and has pharmacological effects, such as liver protection action, cholesterol lowering action, blood pressure and blood glucose lowering action, etc.

[24] Cassia tora is an herbal medicinal material, which contains anthraquinone derivatives, and thus has tonic, diuretic and anti-hypertensive effects, as well as an effect for a weak stomach. Also, it is known to strengthen the liver and the kidneys and assist in making complexion better.

[25] The inventive beverage composition for the prevention of hypertension is prepared in the following manner using the above-described materials.

[26] First, Hizikia fusiforme collected from clean areas is washed 8-10 times with purified water, until salts in Hizikia fusiforme is removed. The washed Hizikia fusiforme is immersed in water for 24-72 hours to remove salts, before use in the preparation of the inventive composition.

[27] Allium cepa is peeled and washed several times with water before use. Allium cepa is preferably used in an amount of 50-80 parts by weight, and most preferably 75 parts by weight, based on 100 parts by weight of Hizikia fusiforme.

[28] Also, in the present invention, Acanthopanax senticosus is preferably used in an amount of 1-5 parts by weight, and most preferably 1.5 parts by weight, based on 100 parts by weight of Hizikia fusiforme.

[29] In the present invention, Lycii fructus is preferably used in an amount of 1-5 parts by weight, and most preferably 1 part by weight, based on 100 parts by weight of Hizikia fusiforme .

[30] Moreover, Cassia tora in the present invention is used in the form of extract, and the Cassia tora is prepared by heating water, preferably loess water (Jijang-soo), cooling the heated water to a temperature of 70-80 ⁰C, extracting Cassia tora in the heated water for 10-30 minutes, and then filtering the extract.

[31] The Cassia tora thus prepared is preferably used in an amount of 1-5 parts by weight based on 100 parts by weight of Hizikia fusiforme. [32] In addition, vinegar is used in an amount of 1-5 parts by weight based on 100 parts by weight of Hizikia fusiforme in order to further increase the taste and flavor of the beverage composition. [33] The inventive beverage composition prepared according to the above-described method was measured for angiotensin I-converting enzyme (ACE) inhibitory activity that indicates anti-hypertensive activity. As a result, it could be seen that the inventive beverage composition had excellent ACE inhibitory activity, suggesting that the inventive beverage composition had anti-hypertensive activity (see Table 1). [34] The inventive beverage composition including Hizikia fusiforme and Allium cepa is a beverage composition for the prevention of hypertension, which has an excellent taste and flavor and, at the same time, can be simply and conveniently drunk. [35] Hereinafter, a process of preparing the inventive beverage composition for the prevention of hypertension using Hizikia fusiforme and Allium cepa will be described in further detail. [36] <Process of preparing hypertension-preventing beverage composition using Hizikia fusiforme and Allium cepa> [37] 1. Step 1: Preparation of materials

[38] Hizikia fusiforme is washed 8-10 times with purified water, until salts are removed.

Then, it is immersed in water for 24-72 hours to remove salts. [39] Allium cepa is peeled, washed and dried.

[40] Also, Acanthopanax senticosus, Lyciifructus, Cassia tora, vinegar and loess water are prepared.

[41] 2. Step 2: Mixing

[42] 100 parts by weight of Hizikia fusiforme, 50-80 parts by weight of Allium cepa, 1-5 parts by weight of Acanthopanax senticosus and 1-5 parts by weight Lyciifructus, prepared in step 1, are mixed with each other. [43] 3. Step 3: Heating

[44] Loess water is added to the mixture of step 2 in an amount of 6 liters per kg of

Hizikia fusiforme , and the mixture solution is heated to 100 ⁰C, and additionally heated for 1-2 hours.

[45] 4. Step 4: Filtration

[46] The mixture heated in step 3 is filtered through, for example, a fine sieve.

[47] 5. Step 5: Preparation of Cassia tora extract

[48] Loess water is heated.

[49] 10 g of Cassia tora is added to 2 liters of the heated loess water and extracted for

10-20 minutes, followed by filtration, thus preparing a Cassia tora extract. [50] 6. Step 6: Preparation of beverage composition

[51] The Cassia tora extract prepared in step 5 is added to the filtrate of step 4 in an amount of 1-5 parts by weight based on 100 parts by weight of Hizikia fusiforme, and vinegar is added thereto in an amount of 1-5 parts by weight based on 100 parts by weight of Hizikia fusiforme, thus preparing the beverage composition of the present invention.

