CN105203693A - Thin layer detection method for glabrousleaf pittosporum seeds - Google Patents
Thin layer detection method for glabrousleaf pittosporum seeds Download PDFInfo
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- CN105203693A CN105203693A CN201510601446.4A CN201510601446A CN105203693A CN 105203693 A CN105203693 A CN 105203693A CN 201510601446 A CN201510601446 A CN 201510601446A CN 105203693 A CN105203693 A CN 105203693A
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- detection method
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- ethyl acetate
- quercetin
- glabrousleaf pittosporum
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Abstract
The invention discloses a thin layer detection method for glabrousleaf pittosporum seeds. The method includes the steps that 1, in preparation of a test article solution, the herbs to be detected are taken and smashed, petroleum ether is added for ultrasonic extraction, filtering is performed, filter residues are taken, ethyl acetate is added for reflux, filtering is performed, filtrate is evaporated to be dry, methyl alcohol is added into residues for redissolving, and then the mixture serves as the test article solution; 2, in thin layer detection, with quercetin being a contrast, sample application is performed on the test article solution and the quercetin contrast on a thin layer board, developing is performed with methylbenzene-ethyl acetate-formic acid being developing solvent, methylbenzene-ethyl acetate-formic acid=5:4:1, aluminum chloride color development is performed, and then visual inspection is performed. The new index component quercetin in the glabrousleaf pittosporum seeds is disclosed, serves as a spot of qualitative contrast and is used for detecting the glabrousleaf pittosporum seeds, and effective guarantees are provided for monitoring the quality of the glabrousleaf pittosporum seed herbs.
Description
Technical field
The present invention relates to medicinal material detection field, particularly relate to a kind of thin layer detection method of glabrousleaf pittosporum seed.
Background technology
Glabrousleaf pittosporum seed, this product is the drying kind of Pittosporaceae Chart database plant sea gold PittosporumillicioidesMak. or wrinkle leaf pittosporum tobira PittosporumcrispulumGagnep., there is the effects such as clearing heat, relieving sore-throat, puckery intestines controlling nocturnal emission with astringent drugs, astringing to arrest diarrhea, can be used for the treatment of the diseases such as pharyngalgia, dysentery, enteritis, leukorrhea, involuntary emission.
A kind of thin-layer identification method of glabrousleaf pittosporum seed is disclosed in the people such as Zhang Jun (Zhang Jun etc., glabrousleaf pittosporum seed quality standard Primary Study, Chinese medicine and clinical, 01 phase in 2011,15-19 page).The method, with the ultrasonic extraction of the sherwood oil of boiling range 30-60 DEG C twice medicinal material to be checked, prepares need testing solution; Thin-layer chromatography detects, and be that developping agent launches with toluene, iodo steam displaing color, inspects under daylight, carries out contrast TLC distinguish with glabrousleaf pittosporum seed control medicinal material.
But the method is when needs detect fast, comparatively loaded down with trivial details.
Summary of the invention
The invention provides a kind of thin layer detection method of glabrousleaf pittosporum seed, comprise the following steps: the preparation of (1) need testing solution: get medicinal material to be checked, pulverize, add the ultrasonic extraction of sherwood oil, filter, get filter residue, add ethyl acetate backflow, filter, evaporate to dryness filtrate, residue adds methyl alcohol and redissolves, as need testing solution; (2) thin layer detects: take Quercetin as contrast, the point sample on thin layer plate by need testing solution and Quercetin reference substance respectively, and with toluene-ethyl acetate-formic acid=5:4:1 for developping agent launches, aluminium choride develops the color, and inspects.
Preferably, described sherwood oil is the sherwood oil of boiling range 60-90 DEG C.
Preferably, in step (1), described sherwood oil is 20:1mL/g with the volume mass ratio of medicinal material to be checked.
Preferably, in step (1), described ethyl acetate is 25:1mL/g with the volume mass ratio of medicinal material to be checked.
Preferably, in step (1), described methyl alcohol is 1:1mL/g with the volume mass ratio of medicinal material to be checked.
Preferably, in step (1), the time of described ultrasonic extraction is 15 minutes.
Preferably, in step (1), the time of described backflow is 50 minutes.
Preferably, in step (2), described thin layer plate is silica G plate.
Preferably, in step (2), the concentration of described aluminium choride is 3%.
Preferably, in step (2), described in the wavelength inspected be 365nm.
