DOC

Danqin particles TLC_873

By Gladys Turner,2014-10-30 14:45
17 views 0
Danqin particles TLC_873

Danqin particles TLC

     Author: Zhang Tiejun Cheng Tian Wang Gong Su Xiao Jun Yan Xue LIAO Mao-Liang Xu

     Abstract Objective To establish Danqin particles TLC (TLC) identification method, in order to provide a basis for

    controlling the quality of their products. Methods TLC method Agrimony, Zhe roots, Hedyotis diffusa, Gynostemma, Bupleurum, Ranunculus grass, Millettia were qualitatively identified. Results TLC chromatography can be detected Agrimony, Zhe roots, Hedyotis diffusa, Gynostemma, Bupleurum, Ranunculus grass, Millettia. Conclusion qualitative method is accurate and feasible, reproducible and can be used as Danqin particle quality standards.

     Key words TLC Danqin quality standards for particulate

     Abstract: ObjectiveTo establish TLC method for Danqin Granules. MethodsAgrimonia pilosa Ledeb, Cudrania tricuspidata (carr.) Bur., Hedyotis diffusa Willd, Gynostemma pentaphyllum (Thunb.) Makino, Bupleurum chinense DC., Ranunculus ternatus Thunb., Spatholobus Suberectus Dumn in Xianlingcao Granules were identified by TLC method. ResultsAgrimonia pilosa Ledeb, Cudrania tricuspidata (carr.) Bur., Hedyotis diffusa Willd, Gynostemma pentaphyllum (Thunb.) Makino, Bupleurum chinense DC., Ranunculus ternatus Thunb., Spatholobus suberectus Dumn

    could be identified by TLC. ConclusionThis method is accurate and highly reproducible. It can be used for the quality control of Danqin Granules.

     Key words: Danqin Granules; TLC; Quality standard

     Danqin particles Tianjin Institute of Pharmaceutical Research based on years of clinical experience side study of Chinese herbal compound preparation, with nourishing Qi, Sanyu pain, detoxification swelling, spleen phlegm, soft-fried

    Sanjie role, for the treatment of digestive tract tumor. The

    preparation by the Agrimony, Tsugeki, Huang Qin, Salvia and other drug composition, chemical composition is very complicated. In order to better control the quality of the product, the author used HPLC method for their monarch herb

    Salvia and baicalin were assay (reported in another paper), using thin-layer chromatography of the preparation of the Agrimony, Zhe roots, white flowers snake tongue grass, Gynostemma, Bupleurum, Ranunculus grass, Millettia been identified.

     An instrument and reagent

     Ultrasonic Instrument (Autoscience AS3120); silica gel G plate, Silica gel GF254 plates (Qingdao Marine Chemical Plant); methanol, chloroform, ethyl ether, ethyl acetate and other reagents were analytical pure.

     Danqin particles (homemade); Agrimony, Zhe roots,

    Ranunculus grass, Millettia, Hedyotis diffusa, Gynostemma, Bupleurum (Bozhou medicines purchased from Anhui Co., Ltd.).

     2 Methods and Results

     2.1 Agrimony by TLC to take the product powder 10 g, plus petroleum ether (60 ~ 90 ?) 30 ml, ultrasonic treatment 30

    min, filtration, the filtrate Hui dry petroleum ether, add 2 ml chloroform to make dissolved, as a solution for the test items. Another take control Agrimony herbs 5 g, with the rule of law must control medicinal solution. According to thin layer chromatography [1] test, to learn for the test product solution 10 μl, control medicinal liquid 5μl. Each point on

    the same piece of silica gel G thin-layer board with

    cyclohexane - ethyl acetate - glacial acetic acid (25:5:1) as

    the agent, started out, drying, at under 365 nm UV view. Test products for chromatography, chromatography with reference substance the same as the corresponding position of substantial color spots. Figure 1.

