Capsule thin-layer chromatography Xinkening Identifying the Quality Improvement
【Abstract】 Objective To improve Xinkening Capsule TLC method. Method of discriminant analysis using thin-layer
chromatography. Resulted in an increase Sal B, Chinese toad
venom poisoning base and borneol herbs such as identification, thin-layer chromatography atlas clear, specific, and reproducible. CONCLUSION This method is quick and easy, stability, and specificity, good for improving Xinkening capsules provide a basis for quality standards.
Key words high-performance liquid chromatography; thin-layer
chromatography; Xinkening capsules
Xinkening standards of traditional Chinese medicine capsule for the Ministry of Health set prescription drug
formulations ninth book (WS3 B 1714 94) closed set of
proprietary Chinese medicine, from Salvia, 37, borneol, Toad, etc. 8 medicine flavor composition, the main for the treatment of coronary heart disease, angina, chest tightness, palpitations, dizziness embolism [1,2]. In order to better control product quality, to ensure drug safety, effective, and the present study, thin-layer chromatography to conduct
qualitative research on this product, in order to Xinkening capsule lay the foundation for quality control. Results are as
follows.
An instrument and reagent
CAMAG REPROSTAR 3-phase system and the digital into a
semi-automatic injector (CAMAG), Sartorius BP211D Electronic
Analytical Balance (Germany), electric water bath pot (Beijing
Medical Equipment Factory), ultrasonic cleaning device (Beijing Medical Equipment Factory), silicon plastic thin precast panels G and GF254 (Zhejiang Taizhou).
Reference substance: Chinese toad venom poisoning the base (803 9202), Sal B (111562 200403), borneol
reference substance (110743 200504), acid reference
substance (100078 200414), deoxycholic acid reference substance ( 0724 2000207) by the Chinese drugs and
biological products offered, methanol, ethyl ether, ethyl acetate and other reagents were analytically pure water for the triple-distilled water.
2 Methods and Results
2.1 Identification of borneol to take this product 10, dumping out the contents, add ethyl ether 10 ml, sonication 5 min, filtration, dregs back, waving filtrate dried ethyl 2 ml vinegar residue allows the dissolved, As a solution for the test items. Lack of borneol obtained by the negative reference substance for the preparation of test materials were prepared by solution-negative reference substance solution. Another
take borneol reference substance, made of vinegar acid ethyl ester 0.5 mg per ml of solution, as a reference substance solution. And then take borneol herbs, vinegar is made of ethyl 0.5 mg per ml of solution, as a control solution of the
original medicine. In accordance with thin-layer
chromatography [2] experiment, to learn all the above-
mentioned four kinds of solution, 5 μl, respectively, points
on the same silica gel G thin-layer board V to V benzene,
ethyl acetate (19:1) as the agent, to start out, dried,
sprayed with 1% vanillin sulfuric acid solution, heated at 110 ? to spot color definition. Test products for chromatography, chromatography with the corresponding reference substance borneol position, substantially the same
color spots. The blank reference substance and reference substance in the corresponding position, without the same color spots. The results shown in Figure 1.
2.2 Identification of Salvia take [identification] (1) under the dregs, add 100 ml of methanol ultrasonic extraction
15 min, filtration, the filtrate as a solution for the test items. Salvia lack of negative reference substance obtained by the preparation for the test product solution was prepared by negative reference substance solution. An alternative medicine
Danshen 1 g, plus methanol 10 ml, with the rule of law into, as a control solution of the original medicine. And then take Sal B reference substance, add methanol made from 1 mg per ml of solution, as a reference substance solution. In accordance
with thin-layer chromatography [2] experiment, to learn all the above-mentioned four kinds of solution, 5 μl,
respectively, points on the same silica gel GF254 thin-layer
board with ethyl acetate V toluene V methanol V acid
V V water (4:8:1:4:6) in the upper solution as the mobile phase, to start out, dried, was observed under ultraviolet wavelength 254nm, the then sprayed with 1% ferric chloride ethanol solution color, was observed under visible light for the test materials chromatography, chromatography with the
reference substance for the corresponding position, substantially the same color spots. The blank reference substance and reference substance in the corresponding position, without the same color spots. The results shown in Figure 2. Reposted elsewhere in the paper for free download http://
