Comparative experimental study on unilateral and compound cell-grade pulverization and common pulverization quality standards

Unilateral, compound cell grade crushing and
Comparative Experimental Study on Common Crushing Quality Standards
 
Shandong Institute of Pharmaceutical Industry   Guo Qi   Du Xiaomin
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The ultrafine powder is prepared by pulverizing a compound (multi-flavored medicine) or a single-side medicine using a cell-level pulverizing apparatus. The smashing feature is the medicinal material
The cell wall breaks, and the active ingredient in the medicinal cell can be directly extracted without passing through the cell wall or membrane in the presence of a solvent.
Come out to speed up the drug extraction rate. The second is the insoluble active ingredient of the medicinal material, which helps each other in the process of extracting organic solvents.
Dissolved, extracted. Ordinary pulverization is a process of pulverizing a compound or a single medicinal material using a general pulverizing apparatus. Specific test
The sac and its prescription single medicinal herbs were tested as an example.
First, instruments and reagents
Microscope Thin layer scanner Reference product (China National Institute for the Control of Pharmaceutical and Biological Products)
The medicines were purchased from Jianlian Pharmacy, and the samples of the sugar capsules were made by the company. The reagents were of analytical grade (commercially available).
Second, experimental methods and results
1. Preparation of two specifications of Tangtai capsule, Zhimu medicine, Jinqi Shenqi pills powder
Take the medicine mixed with the sugar Thai prescription, half the amount is made into fine powder by the cell-level pulverizing equipment; the other half is crushed by ordinary pulverizing equipment.
80 mesh sieve, made into coarse powder; take the medicine mixed with the prescription of Jinqi Shenqi Pill, half of the amount is made into fine powder by cell-level crushing equipment; the other half
It is pulverized by ordinary pulverizing equipment and passed through a mesh of 80 mesh to make a coarse powder; the medicinal materials of Zhimu, Pueraria, and Phellodendron are made in the same way.
Fine powder; for testing.
2. Comparison of extraction methods for identification test of Pueraria lobata and Phellodendron chinense
Take 4g of sugar capsules, refer to the pharmacopoeia identification method, add 15ml of 95% ethanol, shake for 1 hour, 2 hours, filter,
The solvent was evaporated to dryness, and the residue was added with methanol to prepare a test solution for the identification of pueraria and cork. Sugar Thai capsule coarse powder 4g, made by the same method 3
Test liquid. The silica gel G chromatogram of the test sample was prepared by thin layer chromatography. The 1, 2, and 3 liquids showed the same size of the Pueraria root identification spot.
However, the two liquids contained many spots of impurities. The identification of Cork is to weigh 4g of sugar capsules, refer to the pharmacopoeia plus methanol, and heat reflux
Take 15 minutes to make 4 test solutions. The chromatogram of silica gel G was prepared by thin layer chromatography, and the spots presented by 1, 2, 3, and 4 were the same.
Therefore, after the cell material is pulverized by the cell, the cell wall is broken, and the active ingredients of the medicinal material are not dissolved by the cell wall exchange, which is simple and easy to mention.
Taking the method, the extraction time is shortened.
3, Jinshen Shenqi Pills crude, fine powder microscopic identification control
Take the prescription of Jinshen Shenqi Pills and smash them into coarse and fine powders. Take the coarse and fine powder and make the microscopic identification slides.
Observe and take photos under the microscope. As can be seen from the figure, the coarse and fine powders are greatly different on the particles.
4. Control experiment of crude and fine powder content of Zhimu medicinal materials
Precisely take about 1g of coarse and fine powder of the parent medicine, and accurately weigh it. According to the 95th edition of the pharmacopoeia, the determination of the content of the medicinal material
Test method, the measured content list is as follows

Test number
Coarse powder
Fine powder
1
1.26%
1.39%
2
1.33%
1.45%
3
1.29%
1.42%
It can be seen from the results that the content of the extracted saponins is higher than that of the coarse powder after the cell-grade pulverization.
5, Comparative test of crude and fine powder content in the compound of Tangtai capsule
Take 8g of crude and fine powder contents of Tangtai Capsule, accurately weighed, add ethanol, sonicate for 40 minutes, let stand, filter, and set the filtrate
Contained in a measuring bottle. Precisely take 10ml of filtrate , add hydrochloric acid for 1 hour, let cool, add sodium hydroxide to adjust the pH to neutral, take
The supernatant was placed in a 50 ml volumetric flask, and 10 ml of the filtrate was taken, and the solvent was evaporated to dryness. The residue was dissolved in benzene and quantitatively transferred to a 2 ml volumetric flask for use as a test sample.
Solution 1, 2. Another saponin reference material plus benzene was made into a solution containing 2 mg per 1 ml as a reference solution. According to thin layer chromatography,
Take the test solution 1, 2 each of 8 μ l, reference solution 2 μ l, 4 μ l, respectively, the intersection of the same silica gel G plates, developing solvent to benzene,
Acetone (9 : 7) , unrolled, taken out, dried, sprayed with color developer, dried at 105 °C until clear color, covered glass plate, fixed, at λ s=445nm
At the wavelength, the absorbance integral value of the reference product and the test solution is measured, and the results are as follows.
Test number
菝 甙 甙 甙 content (mg / grain)
菝 甙 甙 甙 content (mg / grain)
1
0.68
0.89
2
0.75
0.93
3
0.71
0.84
It can be seen from the results that the content of the saponins contained in the compound after the cell-level pulverization is higher than the content of the saponins contained in the compound of the coarse powder.
In summary, ordinary pulverization and cell-level pulverization have poor extraction time, extraction method, microscopic identification, and ingredients in medicinal materials.
different. Cell-grade pulverized fine powder can shorten the static extraction time; heat extraction can be replaced by dipping method; microscopic identification can be observed
The particle size of the brown lumps characteristic structure is very different under the same magnification conditions ( photo observation ) ; single medicinal herbs or compound
Medium cell pulverization is higher than ordinary pulverized powder. We carry out cell-level pulverization made of finished products or unilateral, from several aspects
The results are only preliminary explorations; if there are similar results for other single-flavored herbs or compounds, more extensive and further tests are needed.
Study.
 
 
 
 

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