CN104007213B - The method for building up of Chinese pothos herb medicinal materials fingerprint and finger-print thereof - Google Patents
The method for building up of Chinese pothos herb medicinal materials fingerprint and finger-print thereof Download PDFInfo
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- CN104007213B CN104007213B CN201310519444.1A CN201310519444A CN104007213B CN 104007213 B CN104007213 B CN 104007213B CN 201310519444 A CN201310519444 A CN 201310519444A CN 104007213 B CN104007213 B CN 104007213B
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Abstract
The present invention discloses a kind of method for building up and finger-print thereof of Chinese pothos herb medicinal materials fingerprint, relate to the fingerprint pattern technology field of Chinese crude drug, the method comprises preparation and the high performance liquid chromatography testing conditions of test sample, gets Chinese pothos herb medicinal powder and is placed in test tube, adds proper amount of methanol solution and soaks 24h, ultrasonic vibration 40min, let cool, shake up, coarse filtration, use filtering with microporous membrane again, filtrate is as need testing solution; Carry out high performance liquid chromatography detection to need testing solution, chromatographic column take octadecylsilane chemically bonded silica as filler, and mobile phase is acetonitrile-0.085% phosphoric acid; Sample size is 10 ~ 25 μ L; Adopt gradient elution mode, determined wavelength 310nm, flow velocity is 0.8mL/min, and column temperature is 20 DEG C ~ 35 DEG C, obtains Chinese pothos herb medicinal materials fingerprint, and the Chinese pothos herb medicinal materials fingerprint that the present invention sets up effectively can monitor the quality of Chinese pothos herb medicinal material and mirror determines whether it is true or false.
Description
Technical field
The present invention relates to the fingerprint pattern technology field of Chinese crude drug, especially the method for building up of Chinese pothos herb medicinal materials fingerprint and finger-print thereof.
Background technology
Although Chinese medicine has had the application development history of several thousand, how the quality of effectively evaluating Chinese crude drug quality, has been the Focal point and difficult point of Chinese crude drug research and apply always.Along with the development of science and technology, finger-print Quality Control technology is suggested at the field of Chinese medicines and is extensively approved, its application in Chinese crude drug Quality Control also gets more and more; Fingerprint of Chinese medicine materia refers to that Chinese crude drug is after suitably processing, certain analysis means and detecting instrument is adopted to obtain, the collection of illustrative plates of this Chinese crude drug characteristic can be indicated, it can reflect one of the most effective means of Chinese crude drug inherent quality more all sidedly at present stage, have also been obtained the accreditation of international community.
Chinese pothos herb is the herb of aroid Chinese pothos herb, has dispeling wind and dehumidification, promoting blood circulation to remove blood stasis, and disappear long-pending and cough-relieving effect, can be used for treating traumatic injury, advanced schistosomiasis, hepatosplenomegaly, rheumatism joint inflammation.But there is no the quality standard of Chinese pothos herb medicinal material at present, the control of Chinese pothos herb quality of medicinal material is just seemed very weak, only includes microscopical characters etc. and check routinely, lack perfect quality evaluation system, be difficult to reach the effective control to Chinese pothos herb quality.
Summary of the invention
Problem to be solved by this invention is to provide a kind of method for building up and finger-print thereof of Chinese pothos herb medicinal materials fingerprint, utilizes this collection of illustrative plates can monitor the quality of Chinese pothos herb medicinal material and discern the false from the genuine.