Existing method (" glabrousleaf pittosporum seed quality standard Primary Study "), to contrast through the glabrousleaf pittosporum seed medicinal material of qualification, needs when detecting to prepare reference substance solution.Meanwhile, owing to contrasting with standard medicinal material, clearly do not need the index composition contrasted, must carry out extracted twice to medicinal material, ability Extraction and separation goes out more spot and detects.Can find out, owing to not finding the index composition in glabrousleaf pittosporum seed, the method entirety of making is comparatively loaded down with trivial details, consuming time longer.
And thin layer chromatography of the present invention, disclose index ingredient Quercetin new in glabrousleaf pittosporum seed, and with the spot that it is quality control, for the detection of glabrousleaf pittosporum seed, for the quality of monitoring glabrousleaf pittosporum seed medicinal material provides effective guarantee.Compared with the thin-layered chromatography detection method of existing report, method of the present invention does not need to prepare reference substance solution, only needs once to extract simultaneously, more simple and quick, is more suitable for actual application.
Obviously, according to foregoing of the present invention, according to ordinary technical knowledge and the customary means of this area, not departing under the present invention's above-mentioned basic fundamental thought prerequisite, the amendment of other various ways, replacement or change can also be made.
The embodiment of form by the following examples, is described in further detail foregoing of the present invention again.But this should be interpreted as that the scope of the above-mentioned theme of the present invention is only limitted to following example.All technology realized based on foregoing of the present invention all belong to scope of the present invention.
Accompanying drawing explanation
Fig. 1 is the efficient liquid phase testing result of Quercetin reference substance.Appearance time 10.842min
Fig. 2 is the efficient liquid phase testing result of glabrousleaf pittosporum seed, peak time: 10.765min.
Fig. 3 is the thin layer testing result of glabrousleaf pittosporum seed and Quercetin, is numbered blank, and numbering 1-10 is 10 batches of glabrousleaf pittosporum seeds, and numbering 11 is Quercetin reference substance
Embodiment
Agents useful for same and instrument all come from commercially available commodity, specific as follows:
Silica gel plate G: Qingdao Haiyang chemical industry subsidiary factory, lot number 20150108.
Quercetin reference substance: National Institute for Food and Drugs Control, lot number 100081-201408.
Sherwood oil: Chengdu Ke Long chemical reagent factory, lot number 014111401.
Ethyl acetate: Chengdu Ke Long chemical reagent factory, lot number 2015031801.
Methyl alcohol: Chengdu Ke Long chemical reagent factory, lot number 2015020501.
Formic acid: Chengdu Ke Long chemical reagent factory, lot number 2014031301.
Uv analyzer: Shanghai Jia Peng Science and Technology Ltd. model: ZF1-II.
Glabrousleaf pittosporum seed: through Chengdu University of Traditional Chinese Medicine professor Jiang Guihua qualification is the dry seed of Pittosporaceae Chart database plant sea gold PittosporumillicioidesMak.
Embodiment 1 glabrousleaf pittosporum seed detection method of the present invention
Get medicinal powder 2g to be checked, add sherwood oil (60 ~ 90 DEG C) 50mL, ultrasonic process 15 minutes, filter, discard filtrate.Residue adds ethyl acetate 50mL water-bath backflow 50min, and filter, filtrate evaporate to dryness, residue adds methyl alcohol 2mL makes dissolving, as need testing solution.
With Quercetin (1.5mg/mL) for reference substance.
Draw need testing solution 10 μ L, reference substance solution 5 μ L.Take silica G as adsorbent, with toluene-ethyl acetate-formic acid=5:4:1 (volume ratio) for developping agent, launch, take out, dry, spray with 3% aluminium choride test solution colour developing, inspect under ultraviolet lamp 365nm.
If test sample thin layer plate there is the corresponding spot of reference substance Quercetin, qualified glabrousleaf pittosporum seed medicinal material can be judged to be.
For proving to there is Quercetin in glabrousleaf pittosporum seed further, inventors performed high performance liquid chromatography checking,
The method of high performance liquid chromatography is as follows:
Efficient liquid-phase condition: water: methyl alcohol (53:47);
Agilent1200 high performance liquid chromatograph (Agilent company of the U.S.);
Chromatographic column is DiamonsilC18 post (250mm × 4.6mm, 5um); Mobile phase water: methyl alcohol (53:47), time 50min.
Result as depicted in figs. 1 and 2.Result shows, and near retention time 10.8min, glabrousleaf pittosporum seed exists the peak corresponding to Quercetin reference substance, proves that Quercetin can effectively as the index composition detecting glabrousleaf pittosporum seed quality of medicinal material.
