CN109187841A - The thin-layer identification method of American lotus - Google Patents
The thin-layer identification method of American lotus Download PDFInfo
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- CN109187841A CN109187841A CN201811009945.4A CN201811009945A CN109187841A CN 109187841 A CN109187841 A CN 109187841A CN 201811009945 A CN201811009945 A CN 201811009945A CN 109187841 A CN109187841 A CN 109187841A
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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
- G01N30/90—Plate chromatography, e.g. thin layer or paper 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
- G01N30/90—Plate chromatography, e.g. thin layer or paper 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
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Abstract
The invention discloses the thin-layer identification method of American lotus, includes the following steps: that (1) takes American lotus to be identified, smashed after drying, it takes 0.25g American lotus powder in conical flask, adds anhydrous methanol 25ml, ultrasonic 30min, filtration, takes subsequent filtrate as test solution；(2) Berberine hydrochloride is taken, the solution that concentration is 800ug/ml is configured to, as reference substance solution；(3) test solution and control solution are drawn to be put respectively on same silica gel g thin-layer plate, it is unfolded using volume ratio for 60 DEG C~90 DEG C petroleum ether-chloroform-methanol of 5:3:2 as solvent, it takes out, it dries, sets and inspected under 365nm ultraviolet lamp, in sample chromatogram, compared with reference substance chromatography, in the corresponding position that Rf value is 0.93 ± 0.02, the spot of same color is shown, while sample chromatogram also spot occurs on the position that Rf value is 0.35 ± 0.05 and 0.77 ± 0.05.The method of the present invention facilitates the quality control of American lotus, provides scientific basis to formulate the quality standard of American lotus.
Description
Technical field
The present invention relates to a kind of thin-layer identification methods of American lotus, belong to Analysis of Chinese Traditional Medicine technical field.
Background technique
American lotus (Lysimachia davurica Ledeb.) is the ranunculaceae plant coptis
(CoptischinensisFranch.), the triangle leaf coptis (C.deltoideaC.Y.ChengetHsiao) or cloud connect
(C.teetaWall.) flower opened, document report, the amino acid and mineral matter element useful to human body rich in.It is yellow
Continuous cropping is a kind of traditional Chinese medicine, has very strong antibacterial purging intense heat ability, and modern medicine study shows also there is hypoglycemic, drop blood
More than 20 function such as rouge, anti-platelet aggregation.Flower has weight as plant nutrient ingredient richness product position, development and utilization American lotus
The economic value and social value wanted.Thin layer identifies the quality control for facilitating American lotus.Currently, pharmacopeia and each province's Chinese medicine mark
The quasi- record without American lotus thin-layer identification method.
Summary of the invention
The purpose of the present invention is to provide the thin-layer identification methods of American lotus.
The thin-layer identification method of American lotus provided by the invention includes the following steps:
(1) American lotus to be identified is taken, is smashed after drying, takes 0.25g American lotus powder in conical flask, adds anhydrous methanol
25ml, ultrasonic 30min, filtration, take subsequent filtrate as test solution；
(2) Berberine hydrochloride is taken, the solution that concentration is 800ug/ml is configured to, as reference substance solution；
(3) test solution and control solution are drawn to be put respectively on same lamellae, is the 60 of 5:3:2 with volume ratio
DEG C~90 DEG C of petroleum ether-chloroform-methanol be solvent expansion, take out, dry, set and inspected under 365nm ultraviolet lamp, test sample
In chromatography, compared with reference substance chromatography, in the corresponding position that Rf value is 0.93 ± 0.02, the spot of same color is shown, is supplied simultaneously
Also there is spot in the position that Rf value is 0.35 ± 0.05 and 0.77 ± 0.05 in test product chromatography.
Further, expansion temperature is 29 DEG C, development distance 9.0cm in step (3), and point sample amount is 10 μ l.
Discrimination method of the present invention facilitates the quality control of American lotus, provides science to formulate the quality standard of American lotus
Foundation is laid a good foundation for the sustainable use and exploitation of American lotus.