In order to solve the problems of the technologies described above, the technical solution adopted in the present invention is: the method for building up of this Chinese pothos herb medicinal materials fingerprint comprises the steps:
(1) preparation of test sample:
Get Chinese pothos herb medicinal powder 1.0g-5.0g and be placed in test tube, add 55%-65% methyl alcohol 20mL-100mL, soak 24h, ultrasonic vibration 40min, lets cool, and shakes up, coarse filtration, then uses filtering with microporous membrane, and filtrate is as need testing solution;
(2) high performance liquid chromatography detects:
Draw above-mentioned steps (1) gained need testing solution, inject high performance liquid chromatograph and carry out high performance liquid chromatography detection, the finger-print in record 60min:
Wherein, fingerprint chromatogram condition is:
Adopt octadecylsilane chemically bonded silica to be the chromatographic column of filler, 4.6 × 250mm, 5 μm, mobile phase is acetonitrile-0.085% phosphoric acid; Adopt gradient elution mode: 0min → 10min → 20min → 30min → 40min → 50min → 60min, acetonitrile 10% → 15% → 20% → 25% → 30% → 35% → 40%; Sample size is 10 ~ 25 μ L; Determined wavelength is 310nm, and flow velocity is 0.8mL/min, and column temperature is 20 DEG C ~ 35 DEG C.
The finger-print of this Chinese pothos herb medicinal material, is made up of 14 total fingerprint peakses, and relative retention time ranges and the relative standard deviation of 14 total fingerprint peakses of described finger-print are as follows:
No. 1 peak: 0.226 ~ 0.233, RSD is 1.03%;
No. 2 peak: 0.453 ~ 0.458, RSD are 0.36%;
No. 3 peak: 0.747 ~ 0.761, RSD are 0.60%;
No. 4 peak: 0.864 ~ 0.887, RSD are 0.77%;
No. 5 peak: 0.905 ~ 0.908, RSD are 0.07%;
No. 6 peak: 0.950 ~ 0.968, RSD are 0.65%;
No. 7 peak: 1, RSD are 0%
No. 8 peak: 1.100 ~ 1.132, RSD are 0.76%;
No. 9 peak: 1.176 ~ 1.198, RSD are 0.63%;
No. 10 peak: 1.216 ~ 1.240, RSD are 0.62%;
No. 11 peak: 1.371 ~ 1.398, RSD are 0.65%;
No. 12 peak: 1.820 ~ 1.839, RSD are 0.31%;
No. 13 peak: 1.894 ~ 1.907, RSD are 0.23%;
No. 14 peak: 1.977 ~ 2.009, RSD are 0.51%.
The present invention compared with prior art, has following beneficial effect:
The present invention establishes the method for building up of Chinese pothos herb medicinal materials fingerprint, the standard finger-print of Chinese pothos herb medicinal material can be obtained by the method, relatively have the presence or absence at peak in finger-print, effectively can monitor the quality of Chinese pothos herb medicinal material, the perfect quality evaluation system of Chinese pothos herb medicinal material, for comprehensive, effective control of Chinese pothos herb quality of medicinal material provides theory and practice basis.
Accompanying drawing explanation
Fig. 1 is this Chinese pothos herb HPLC-FPS.
Fig. 2 is 10 batches of Chinese pothos herb medicinal material original fingerprint collection of illustrative plates.
Embodiment
Below in conjunction with attached Example, the invention will be further described:
The present embodiment is fingerprint to adopting from 10 batches of Chinese pothos herb medicinal materials of Different producing area and the finger-print that obtains accordingly:
10 batches of Chinese pothos herb medicinal materials picking up from Different producing area in different time comprise Nanning, Guilin, Liuzhou, Wuming, Guangxi, Yunnan, Guangxi Gold show, Guangxi Yulin; The essential informations such as each Chinese pothos herb medicinal material test sample source are as table 1:
Instrument and medicine: use UltiMate3000 type high performance liquid chromatograph; Chinese pothos herb medicinal material totally 10 batches, is all purchased from medium-height grass pharmacy, and other reagent is chromatographically pure or analyzes pure.
