CN110057931A - The detection method of reversed-phased high performace liquid chromatographic detection osmund ketone standard substance - Google Patents
The detection method of reversed-phased high performace liquid chromatographic detection osmund ketone standard substance Download PDFInfo
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- CN110057931A CN110057931A CN201910282644.7A CN201910282644A CN110057931A CN 110057931 A CN110057931 A CN 110057931A CN 201910282644 A CN201910282644 A CN 201910282644A CN 110057931 A CN110057931 A CN 110057931A
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- G—PHYSICS
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- G01N—INVESTIGATING OR ANALYSING MATERIALS BY DETERMINING THEIR CHEMICAL OR PHYSICAL PROPERTIES
- G01N30/00—Investigating or analysing materials by separation into components using adsorption, absorption or similar phenomena or using ion-exchange, e.g. chromatography or field flow fractionation
- G01N30/02—Column chromatography
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- G—PHYSICS
- G01—MEASURING; TESTING
- G01N—INVESTIGATING OR ANALYSING MATERIALS BY DETERMINING THEIR CHEMICAL OR PHYSICAL PROPERTIES
- G01N30/00—Investigating or analysing materials by separation into components using adsorption, absorption or similar phenomena or using ion-exchange, e.g. chromatography or field flow fractionation
- G01N30/02—Column chromatography
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Abstract
The invention discloses a kind of detection methods of reversed-phased high performace liquid chromatographic detection osmund ketone standard substance, comprising the following steps: dissolves test sample with methanol solution；It is the liquid-phase chromatographic column of filler using octadecylsilane chemically bonded silica；High performance liquid chromatograph is provided that with -0.1~0.5% aqueous acetic acid (B) of methanol (A) as mobile phase, gradient are as follows: 0~2min (20%A → 20%A), 2~20min (20%A → 45%A), 20~40min (45%A → 100%A), 40~50min (100%A → 20%A)；Flow velocity is 0.5ml/min；25 DEG C of column temperature；Detection wavelength 320nm；5 μ l of sample volume.High performance liquid chromatography response of the present invention is high, and detection error is small, and precision and accuracy are all preferable, is suitable for the assay of osmund ketone content in mixed system.
Description
Technical field
The present invention relates to a kind of detection methods of osmund ketone standard substance, it is more particularly related to a kind of reverse phase
The detection method of high performance liquid chromatography detection osmund ketone standard substance.
Background technique
Osmund ketone molecular formula are as follows: C10H10O3, molecular weight 178, No. CAS is 37079-84-8, and it is brown to be present in macro fungi birch
In pore fungi and Chinese medicine Japanese Flowering Fern Rhizome etc., belong to ketones component, structure is as follows:
Tool document report osmund ketone has anti-oxidant and killing cancer cell pharmacological activity, and osmund ketone detects in Japanese Flowering Fern Rhizome
When have been reported that and eluted using acetonitrile and phosphate aqueous solution as mobile phase, and there has been no osmund ketone phases in Inonotus obliquus at present
Close the document report of detection method.Therefore, it is necessary to explore, easier to operate, safety is higher, accurate osmund ketone is containing measurement
Determine method.
Summary of the invention
In view of the deficiencies of the prior art, the present invention intends to provide a kind of reversed-phased high performace liquid chromatographic detection
The detection method of osmund ketone standard substance in natural products mixed system.
To achieve the above object, the present invention adopts the following technical scheme:
A kind of detection method of reversed-phased high performace liquid chromatographic detection osmund ketone standard substance, it is mixed for detecting natural products
Osmund ketone standard substance in zoarium system, includes the following steps,
(1) test sample is dissolved with methanol solution；
It (2) the use of octadecylsilane chemically bonded silica is the liquid-phase chromatographic column of filler；
(3) high performance liquid chromatograph is provided that with -0.1~0.5% aqueous acetic acid (B) of methanol (A) as mobile phase,
Gradient are as follows: 0~2min (20%A → 20%A), 2~20min (20%A → 45%A), 20~40min (45%A →
100%A), 40~50min (100%A → 20%A)；Flow velocity is 0.5ml/min；25 DEG C of column temperature；Detection wavelength 320nm；Sample introduction
Measure 5 μ l.
