Effect of ultrafine pulverized cassia seed on its dissolution amount of chrysophanol
Li Xiaoming, Wang Yuesheng, Yan Han, Zhang Jun, Tang Xiaojun
(Institute of Chinese Materia Medica, China Academy of Traditional Chinese Medicine, Beijing 100700 , China)
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Abstract: A comparative study on the amount of chrysophanol eluted from Cassia after ultrafine pulverization. The results showed that the extraction rate of chrysophanol was only 7.6% after dehydration of cassia seed under the same extraction time and conditions, and the ultrafine granules were obtained after different conditions. The extraction rate of cassia seed was increased to 69.7%, 57.1%, and 32.4%, respectively. Under the 5min water soaking, the total chrysophanol content in Cassia seed powder was equivalent to that of medicinal water decoction for 90min. Proper drying of the sample before pulverization can improve the total. The amount of chrysophanol dissolved.
Key words: ultrafine pulverization; cassia seed; chrysophanol
CLC number: R284.1 Document code: B Â Â Â Â Article ID: 1005-9903 (2001) 06-0006-03
The application of ultrafine pulverization technology in the field of traditional Chinese medicine is a new technology that has emerged in recent years. After ultrafine pulverization, the Chinese medicinal materials have fine and uniform particle size, and the cell walls are mostly broken or even completely broken, so the specific surface area is increased, which is beneficial to the dissolution of the contents and facilitates the extraction of the active ingredients. Therefore, the use of ultra-fine pulverization technology to treat Chinese medicinal materials is an important aspect of the application of this technology in the field of traditional Chinese medicine, so the rational application of this technology has a more realistic research significance.
Cassia is a mature seed of the leguminous plant Cassia obtusifolia L. or small cassia C. tora L., which is a commonly used traditional Chinese medicine  . Cassia has the functions of dispelling wind and dissipating heat, clearing the liver and improving eyesight, and relaxing bowel movements. It is often used for the treatment of redness and swelling, blue-blindness, finch, and constipation. Modern studies have shown that cassia has a high content of zui, which is about 0.25% in the literature  , and the total strontium content is about 0.61%  ; it also contains vitamin A-like substances, mucus, protein, sitosterol, amino acids. And fat oil and other ingredients. In recent years, studies have shown that Cassia has a hypotensive effect  , in addition, Cassia has a hypotensive effect  and significantly improve the distribution of cholesterol in the body, which are conducive to the prevention of atherosclerosis  and other cardiovascular and cerebrovascular disease. This paper intends to study the effect of ultrafine pulverized cassia seed on the dissolution of the quinone compound, rhubarb, in its fine powder.
1, instruments and materials
1.1 Instrument Superfine pulverizer: Model: SQW-6 superfine pulverizer.
1.2 Hitachi 7400 High Performance Liquid Chromatograph.
1.3 Cassia cassia seed is provided by Tongrentang Pieces Factory, which is a mixture of mature seeds of C. obtusifolia LT C.tora L.; Cassia is subjected to ultrafine pulverization processing and particle size measurement is carried out on a computer imaging particle size analyzer, and the pulverization of each micropowder sample The conditions are as follows:
Cassia comminution conditions and particle size
Â Â Â Â Â Â Â Â Â Â Â Â Â Â Â Â Â Crush 25' Â Â Â Â Â Â Â Crush 32' Â Â Â Â Â Â Â Â Â Â Â Crush 40'
200 mesh pass rate 300 mesh pass rate 300 mesh pass rate
Cassia sample Â Â Â Â Â (%) / average grain Â Â Â (%) / average grain Â Â Â Â Â Â Â (%) / average grain
Â Â Â Â Â Â Â Â Â Â Â Â Â Â Â Trail D 50 (?m) Â Â Â Â Trail D 50 (?m) Â Â Â Â Â Â Â Trail D 50 (?m)
Not dried 88/8.29 65/6.71 72/6.12
Dry at 80 Â° C 1h 94/7.31 76/8.45 81/7.36
Dry at 80 Â° C for 4 h 99/8.18 81/8.18 881.76
1. Â Â Â Â Â Â 4 Reagents The rhubarb reference substance was purchased from the China National Institute for the Control of Pharmaceutical and Biological Products (batch number: 796-9302). Methanol is chromatographically pure, chloroform and phosphoric acid are of analytical grade, and water is ultrapure water.
2, methods and results
2. Â Â Â Â Â Â 1 Chromatographic conditions Column: YWGC 18 10?m (4.6 mm Ã— 250 mm), mobile phase: methanol - 0.1% phosphoric acid (90: 10), flow rate: 1 ml / min, detection wavelength: 254 nm, column temperature: 30 Â° C.