     2.2 Identification of Zhe root powder to take this

    product 10 g, plus methanol 40 ml, ultrasonic extraction 30 min, centrifuged and the supernatant evaporated and the residue dissolved in 10 ml water, centrifuged and the supernatant liquid funnel in the home sub - , add chloroform 5

    ml, Zhen Yao extraction, abandoned to the chloroform solution, water, waving to the chloroform layer, add diethyl ether extraction twice Zhen Yao, 10 ml / times, combined ether layer evaporated the residue add 1 ml of methanol allows the dissolved, as a solution for the test items. Zhe-roots control

    an alternative medicine 2 g, water 50 ml, reflux extraction 2 h, put cold, filtration, the filtrate home Separating funnel, the ethyl Zhenyao vinegar extract twice 30 ml, combined vinegar Ethyl layer, evaporated and the residue dissolved in 1 ml methanol added as a medicinal solution of the control. Absorb medicinal solution of the control, respectively, for each test product solution 10 μl, respectively, points on the

    same silica gel G thin-layer plate to cyclohexane

    chloroform ethyl acetate (4:1:2) as the agent to start, take out, drying, home ultra-violet light (365 nm), under review

    for the test materials chromatography, chromatography with the corresponding position of the control medicines, the same

    color of the fluorescent spots significantly. Figure 2.

     2.3 Identification of Hedyotis diffusa, said taking the product powder 10 g, plus methanol 30 ml, ultrasonic extraction 30 min, let cool to room temperature, centrifuged and supernatant was evaporated and methanol, the residue

    dissolved in 10 ml water, centrifuged and supernatant set points in the funnel with petroleum ether (60 ~ 90 ?) Zhenyao

    extracted three times, 10 ml / times, abandoned to the ether solution, the water layer Hui dry petroleum ether, extracted

    with chloroform Zhenyao 3 times, 10 ml / times, combined chloroform layer, evaporated and the residue add 1 ml of methanol allows the dissolved, as a solution for the test items. Hedyotis diffusa against an alternative medicine 1.0 g,

    plus petroleum ether (60 ~ 90 ?) 30 ml, ultrasonic Zhenyao

    extraction 30 min, let cool to room temperature, filtration, residues Hui dry petroleum ether, residues plus 30 ml methanol , ultrasonic extraction 30 min, let cool to room temperature, filtration, the filtrate evaporated and methanol, residual methanol solvent to 2 ml, filtration, the filtrate solution as a control medicine. Were drawn for the test product solution 10 μl, control medicinal solution 5 μl,

points on the same silica gel GF254 thin-layer board with

    chloroform - methanol glacial acetic acid (30:5:1) as the

    agent, started removed, dried, setting UV lamp (254 nm), under review for the test materials chromatography, chromatography with the corresponding position control medicines, significantly the same color of the fluorescence quenching spots. Figure 3.

     2.4 Identification of Gynostemma take this product, said fine powder 5 g, set a plug centrifuge tube, add water, 8 ml, so that was moist state, coupled with water saturated n-

    butanol 25 ml, Zhen Yao extraction, centrifugation, take n-

    butanol layer Purchase 40 ml centrifuge tube with plug, to be n-butanol saturated with water, 10 ml, Zhen Yao extraction, centrifugation, take n-butanol layer, evaporated and the

    residue dissolved with methanol to 2 ml, filtration, the

    filtrate for the test as product solution. Taking medicines called Gynostemma control 0.5 g, buy a plug centrifuge tube, add water, 2 ml, so that was wetting the state, coupled with water saturated n-butanol 20 ml, Zhen Yao extraction,

    centrifugation, take n-butanol, and placing 40 ml with Cyprus centrifuge tube, to be n-butanol saturated with water, 10 ml, Zhen Yao extraction, centrifugation, take n-butanol layer,

    evaporated and the residue dissolved with methanol to 2 ml,

    filtration, the filtrate as a solution for the test items. The control solution of the above-mentioned ingredients were drawn

    for each test product solution 5 μl, respectively, point to

    the same high-performance silica gel G TLC plate, ethyl acetate, n-butanol water (4:1:5) solution as the upper

    Expand agent, started out, dried, sprayed with sulfuric acid solution (1 ? 10), heated at 105 ? to the spots clear, set

    UV lamp (365 nm), under review, in the chromatographic products for the test, in the control herbs chromatography

    corresponding position, substantially the same color of the fluorescent spots. Figure 4. Reposted elsewhere in the paper for free download http://

     2.5 Identification of Bupleurum take this product powder 20 g, add water, 60 ml allows the dissolved, centrifuged and the supernatant of water-saturated n-butanol extract Zhenyao 4

    times (75,75,50,50 ml), combined n-butanol solution, Ammonia

    test solution was washed twice (50,50 ml), vacuum concentrated to the dry residue add 40 ml of water allows the dissolved,

    centrifuged and supernatant by D101 (10 ml)-type macroporous

    resin column (diameter 1.5 cm, length 15 cm), eluted with water 50 ml, abandoned to the water liquid, and then 30% ethanol 40 ml elution, discard to the eluate, following with