Preferably, solvent used is that HPLC rank methanol, acetic acid and ultrapure water, sample are matched in the step (1)
Concentration processed is 0.1mg/ml~1.0mg/ml.
Preferably, mobile phase used is -0.5% aqueous acetic acid of methanol in the step (3).
Preferably, detector used is UV detector or DAD detector in the step (3).
The present invention compares have the advantage that compared with the prior art
(1) high performance liquid chromatography response is high, and detection error is small, and precision and accuracy are all preferable；
(2) method is easy to operate, practical, is suitable for the assay of osmund ketone content in mixed system；
(3) phosphoric acid commonly used in the prior art is eliminated in method mobile phase, has selected low-concentration acetic acid.
Detailed description of the invention
Fig. 1 is the sample for the detection method embodiment 1 that reversed-phased high performace liquid chromatographic of the present invention detects osmund ketone standard substance
Product map, the concentration of aqueous acetic acid is 0.1% in mobile phase；
Fig. 2 is the sample for the detection method embodiment 2 that reversed-phased high performace liquid chromatographic of the present invention detects osmund ketone standard substance
Product map, the concentration of aqueous acetic acid is 0.5% in mobile phase；
Fig. 3 is the detection that reversed-phased high performace liquid chromatographic of the present invention detects osmund ketone standard substance in Inonotus obliquus crude extract
The sample map of embodiment of the method 3；
Specific embodiment
The present invention is described in further detail With reference to embodiment, but the present invention is not limited only to the reality
Apply example.
Embodiment 1:
Chromatographic condition and system suitability: chromatographic column uses Agilent Extend-C18 (4.6 × 150mm, 5 μm)；
Mobile phase: methanol (A), 0.1% acetic acid water (B)；
Condition of gradient elution: 0~2min (20%A → 20%A), 2~20min (20%A → 45%A), 20~40min
(45%A → 100%A), 40~50min (100%A → 20%A)；Column temperature: 25 DEG C；Detection wavelength: 320nm；Flow velocity: 0.5mL/
min；Sample volume: 5 μ L.
The preparation of test solution: accurately weighed osmund ketone 0.5mg, precision be added chromatography methanol 1.0ml dissolution to get.
Measuring method: precision draw 5 μ l of test solution, inject high performance liquid chromatograph, measurement to get.
As a result: the normalization method content for measuring osmund ketone is 99.5%, and peak shape is symmetrical.Sample map is shown in Fig. 1.
Embodiment 2:
Chromatographic condition and system suitability: chromatographic column uses Agilent Extend-C18 (4.6 × 150mm, 5 μm)；
Mobile phase: methanol (A), 0.5% acetic acid water (B)；
Condition of gradient elution: 0~2min (20%A → 20%A), 2~20min (20%A → 45%A), 20~40min
(45%A → 100%A), 40~50min (100%A → 20%A)；Column temperature: 25 DEG C；Detection wavelength: 320nm；Flow velocity: 0.5mL/
min；Sample volume: 5 μ L.
The preparation of test solution: accurately weighed osmund ketone 0.5mg, precision be added chromatography methanol 1.0ml dissolution to get.
Measuring method: precision draw 5 μ l of test solution, inject high performance liquid chromatograph, measurement to get.
As a result: the normalization method content for measuring osmund ketone is 99.5%, and peak shape is symmetrical.Sample map is shown in Fig. 2.
Embodiment 3:
Chromatographic condition and system suitability: chromatographic column uses Agilent Extend-C18 (4.6 × 150mm, 5 μm)；
Mobile phase: methanol (A), 0.5% acetic acid water (B)；
Condition of gradient elution: 0~2min (20%A → 20%A), 2~20min (20%A → 45%A), 20~40min
(45%A → 100%A), 40~50min (100%A → 20%A)；Column temperature: 25 DEG C；Detection wavelength: 320nm；Flow velocity: 0.5mL/
min；Sample volume: 5 μ L.