2.2 Standard curve preparation Precision weighing rhodamine reference substance 4.18mg, dissolved in methanol and fixed to 50ml brown volumetric flask, accurately absorb 0.5, 1.0, 2.0, 4.0, 5.0ml in 5 10ml volumetric flask, add methanol to dilute To the scale, shake well. According to the chromatographic conditions, the injection volume was 20 Î¼l. The linear range is 0.0836~0.8360?g, and the linear regression equation is y=2.69 Ã—10 6 X-7.83Ã—10 3 , r= 0.9998.
2.3 Precision test Take the rhubarb reference solution, repeat the injection 5 times, each time 10?l, the RSD of the reference area of â€‹â€‹the reference product of the rhubarb peak is 1.4%.
2.4 Stability test Depending on the sample solution of Mingzi micropowder (dried for 1 hr, pulverized 32', extracted 15'), 10?l was injected at 0, 2, 4 , and 6 hr, respectively, and the peak area was recorded. The results showed that the peak area of â€‹â€‹the four injections was RSD. 1.9%.
2.5 Repeatability test Â Â 5 parts of the Mingzi micropowder sample solution (dried for 1 hr, pulverized 32', extracted 15'). As a result of the sample measurement method, the average content of chrysophanol was 1.34 mg/g, and the RSD was 1.8%.
2.6 Sample recovery test Take a known amount of Cassia seed micropowder sample (dry 1hr, crush 32', extract 15') about 0.10g, accurately weighed, add appropriate amount of reference solution (0.116 ~ 0.155mg), spin, according to the sample The average recovery was 93.5% and the RSD was 2.5% (n=4) as determined by the assay.
3 Preparation and determination of test solution
3.1 Depending on the powder of Mingzi (crushed with a small pulverizer, passed through a 40 mesh sieve, without peeling) 2g, accurately weighed, extracted with methanol in Soxhlet extract to a colorless extract to a volume of 100ml volumetric flask; precision extraction of the extract 10ml in the evaporating dish, evaporated in a 50 Â° C water bath, add 2ml 2.5mol / L sulfuric acid solution to dissolve the residue, wash into 20ml plugged test tube, hydrolyze on boiling water bath for 2h, intermittently shake three times (8,8,4ml), merge Chloroform solution, washed twice with distilled water, evaporated to dryness, dissolved in methanol and dissolved in a 10 ml volumetric flask, shake well, that is.
3.2 Take a total of 5 parts of about 10g of Mingzi , precise and stable, add 100ml of distilled water to the flask with a stopper, weigh it, heat it back 15', 30', 45', 60', 90', let cool, weigh, add Distilled water to make up the weight, shake, filter, and the filtrate is ready for use; accurately extract 10 ml of each of the above extracts , evaporate in a water bath, evaporate in a water bath, place in a desiccator to constant weight, and weigh for the amount of leachate.
3.3 Determination of total chrysophanol content and extraction rate in cassia seed before ultrafine pulverization Â Â Pipette 2ml of the above five groups of extracts into a large test tube, add 2ml of 5mol/L sulfuric acid solution, and prepare the sample solution according to 3.1 for the rest of the operation, and determine according to the chromatographic conditions. The results are shown in Table 1:
Table 1 Effect of Different Extraction Time on Total Extract Content and Total Chrysophanol Content of Cassia
Extraction time Â Â Â Â Â Â Total extract content Â Â Â Â Â Â Â Â Total chrysophanol content Â Â Â Â Â Extraction rate
(min) Â Â Â Â Â Â Â Â Â Â (%) Â Â Â Â Â Â Â Â Â Â Â Â Â Â (mg/g) (%)
15 10 0.18 7.6
30 14 0.62 26.1
45 15 0.78 32.8
60 19 1.02 42.9
90 22 1.69 71.0
Soxhlet extraction (6h) - 2.38 100
3.4 Determination of total chrysophanol in cassia seed after ultrafine pulverization Â Â Depending on the micropowder of the micro-powder group of Mingzi, about 1g of 4 parts, put it in a stoppered triangle bottle, add 50ml of distilled water, and immerse it in a water bath of 80Â°C for 5, 15, 30, 45min; take it out, let it cool, centrifuge, and absorb the supernatant. 2 ml was placed in a 20 ml large test tube, and 2 ml of a 5 mol/L sulfuric acid solution was added. The rest of the operation was carried out according to 3.1, and the sample liquid was prepared according to the chromatographic conditions. The results are shown in Table 2 and Table 3:
Table 2 Effect of different temperature on the content of chrysophanol in extracting Cassia seed powder (drying 4h, crushing 25')
Temperature (Â°C) 60 70 80 90
Content (mg/g) 1.33 1.34 1.58 1.46
Table 3 Effect of extraction of total chrysophanol in Cassia seed powder at different times (mg/g) (80 Â°C)
Micro powder group Â Â Â Â Â Â Â Â Â Â Â Â Extract 5min/ Â Â Â Â Â Extract 15min/ Â Â Â Extract 30min/ Â Â Â Extract 45min /