    70% ethanol 40 ml elution, collecting eluate, evaporated, residue dissolved with methanol to 2 ml, filtration, the filtrate as a solution for the test items. Bupleurum control an alternative medicine 1.0 g, buy a plug flask, add methanol 20 ml, ultrasonic treatment 30 min, filtration, the filtrate evaporated and the residue dissolved in methanol to 2 ml, filtration, the filtrate as a control medicine solution. According to thin-layer chromatography test, drawing the

    above-mentioned two kinds of solutions of 5 μl, respectively,

    points on the same silica gel G thin-layer plate, pre-

    saturated 2 min, with ethyl acetate, chloroform

    methanol-water (15 : 50:22:10) of the lower solution as the mobile phase, to start out, dried. Sprayed with 10% ethanol

    solution of sulfuric acid, hot winds to the color clear, set 365 nm to view, test products for chromatography, chromatography with the corresponding position of the control medicines, the obvious spots the same color. Figure 5.

     2.6 Identification of Maozhaocao [2]

     To take this product 10 g, ethyl acetate plus 30 ml, ultrasonic treatment 30 min, filtration, the filtrate Hui dry ethyl acetate, ethyl acetate residue with 1 ml allows the dissolved, as a solution for the test items. Control an

    alternative medicine Maozhaocao 5 g, in accordance with test materials for the preparation method of solution obtained in control medicinal solution. Lessons for the solution of test materials and control of various medicinal solution 10μl,

    respectively, points on the same silica gel G TLC plate, ethyl acetate, toluene glacial acetic acid (20:4:0.5) as the agent, started out , dried, sprayed with 10% ethanol solution of sulfuric acid, 105 ? Kaozhi spots were clear. In the test materials for chromatography, in contrast with the herbs chromatography Maozhaocao the corresponding position, substantially the same color spots. Figure 6.

     2.7 Identification of Millettia [3]

     To take this product 10 g, plus methanol 30 ml, ultrasonic treatment 30 min, filtration, the filtrate Hui dry methanol, add 20 ml of water allows the dissolved residue to

    transfer to a separatory funnel, add ether extracted three times, 10 ml / times, combined extract, Hui dry ether, add 2 ml of methanol allows the dissolved, as a solution for the

    test items. Millettia control an alternative medicine 5 g, in accordance with test materials for the preparation method of solution obtained in control medicinal solution. Lessons for the solution of test materials and control of various

    medicinal solution, 10 μl, respectively, points on the same

    silica gel G TLC plate, ethyl acetate, toluene glacial

    acetic acid (9:4:1) as the agent, started removed, dried, sprayed with 10% ethanol solution of sulfuric acid, hot winds

    to the spots were clear. In the test materials for chromatography, in contrast with Millettia medicinal chromatography corresponding position, substantially the same color spots.

     3 Discussion

     The preparation of 22 Chinese herbal medicines by the

    composition of ingredients is very complicated. In order to better control the quality of the finished product, I used TLC method which seven were identified taste the main ingredients. The three batches of samples test proved that the method is easy to spot separation clear, reproducible, negative control without interfering with the quality of the product can be used as control methods.

     This prescription medicine that contains a lot of people in the "Chinese Pharmacopoeia" and the corresponding local

    standards are not given the appropriate TLC method, so this paper, the method of identifying medicinal herbs and their preparations for their identification with a very good learn.

     References

     [1] State Pharmacopoeia Commission. Chinese

    Pharmacopoeia, ? Division [M]. Beijing: Chemical Industry Press, 2005: Appendix 31.

     [2] Lu Bin, DONG Shu-min, FU Xiao-6, et al. Maozhaocao

    the physical and chemical identification of its preparation [J]. Henan Journal of TCM, 1999,14 (2): 17.

     [3] Deng Xiaomei, Sun Yi-qun. Tongbiling were identified

    by TLC and the mixture of Millettia Celastrus [J]. Guangdong Pharmacology, 2004,14 (5): 7. Reposted elsewhere in the paper for free download http://

Report this document

For any questions or suggestions please email
cust-service@docsford.com