Set up Chinese pothos herb medicinal materials fingerprint as follows:
(1) preparation of need testing solution:
Precision takes the test tube that Chinese pothos herb medicinal powder 1.0g is placed in band plug, and precision adds 60% methyl alcohol 20mL, and soak 24h, ultrasonic process 40min, lets cool, and supply the weight of loss with corresponding methanol solution, shake up, coarse filtration, filtrate is with 0.45
filtering with microporous membrane, filtrate is as need testing solution;
(2) high performance liquid chromatography detects:
Draw above-mentioned steps (1) gained need testing solution, inject high performance liquid chromatograph and carry out high performance liquid chromatography detection, the finger-print in record 60min:
Wherein, fingerprint chromatogram condition is:
Adopt DionexC18 chromatographic column (4.6 × 250mm, 5 μm), mobile phase is acetonitrile-0.085% phosphoric acid; Adopt gradient elution mode: 0min → 10min → 20min → 30min → 40min → 50min → 60min, acetonitrile 10% → 15% → 20% → 25% → 30% → 35% → 40%; Sample size is 20 μ L; Determined wavelength is 310nm, and flow velocity is 0.8mL/min, and column temperature is 25 DEG C, analyzes test sample with this understanding, obtains the finger-print of Chinese pothos herb medicinal material, as shown in Figure 1.
According to the method described above, HPLC finger-print is established to 10 batches of Chinese pothos herb medicinal materials, as shown in Figure 2, by com-parison and analysis, determine 14 total fingerprint peakses, i.e. characteristic peak, with No. 7 peaks for internal reference peak, its retention time is 20.59 ~ 20.97min, RSD is 0.68%, calculate the relative retention time of each total fingerprint peaks, each total fingerprint peaks relative retention time ranges and relative standard deviation specific as follows:
No. 1 peak: 0.226 ~ 0.233, RSD is 1.03%;
No. 2 peak: 0.453 ~ 0.458, RSD are 0.36%;
No. 3 peak: 0.747 ~ 0.761, RSD are 0.60%;
No. 4 peak: 0.864 ~ 0.887, RSD are 0.77%;
No. 5 peak: 0.905 ~ 0.908, RSD are 0.07%;
No. 6 peak: 0.950 ~ 0.968, RSD are 0.65%;
No. 7 peak: 1, RSD are 0;
No. 8 peak: 1.100 ~ 1.132, RSD are 0.76%;
No. 9 peak: 1.176 ~ 1.198, RSD are 0.63%;
No. 10 peak: 1.216 ~ 1.240, RSD are 0.62%;
No. 11 peak: 1.371 ~ 1.398, RSD are 0.65%;
No. 12 peak: 1.820 ~ 1.839, RSD are 0.31%;
No. 13 peak: 1.894 ~ 1.907, RSD are 0.23%;
No. 14 peak: 1.977 ~ 2.009, RSD are 0.51%.
These total fingerprint peakses constitute the fingerprint characteristic of Chinese pothos herb medicinal material, can be used as the finger-print of Chinese pothos herb medicinal material.
Control sample spectrogram is generated after the Chinese pothos herb medicinal material chromatogram coupling of 10 different batches, then be reference spectrum according to this, relatively 10 different batches Chinese pothos herb spectrograms similarity with it, according to the similarity of the relative retention time between Cosin method and correlation coefficient process different batches spectrogram all more than 0.99.
Therefore, by building HPLC finger-print and analysis, can from the material base of Chinese pothos herb pharmacological action, the quality condition of effective evaluation Chinese pothos herb medicinal material, the quality reaching monitoring Chinese pothos herb medicinal material and the object of discerning the false from the genuine.
Claims (2)
1. a method for building up for Chinese pothos herb medicinal materials fingerprint, is characterized in that comprising the steps:
(1) preparation of need testing solution:
Get Chinese pothos herb medicinal powder 1.0g-5.0g and be placed in test tube, add 55%-65% methyl alcohol 20mL-100mL, soak 24h, ultrasonic vibration 40min, lets cool, and shakes up, coarse filtration, then uses filtering with microporous membrane, and filtrate is as need testing solution;
(2) high performance liquid chromatography detects:
Draw above-mentioned steps (1) gained need testing solution, inject high performance liquid chromatograph and carry out high performance liquid chromatography detection, the finger-print in record 60min:
Wherein, fingerprint chromatogram condition is:
Adopt octadecylsilane chemically bonded silica to be the chromatographic column of filler, 4.6 × 250mm, 5 μm, mobile phase is acetonitrile-0.085% phosphoric acid; Adopt gradient elution mode: 0min → 10min → 20min → 30min → 40min → 50min → 60min, acetonitrile 10% → 15% → 20% → 25% → 30% → 35% → 40%; Sample size is 10 ~ 25 μ L; Determined wavelength is 310nm, and flow velocity is 0.8mL/min, and column temperature is 20 DEG C ~ 35 DEG C.