The preparation of test solution: taking Inonotus obliquus powder about 5.0000g, is added the methanol of 100mL, ultrasonic extraction 1h,
Filter, filtrate decompression be recycled to it is dry, then with 4mL chromatography methanol dissolve, mistake 0.45 μM of filter membrane to get.
Measuring method: precision draw 5 μ l of test solution, inject high performance liquid chromatograph, measurement to get.
As a result: the content for measuring osmund ketone in Inonotus obliquus is 0.107%, and peak shape is symmetrical, and baseline separation is realized in coarse extraction.
Sample map is shown in Fig. 3.
The above is only a preferred embodiment of the present invention, protection scope of the present invention is not limited merely to above-mentioned implementation
Example, all technical solutions belonged under thinking of the present invention all belong to the scope of protection of the present invention, it is noted that for the art
Those of ordinary skill for, several improvements and modifications without departing from the principles of the present invention, these improvements and modifications
It should be regarded as protection scope of the present invention.
Claims (4)
1. a kind of detection method of reversed-phased high performace liquid chromatographic detection osmund ketone standard substance, for detecting natural products mixing
Osmund ketone standard substance in system, which is characterized in that include the following steps,
(1) test sample is dissolved with methanol solution；
It (2) the use of octadecylsilane chemically bonded silica is the liquid-phase chromatographic column of filler；
(3) high performance liquid chromatograph is provided that with -0.1~0.5% aqueous acetic acid (B) of methanol (A) elution for mobile phase
Gradient are as follows: 0~2min (20%A → 20%A), 2~20min (20%A → 45%A), 20~40min (45%A → 100%A),
40~50min (100%A → 20%A)；Flow velocity is 0.5ml/min；25 DEG C of column temperature；Detection wavelength 320nm；5 μ l of sample volume.
2. a kind of detection method of reversed-phased high performace liquid chromatographic detection osmund ketone standard substance as described in claim 1,
It is characterized in that, in the step (1), solvent used is HPLC rank methanol, acetic acid and ultrapure water, and sample preparation concentration is
0.1mg/ml~1.0mg/ml.
3. a kind of detection method of reversed-phased high performace liquid chromatographic detection osmund ketone standard substance as described in claim 1,
It is characterized in that, in the step (3), mobile phase used is -0.5% aqueous acetic acid of methanol.
4. a kind of detection method of reversed-phased high performace liquid chromatographic detection osmund ketone standard substance as described in claim 1,
It is characterized in that, detector used is UV detector or DAD detector in the step (3).
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Cited By (1)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN113069484A (en) * | 2021-03-12 | 2021-07-06 | 黑龙江中医药大学 | Anti-aging medicine and preparation method of microcapsule preparation thereof |
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| CN101690739A (en) * | 2009-06-30 | 2010-04-07 | 长春师范学院 | Preparation method of dogbane leaf extractive |
| WO2018062895A1 (en) * | 2016-09-30 | 2018-04-05 | 주식회사 코팜 | Composition comprising osmundacetone or pharmaceutically acceptable salt thereof for preventing or treating bone disease |
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Patent Citations (2)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN101690739A (en) * | 2009-06-30 | 2010-04-07 | 长春师范学院 | Preparation method of dogbane leaf extractive |
| WO2018062895A1 (en) * | 2016-09-30 | 2018-04-05 | 주식회사 코팜 | Composition comprising osmundacetone or pharmaceutically acceptable salt thereof for preventing or treating bone disease |
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Cited By (2)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN113069484A (en) * | 2021-03-12 | 2021-07-06 | 黑龙江中医药大学 | Anti-aging medicine and preparation method of microcapsule preparation thereof |
| CN113069484B (en) * | 2021-03-12 | 2022-05-13 | 黑龙江中医药大学 | Preparation method of microcapsule preparation of anti-aging medicine |
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Application publication date: 20190726 |