Advantageous Effects

[52] According to the present invention, there is provided a method for preparing a beverage composition, which contains Hizikia fusiforme and Allium cepa as main components, together with Chinese medicinal materials, including Acanthopanax senticosus, Lycii fructus and Cassia tora. [53] Also, according to the present invention, there is provided a beverage composition for the prevention of hypertension, which has an excellent anti-hypertensive effect.

Best Mode for Carrying Out the Invention [54] Hereinafter, the inventive beverage composition containing Hizikia fusiforme and

Allium cepa will be described in further detail with examples and test examples, but the scope of the present invention is not limited to these examples. [55] Example 1: Preparation 1 of beverage composition Hizikia fusiforme and Allium cepa [56] 2 kg of Hizikia fusiforme, collected in Jeju, Korea, was washed 10 times with drinking water, until salts were removed. Then, the washed Hizikia fusiforme was immersed in water for 72 hours to remove salts. [57] 1.5 kg of Allium cepa was peeled, washed and then dried.

[58] To the prepared Hizikia fusiforme and Allium cepα, 30 g of Ac αnthopαnαx senticosus and 20 g of Lycii fructus were added, to which 12 liters of loess water was added. The mixture solution was heated to 100 ⁰C, and then additionally heated for 1 hour and 30 minutes at a temperature of 100 ⁰C. Then, the heated mixture was filtered through a fine sieve and cooled. [59] Meanwhile, a Cassia tora extract was prepared in the following manner. 4 liters of loess water was heated to 100 ⁰C, and then cooled to a temperature of 70-80 ⁰C. 20 g of

Cassia tora was added and extracted in the hot loess water for 20 minutes, followed by filtration, thus preparing a Cassia tora extract. [60] 60 g of the Cassia tora extract was added to the above-prepared filtrate, and 60 g of brown rice vinegar was added thereto, thus preparing the beverage composition of the present invention.

Mode for the Invention [61] Example 2: Preparation 2 of beverage composition Hizikia fusiforme and Allium cepa [62] 2 kg of Hizikia fusiforme, collected in Jeju, Korea, was washed 8 times with drinking water, until salts were removed. Then, the washed Hizikia fusiforme was immersed in water for 24 hours to remove salts. [63] 1 kg of Allium cepa was peeled, washed and then dried.

[64] To the prepared Hizikia fusiforme and Allium cepa, 20 g of Ac anthopanax senticosus and 20 g of Lycii fructus were added, to which 12 liters of loess water was added. The mixture solution was heated to 100 ⁰C, and then additionally heated for 1 hour at a temperature of 100 ⁰C. Then, the heated mixture was filtered through a fine sieve and cooled. [65] Meanwhile, a Cassia tora extract was prepared in the following manner. 2 liters of loess water was heated to 100 ⁰C, and then cooled to a temperature of 80 ⁰C. 10 g of

Cassia tora was added and extracted in the hot loess water for 10 minutes, followed by filtration, thus preparing a Cassia tora extract. [66] 20 g of the Cassia tora extract was added to the above-prepared filtrate, and 20 g of brown rice vinegar was added thereto, thus preparing the beverage composition of the present invention. [67] Example 3: Preparation 3 of beverage composition Hizikia fusiforme and Allium cepa [68] 2 kg of Hizikia fusiforme, collected in Jeju, Korea, was washed 10 times with drinking water, until salts were removed. Then, the washed Hizikia fusiforme was immersed in water for 72 hours to remove salts. [69] 1.6 kg of Allium cepa was peeled, washed and then dried.