Â Â Â Â Â Â Â Â Â Â Â Â Â Â Â Â Â Â Extraction rate Â Â Â Â Â Â Â Â Â Extraction rate Â Â Â Â Â Â Â Extraction rate Â Â Â Â Â Â Â Â Extraction rate
Â Â Â Â Â Â Crush 25' 0.42/17.6 0.46/19.3 0.50/21.0 0.48/20.2
Undried, crushed 32' 0.42/17.6 0.77/32.4 0.72/30.3 0.85/35.7
Crush 40' 0.65/27.3 0.70/29.4 0.74/31.1 0.55/23.1
Crush 25' 1.60/67.2 1.69/71.0 1.59/66.8 1.56/65.5
Drying 1h, crushing 32' 1.54/64.7 1.36/57.1 1.36/57.1 1.23/51.7
Crush 40' 1.05/44.1 0.87/36.6 0.92/38.7 0.73/30.7
Crush 25' 1.73/72.7 1.48/62.2 1.59/66.8 1.66/69.7
Drying 4h, crushing 32' 1.60/67.2 1.66/69.7 1.96/82.4 1.82/76.5
Crush 40' 0.93/39.1 0.90/37.8 1.00/42.0 1.09/45.8
4.1 Correlation between pulverization conditions and particle size From the table of Cassia pulverization conditions and particle size, it can be seen that: 1 The dryness or water content of the material has a direct influence on the pulverization fineness, that is, the lower the water content, the pulverization into fine Particles; 2 When the water content is the same, the longer the pulverization time, the finer the pulverized particle size, but when the pulverization reaches a certain time point, the pulverization time is prolonged, the influence on the particle size becomes small, suggesting that: when the cassia is pulverized, there is Zui good smashing condition determination problem.
4.2 Comparison of total rhubarb extraction rate of cassia seed before and after pulverization 1 It can be seen from Table 1 that the unextracted cassia seed has the same extraction condition, the longer the extraction time, the higher the extraction rate, and the cooking is carried out 3 times, each time 30 minutes. The extraction rate can reach 71.0%. 2 It can be seen from Table 3 that after ultrafine pulverization, the extension of extraction time has little effect on the extraction rate, suggesting that after ultrafine pulverization, the cell wall is broken, which contributes to the dissolution of total chrysophanol and accelerates the dissolution rate. When the extraction is 5 min, the concentration equilibrium can be reached or approached; in the experiment, it is also found that the viscosity of the solution increases with the extension of the extraction time. Comparison of the two: water decoction cassia seed (extraction 15min), the extraction rate of chrysophanol is only 7.6% (100% by Soxhlet extractor), and the extraction rate of each group of Cassia after superfine pulverization under different conditions respectively Increased to 69.7%,
57.1%, 32.4%; if the total chrysophanol content was compared, the total chrysophanol content of cassia seed micropowder (dried 4h, crushed 32min) was equivalent to the content of medicinal water boiling for 90min at 80 Â°C, 5min water soaking. 3 It can be seen from Table 3 that with the same extraction time, the finer the particle size, the higher the elution amount, such as pulverization for 25 min, extraction for 5 min, undissolved dissolution of 0.42, drying for 1 h is 1.60, and drying for 4 h is 1.73. . However, from the sample group which prolonged the pulverization time and increased the fineness, the smaller the fineness, the lower the amount of dissolution, especially in the 40min group, the dissolution decreased significantly; while the undried group had little effect on the particle size due to the prolonged pulverization time. Therefore, the reduction of the amount of dissolution is not obvious, suggesting that the prolongation of the pulverization time has a certain influence on the total rhubarb phenol component, indicating that from the dissolution and retention of the active ingredient, there is also a problem of determining the smashing condition of the zui. It can be seen that when the ultrafine pulverization technology is applied to the pulverization of traditional Chinese medicine, there are certain scientific problems such as application rules and application conditions, which is not a simple smashing process and should be paid enough attention.
In this experiment, the cassia seed was smashed and peeled, and its total chrysophanol content increased by nearly 74%, suggesting that terpenoids are mainly present in fruits, and the content in the skin is small; free chrysophanol only accounts for 1.47 of total chrysophanol content. %. In addition, research on the stability of anthraquinones in Cassia and its related pharmacodynamic studies after superfine pulverization are underway.
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 Zhang Qiwei, Yin Jian, Zhang Jun, et al. Comparison of some active ingredients in raw and fried cassia seed and its decoction[J]. Chinese Traditional and Herbal Drugs, 1996, 27(2): 79.
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