Detailed description of the invention
Fig. 1 is the thin layer identification chromatogram of test sample and reference substance, and wherein A is Berberine hydrochloride reference substance, and 1~6 successively
For 20180310-1-1,20180310-2-1,20180310-3-1,20180310-4-1,20180310-5-1,20180316-
6-1 American lotus test sample.
Fig. 2 is the test sample thin-layer chromatogram using different lamellaes, and wherein the plate on the left side is silica gel H lamellae, the right
Plate be silica gel g thin-layer plate, 1~6 is followed successively by 20180310-1-1,20180310-2-1,20180310-3-1,20180310-
4-1,20180310-5-1,20180316-6-1 American lotus test sample.
Fig. 3 is the test sample thin-layer chromatogram that is unfolded under condition of different temperatures, and wherein the left side is 6 DEG C, and the right is 29 DEG C, 1
~6 are followed successively by 20180310-1-1,20180310-2-1,20180310-3-1,20180310-4-1,20180310-5-1,
20180316-6-1 American lotus test sample.
Fig. 4 is the test sample thin-layer chromatogram under the conditions of different point sample amounts, and wherein the left side is 10 μ l point sample amounts, and centre is 20
μ l point sample amount, the right be 27 μ l point sample amounts, 1~6 be followed successively by 20180310-1-1,20180310-2-1,20180310-3-1,
20180310-4-1,20180310-5-1,20180316-6-1 American lotus test sample.
Fig. 5 is the test sample thin-layer chromatogram under the conditions of different development distances, wherein the development distance 7.7cm on the left side, in
Between be 8.3cm, the right 9cm, 1~6 be followed successively by 20180310-1-1,20180310-2-1,20180310-3-1,
20180310-4-1,20180310-5-1,20180316-6-1 American lotus test sample.
Specific embodiment
The present invention is described in further details With reference to embodiment, but protection scope of the present invention is not limited to
In this.
A, instrument: BJ-150 type high-speed multifunctional pulverizer, No. 2 pharmacopeia sieves, thin layer of glass plate (100mX200m), HS-
3120 ultrasonic cleaners, FA2004 analyze electronic balance (upper current chart level instruments and meters Co., Ltd), 101-1-S type electric heating drum
Wind drying box (Chengdu Ya Yuan Science and Technology Ltd.), UV-8 ultraviolet analysis instrument for three purposed (Keda Instrument Plant, Wuxi), silica gel g thin-layer plate
(Haiyang Chemical Plant, Qingdao), silica gel H lamellae (Haiyang Chemical Plant, Qingdao), micro syringe, conical flask, internal diameter 0.5mm long
100mm glass capillary (production of instrument plant of Huaxi Medical Univ), 20cm × 10cm chromatography cylinder (vertical), thermometer, funnel, filter
Paper.
B, reagent: anhydrous methanol, methanol, petroleum ether (60-90 DEG C), chloroform, ammonium hydroxide, sodium carboxymethylcellulose are (real
Test reagent, Chengdu section Long Huagongshijichang), (Sichuan Wei Keqi biotechnology is limited for Berberine hydrochloride traditional Chinese chemical contrast
Company), remaining reagent is that analysis is pure.
C, sample source is numbered
Embodiment 1
(1) preparation of test solution: American lotus to be identified is taken, is smashed after 60 DEG C of constant temperature dryings, takes 0.25g American lotus
Powder adds anhydrous methanol 25ml, ultrasonic 30min in conical flask, and filtration takes subsequent filtrate as test solution；
(2) preparation of reference substance solution: taking Berberine hydrochloride, the solution that concentration is 800ug/ml is configured to, as control
Product solution；
(3) it thin-layer chromatography condition, expansion mode and inspects
Lamellae: silica gel g thin-layer plate；
Solvent: petroleum ether (60 DEG C~90 DEG C)-chloroform-methanol (5:3:2)；
Point sample amount: 10 μ l；
Development distance: 9.0cm；
Expansion temperature: 29 DEG C；
Expansion mode: double flute expansion cylinder, it is vertical (20cm × 10mm)；Ascending development first uses ammonium hydroxide presaturation 30min, abandons
Ammonium hydroxide is removed, is unfolded, takes out, dries；
It inspects: setting and inspected under 365nm ultraviolet lamp；
As a result: in sample chromatogram, compared with reference substance chromatography, in the corresponding position that Rf value is 0.91~0.95, showing phase
With the spot of color, while sample chromatogram is also shown and above-mentioned spot on the position that Rf value is 0.30~0.37 and 0.72~0.82
The identical spot of point color.