[70] To the prepared Hizikia fusiforme and Allium cepa, 100 g of Ac anthopanax senticosus and 100 g of Lycii fructus were added, to which 12 liters of loess water was added. The mixture solution was heated to 100 ⁰C, and then additionally heated for 2 hours at a temperature of 100 ⁰C. Then, the heated mixture was filtered through a fine sieve and cooled. [71] Meanwhile, a Cassia tora extract was prepared in the following manner. 2 liters of loess water was heated to 100 ⁰C, and then cooled to a temperature of 70 ⁰C. 10 g of

Cassia tora was added and extracted in the hot loess water for 30 minutes, followed by filtration, thus preparing a Cassia tora extract. [72] 100 g of the Cassia tora extract was added to the above-prepared filtrate, and 100 g of brown rice vinegar was added thereto, thus preparing the beverage composition of the present invention. [73] Comparative Example 1: Preparation of beverage composition containing Allium cepa [74] A beverage composition was prepared in the same manner as in Example 1 of the present invention, except that Hizikia fusiforme was not added. [75] Comparative Example 2: Preparation of beverage composition containing Hizikia fusiforme [76] A beverage composition was prepared in the same manner as in Example 1 of the present invention, except that Allium cepa was not added. [77] Comparative Example 3: Comparative preparation 1 of beverage composition containing Hizikia fusiforme and Allium cepa [78] A beverage composition was prepared in the same manner as in Example 1 of the present invention, except that Acanthopanax senticosus was not added. [79] Comparative Example 4: Comparative preparation 2 of beverage composition containing Hizikia fusiforme and Allium cepa [80] A beverage composition was prepared in the same manner as in Example 1 of the present invention, except that Lycii fructus was not added. [81] Comparative Example 5: Comparative preparation 3 of beverage composition containing Hizikia fusiforme and Allium cepa [82] A beverage composition was prepared in the same manner as in Example 1 of the present invention, except that the Cassia tora extractwas not added. [83] Comparative Example 6: Comparative preparation 4 of beverage composition containing Hizikia fusiforme and Allium cepa [84] A beverage composition was prepared in the same manner as in Example 1 of the present invention, except that vinegar was not added. [85] Test Example 1 : Test of anti-hypertensive activity of hypertension-preventing beverage composition containing Hizikia fusiforme and Allium cepa [86] The hypertension-preventing beverage compositions containing Hizikia fusiforme and Allium cepa, prepared in Examples 1 to 3 of the present invention, were provided. [87] Also, the beverage compositions of Comparative Examples 1 to 6 were provided.

[88] The beverage compositions were measured for angiotensin I-con verting enzyme

(ACE) inhibitory activity according to the Cushman and Cheung s method. [89] In the measurement of ACE inhibitory activity, hippuryl-L-histidyl-L-leucine

(HHL) was used as a substrate. HHL was dissolved in a 50 mM sodium borate buffer

(pH 8.3) containing 300 mM NaCl to make 5 mM HHL. [90] As the enzyme, Sigma- Aldrich ACE (Sigma Co., A6778) isolated from rabbit lungs was used. [91] 100 D of each of the beverage compositions was added to 100 D of the substrate and stabilized at 37 ⁰C for 100 minutes. Then 50 D of the enzyme was added thereto, and the mixture solution was allowed to react at 37 ⁰C for 30 minutes. [92] Then, 250 D of IN hydrochloric acid was added to the reaction solution to stop the reaction. [93] In a blank group, 50 D of sodium borate solution was added instead of the sample solution. [94] After completion of the reaction, 1.5 ml of ethyl acetate was added to the reaction solution and mixed for 30 seconds. The mixture was centrifuged at 3000 rpm for 15 minutes, and 1.25 ml of the ethyl acetate layer as the supernatant was taken and dried at 100 ⁰C for about 1 hour.

[95] The dried sample was completely dissolved in 1.5 ml of distilled water, and the solution was measured for absorbance at 228 nm. Based on the measured absorbance, the ACE inhibition of the sample was calculated according to the following equation.

[96] Inhibition (%) = (1-(S-Sc)/(B-Bc)) x 100 [97] wherein S = the absorbance of the sample, Sc = the absorbance of the control sample, B= the absorbance of the blank, and Bc= the absorbance of the control blank.