2. the finger-print of Chinese pothos herb medicinal material set up of the method for building up of a Chinese pothos herb medicinal materials fingerprint as claimed in claim 1, it is characterized in that: finger-print is made up of 14 total fingerprint peakses, and relative retention time ranges and the relative standard deviation of 14 total fingerprint peakses of described finger-print are as follows:
No. 1 peak: 0.226 ~ 0.233, RSD is 1.03%;
No. 2 peak: 0.453 ~ 0.458, RSD are 0.36%;
No. 3 peak: 0.747 ~ 0.761, RSD are 0.60%;
No. 4 peak: 0.864 ~ 0.887, RSD are 0.77%;
No. 5 peak: 0.905 ~ 0.908, RSD are 0.07%;
No. 6 peak: 0.950 ~ 0.968, RSD are 0.65%;
No. 7 peak: 1, RSD are 0%;
No. 8 peak: 1.100 ~ 1.132, RSD are 0.76%;
No. 9 peak: 1.176 ~ 1.198, RSD are 0.63%;
No. 10 peak: 1.216 ~ 1.240, RSD are 0.62%;
No. 11 peak: 1.371 ~ 1.398, RSD are 0.65%;
No. 12 peak: 1.820 ~ 1.839, RSD are 0.31%;
No. 13 peak: 1.894 ~ 1.907, RSD are 0.23%;
No. 14 peak: 1.977 ~ 2.009, RSD are 0.51%.
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| CN105092724B (en) * | 2015-03-23 | 2017-07-14 | 广东省第二中医院（广东省中医药工程技术研究院） | The construction method and its HPLC finger-prints of Chinese pothos herb HPLC finger-prints |
| CN105092771B (en) * | 2015-03-23 | 2017-04-26 | 广东省第二中医院（广东省中医药工程技术研究院） | Thin-layer chromatography rapid identification method for Pothos chinensis |
| CN113533605A (en) * | 2021-07-14 | 2021-10-22 | 保定天浩制药有限公司 | Liver-refreshing particle fingerprint detection method |
Citations (2)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| EP1915997A1 (en) * | 2005-08-12 | 2008-04-30 | KOHNO, Kenji | Agent for hair growth |
| CA2822178A1 (en) * | 2011-01-11 | 2012-07-19 | Stichting Dienst Landbouwkundig Onderzoek | Serratia plymuthica for biological control of bacterial plant pathogens |
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| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| EP1915997A1 (en) * | 2005-08-12 | 2008-04-30 | KOHNO, Kenji | Agent for hair growth |
| CA2822178A1 (en) * | 2011-01-11 | 2012-07-19 | Stichting Dienst Landbouwkundig Onderzoek | Serratia plymuthica for biological control of bacterial plant pathogens |
Non-Patent Citations (4)
| Title |
|---|
| 柚子枫挥发油化学成分研究;覃振林等;《时珍国医国药》;20120520;第23卷(第5期);第1099～1100页 * |
| 毛细管气相色谱/质谱法定性巴岩油的化学成份;季怡萍等;《福建分析测试》;19950215;第4卷(第1期);第204～208页 * |
| 石蒲藤的生药学研究;马丽莎等;《今日药学》;20080615;第18卷(第3期);第36～37页 * |
| 藏药绿萝花中总黄酮含量的提取工艺研究;李文茂等;《北方园艺》;20130315(第5期);第144～146页 * |
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