2.3 Identification of toadfish to take this product 10, dumping out the contents, add 30 ml chloroform and ultrasonic extraction 15 min, filtration, the filtrate home Separating funnel, add the sodium hydroxide solution (0.1 mol / L) 20 ml. Gently Zhen Yao, abandoned to the sodium hydroxide solution; chloroform solution 20 ml of water washing, abandoned to the water, lotion, chloroform solution with anhydrous sodium sulfate dehydration, recovery of chloroform, ethanol plus 0.5 ml allows the dissolved residue, as for the test solution. The negative reference substance obtained by lack of Toad for the solution of the preparation of test materials prepared by negative reference substance solution. Another take Toad 0.2
g, grinded and ultrasonic extraction with 30 ml chloroform and 15 min, filtration, filtrate recovery of chloroform, 10 ml allows the dissolved residue with ethanol, as a control solution of the original medicine. And then take Chinese toad
venom poisoning the base reference substance, add ethanol, made from 0.05 mg per ml of solution, as a reference substance solution. According to thin layer chromatography [2] test,
drawing test items for the solution of 5 μl, reference
substance solution, 3 μl, respectively, points on the same
silica gel G thin-layer plate to V chloroform V acetone-V
cyclohexane (3:3:5) as the agent, the second to start from the exhibition were 8 cm, removed, dried, sprayed with 10% ethanol solution of sulfuric acid, 105 ? heated to spot color, was
observed under visible light. Test products for
chromatography, chromatography with the reference substance for the corresponding position, substantially the same color
spots. The blank control solution in the corresponding position with reference substance, without the same spots. The results shown in Figure 3.
1. Borneol reference substance 2. Borneol of the original medicine 3 and 4. For the test product 5. Negative samples
Figure 1 borneol identification map (omitted)
2.4 Identification of Bezoar take this product 10, dumping out the contents, add 10 ml of ethanol ultrasonic extraction 10 min, plus a small amount of activated carbon
decolorization, filtration, concentrated on a water bath set to about 1 ml, as a solution for the test items. Bezoar of the negative reference substance obtained by lack of test items for the preparation of solution-negative reference substance
solution was prepared. Bezoar of the original herbs to take 0.1 g, with the control solution prepared by the original ingredients. Take acid and deoxycholic acid reference substance of 2 mg, buy 5 ml Liang Ping, add ethanol capacity to dissolve and is scheduled to scale, shake, as a reference substance solution. In accordance with thin-layer
chromatography [2] experiment, to learn all the above-
mentioned four kinds of solution, 5 μl, respectively, points
on the same silica gel G TLC plate, chloroform V to V ethyl
acetate V formic acid (16:9 : 1) as the agent, started out, dried, sprayed with 10% ethanol solution of sulfuric acid, 105 ? heating 10 ~ 15 min, at 365 nm were observed under UV light. Test products for chromatography, in with the reference
substance, the original medicinal chromatography corresponding position, substantially the same color of the fluorescent spots, while the blank control solution in the corresponding position with reference substance, without the same color spots. The results shown in Figure 4.
Figure 2 Salvia identification map (omitted)
Figure 3 Toad Identification map (omitted)
Figure 4 under 365 nm UV lamp Bezoar identification map (omitted)
3 Discussion
In this study, the former on the basis of the ministerial standard extraction methods and indicators, and such factors as the choice of launch systems to improve on the increase. Salvia identification, due to preparation process using only the water extraction, so refer to the 2005 edition of "Chinese
Pharmacopoeia" ? Salvia Department of identification under the requirements of the water-soluble active ingredients of
Salvia Sal B to identify research, Toad identified an increase of Chinese toad venom poisoning as an indicator-based
reference substance for analysis; borneol in the original identification on the basis of physical and chemical identification of an increase of TLC, the bezoar identified an increase of deoxycholic acid control, and optimize the launch conditions, chromatography more stable and clear. These are further improved Xinkening capsules qualitative
identification.
This method is simple, reproducible, specific, in order to Xinkening capsules to further improve the quality standards laid a good foundation if they can establish control over the content of the corresponding indicators, will be more perfect, it remains to be studied further.
【References】
[1] Liu Donghui, Li Jun, HUANG Yi-sweet, and so on.
High-performance liquid chromatography Xinkening Capsule China
Toad poison-based, lipid content of toad poison ligand [J]. Chinese Journal Experimental prescriptions, 2005,11 (6): 26.
[2] National Pharmacopoeia Committee. Chinese Pharmacopoeia, ? Department of [S]. Beijing: Chemical
Industry Press, 2005:47,52,265,527, Appendix VIB. Reposted elsewhere in the paper for free download http://www.hi138 . com