[98] The inhibitory activity against the angiotensin I-converting enzyme was measured as described above, and the measurement results are shown in Table 1 below. [99] Table 1 Test results for ACE inhibitory activities of beverage compositions

[100] As can be seen in Table 1 above, the beverage compositions of Comparative Examples 1 and 2, containing no Hizikia fusiforme ox Allium cepa, showed a very low ACE inhibitory activity. Moreover, the beverage compositions of Comparative Examples 3 to 5, containing no Acanthopanax senticosus, Lycii fructus or Cassia tora extract, which are Chinese medicinal materials used in the present invention, also showed slightly low ACE inhibitory activities. [101] Meanwhile, the beverage composition of Comparative Example 6, containing no vinegar, showed ACE inhibitory activity similar to those of Examples 1 to 3 of the present invention, suggesting that vinegar did not influence the ACE inhibitory activity of the beverage composition.

[102] However, it could be seen that the beverage compositions of Examples 1 to 3 of the present invention, containing Hizikia fusiforme and Allium cepa, showed a very high ACE inhibitory activity (IC ) that indicates anti-hypertensive activity.

[103] Test Example 2: Sensory test [104] The hypertension-preventing beverage compositions containing Hizikia fusiforme and Allium cepa, prepared in Examples 1 to 3 of the present invention, were provided.

[105] Also, the beverage compositions of Comparative Examples 1 to 6 were provided. [106] In the sensory test of each beverage composition, the taste, flavor and preference of each beverage composition were rated on 9-point scales.

[107] As sensory panels, a total of 40 men and women (10-40-age groups; 10 persons for each age group) were selected. [108] Table 2 Sensory test results

[109] * sensory test rating (9: very good; 0: very poor) [HO] As can be seen in Table 2 above, the beverage compositions prepared according to the methods of Examples 1 to 3 of the present invention showed excellent taste and flavor and high preference.

[111] Also, it could be seen that the taste, flavor and preference of the beverage compos itions of Comparative Examples 1 to 6 were slightly inferior to those of Examples of the present invention.

[112] In particular, the beverage composition of Comparative Example 6, containing vinegar, showed inferior taste, flavor and preference, suggesting that the addition of vinegar improved the taste and flavor of the inventive beverage composition, even though it did not influence the anti-hypertensive activity of the composition. Industrial Applicability

[113] As described above, the present invention provides a beverage composition containing Hizikia fusiforme and Allium cepa as main components, together with Chinese medicinal materials, including A canthopanax senticosus, Lycii fructus and Cassia tora.

[114] The inventive a beverage composition containing Hizikia fusiforme and Allium cepa has a high angiotensin I-converting enzyme (ACE) inhibitory activity that indicates anti-hypertensive activity, and can be simply and conveniently drunk, thus exhibiting an excellent effect on the prevention of hypertension.

[115] According to the present invention, there is provided a beverage composition for the prevention of hypertension, which promotes the consumption of Hizikia fusiforme, and thus can contribute to industrial development and human health promotion.

Claims

Claims [1] A beverage composition for the prevention of hypertension, the composition comprising 100 parts by weight of Hizikia fusiforme, 50-80 parts by weight of Allium cepa, 1-5 parts by weight of Acanthopanax senticosus, 1-5 parts by weight of Ly ciifr uctus, 1-5 parts by weight of Cassia tora extract and 1-5 parts by weight of vinegar. [2] A method of preparing a beverage composition for the prevention of hypertension using Hizikia fusiforme and Allium cepa, the method comprising the steps of:

(1) preparing materials;

(2) mixing 100 parts by weight of Hizikia fusiforme with 50-80 parts by weight of Allium cepa, 1-5 parts by weight of Acanthopanax senticosus and 1-5 parts by weight of Lycii fructus;

(3) adding loess water to the mixture in an amount of 6 liters per kg of Hizikia fusiforme, heating the mixture solution to 100 ⁰C and additionally heating the heated mixture solution for 1-2 hours;

(4) filtering the heated mixture of step (3);

(5) heating loess water, adding the heated loess water to Cassia tora in an amount of 2 liters per 10 g of Cassia tora, extracting Cassia tora in the heated loess water for 10-20 minutes, and then filtering the extract, thus preparing Cassia tora extract; and

(6) adding, based on 100 parts by weight of the Hizikia fusiforme of step (2), 1-5 parts by weight of the Cassia tora extract and 1-5 parts by weight of vinegar to the filtrate of step (4).