Embodiment 2
According to the method for embodiment 1, glabrousleaf pittosporum seed medicinal material is detected, shown in result Fig. 3.
Result shows, and glabrousleaf pittosporum seed all has the corresponding spot of reference substance Quercetin on thin layer plate, clear spot, and Rf value moderate (Rf=0.6-0.7), is separated obviously with other spots, proves that Quercetin is suitable for the reference substance detected as glabrousleaf pittosporum seed thin layer.
Claims (10)
1. a thin layer detection method for glabrousleaf pittosporum seed, comprises the following steps:
(1) preparation of need testing solution:
Get medicinal material to be checked, pulverize, add the ultrasonic extraction of sherwood oil, filter, get filter residue, add ethyl acetate backflow, filter, evaporate to dryness filtrate, residue adds methyl alcohol and redissolves, as need testing solution;
(2) thin layer detects:
Take Quercetin as contrast, the point sample on thin layer plate by need testing solution and Quercetin reference substance respectively, with toluene-ethyl acetate-formic acid=5:4:1 for developping agent launches, aluminium choride develops the color, and inspects.
2. detection method according to claim 1, is characterized in that: described sherwood oil is the sherwood oil of boiling range 60-90 DEG C.
3. detection method according to claim 1 and 2, is characterized in that: in step (1), and described sherwood oil is 20:1mL/g with the volume mass ratio of medicinal material to be checked.
4. detection method according to claim 1, is characterized in that: in step (1), and described ethyl acetate is 25:1mL/g with the volume mass ratio of medicinal material to be checked.
5. detection method according to claim 1, is characterized in that: in step (1), and described methyl alcohol is 1:1mL/g with the volume mass ratio of medicinal material to be checked.
6. detection method according to claim 1, is characterized in that: in step (1), and the time of described ultrasonic extraction is 15 minutes.
7. detection method according to claim 1, is characterized in that: in step (1), and the time of described backflow is 50 minutes.
8. detection method according to claim 1, is characterized in that: in step (2), and described thin layer plate is silica G plate.
9. detection method according to claim 1, is characterized in that: in step (2), and the concentration of described aluminium choride is 3%.
10. detection method according to claim 1, is characterized in that: in step (2), described in the wavelength inspected be 365nm.
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Citations (4)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| US20060111310A1 (en) * | 2003-10-09 | 2006-05-25 | Chan Pui-Kwong | Composition comprising triterpene saponins and compounds with angeloyl functional group, methods for preparing same and uses thereof |
| WO2006116656A2 (en) * | 2005-04-27 | 2006-11-02 | Pacific Arrow Limited | Compositions comprising triterpene saponins and compounds with functional angeloyl groups for inhibition of venous insufficiency, leg swelling and tumors |
| CN102000278A (en) * | 2010-11-22 | 2011-04-06 | 李宗智 | Traditional Chinese medicine for treating amblyopia eye diseases |
| CN103100032A (en) * | 2012-11-15 | 2013-05-15 | 邓华伦 | Chinese herbal medicine for treating chest pains caused by dampness-heat of liver and gallbladder |
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2015
- 2015-09-18 CN CN201510601446.4A patent/CN105203693A/en active Pending
Patent Citations (4)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| US20060111310A1 (en) * | 2003-10-09 | 2006-05-25 | Chan Pui-Kwong | Composition comprising triterpene saponins and compounds with angeloyl functional group, methods for preparing same and uses thereof |
| WO2006116656A2 (en) * | 2005-04-27 | 2006-11-02 | Pacific Arrow Limited | Compositions comprising triterpene saponins and compounds with functional angeloyl groups for inhibition of venous insufficiency, leg swelling and tumors |
| CN102000278A (en) * | 2010-11-22 | 2011-04-06 | 李宗智 | Traditional Chinese medicine for treating amblyopia eye diseases |
| CN103100032A (en) * | 2012-11-15 | 2013-05-15 | 邓华伦 | Chinese herbal medicine for treating chest pains caused by dampness-heat of liver and gallbladder |
Non-Patent Citations (3)
| Title |
|---|
| TSUNG-HSIEN CHOU ET AL: "Phthalides from Pittosporum illicioides var. illicioides with Inhibitory Activity on Superoxide Generation and Elastase Release by Neutrophils", 《J. NAT. PROD.》 * |
| 张俊 等: "山枝仁质量标准初步研究", 《中药与临床》 * |
| 张俊: "川产山枝仁及其近缘种的生药学研究", 《中国优秀硕士学位论文全文数据库 医药卫生科技辑》 * |
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Application publication date: 20151230 |