The screening of 2 thin layer condition of embodiment
Test solution used by the present embodiment is same as Example 1.
(1) different lamellaes are investigated
Test solution point is drawn respectively on silica gel H lamellae and silica gel g thin-layer plate, by the thin-layer chromatography of embodiment 1
Condition and expansion mode expansion, set and inspect under 365nm ultraviolet lamp, thin-layer chromatogram is as shown in Fig. 2, the results show that sample is in silicon
Expansion effect is bad on glue H lamellae, and spot separating effect is poor, and in contrast, the expansion effect on silica gel g thin-layer plate is more
For ideal, spot is relatively clear.
(2) expansion temperature is investigated
Test solution is drawn respectively o'clock in (manufacturer and production batch phase on two identical silica gel g thin-layer plates
Together), it is unfolded by the thin-layer chromatography condition and expansion mode of embodiment 1, expansion temperature is only set to 6 DEG C and 29 DEG C, is set
It is inspected under 365nm ultraviolet lamp, thin-layer chromatogram is as shown in figure 3, the results show that spot more rounding is clear when expansion temperature is 29 DEG C
It is clear.
(3) point sample amount is investigated
Test solution is drawn respectively o'clock in (manufacturer and production batch phase on three identical silica gel g thin-layer plates
Together), it is unfolded by the thin-layer chromatography condition and expansion mode of embodiment 1, point sample amount is only set to 10 μ l, 20 μ l, 27 μ l, is set
It is inspected under 365nm ultraviolet lamp, thin-layer chromatogram clear spot and does not drag as shown in figure 4, the results show that when point sample amount is 10 μ l
Tail, point sample amount is more, and hangover is more obvious.
(4) development distance is investigated
Test solution is drawn respectively o'clock in (manufacturer and production batch phase on three identical silica gel g thin-layer plates
Together), by embodiment 1 thin-layer chromatography condition and expansion mode be unfolded, only by development distance be set to 7.7cm, 8.3cm,
9.0cm sets and inspects under 365nm ultraviolet lamp, and thin-layer chromatogram is as shown in figure 5, the results show that when development distance is 7cm or so, out
Existing 4 points, with the increase of development distance, the unstable spot of one of ingredient is just unobvious, when development distance is 9cm
Three spots are apparent.
Claims (2)
1. the thin-layer identification method of American lotus, it is characterised in that include the following steps:
(1) American lotus to be identified is taken, is smashed after drying, takes 0.25g American lotus powder in conical flask, adds anhydrous methanol
25ml, ultrasonic 30min, filtration, take subsequent filtrate as test solution；
(2) Berberine hydrochloride is taken, the solution that concentration is 800ug/ml is configured to, as reference substance solution；
(3) test solution and control solution are drawn to be put respectively on same silica gel g thin-layer plate, is 5:3:2's with volume ratio
60 DEG C~90 DEG C petroleum ether-chloroform-methanol are solvent expansion, take out, dry, set and inspect under 365nm ultraviolet lamp, for examination
In product chromatography, compared with reference substance chromatography, in the corresponding position that Rf value is 0.93 ± 0.02, the spot of same color is shown, simultaneously
Also there is spot in the position that Rf value is 0.35 ± 0.05 and 0.77 ± 0.05 in sample chromatogram.
2. the thin-layer identification method of American lotus according to claim 1, it is characterised in that: expansion temperature is in step (3)
29 DEG C, development distance 9cm, point sample amount is 10 μ l.
Priority Applications (1)
| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| CN201811009945.4A CN109187841B (en) | 2018-08-31 | 2018-08-31 | Thin-layer identification method of coptidis flos |
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| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| CN201811009945.4A CN109187841B (en) | 2018-08-31 | 2018-08-31 | Thin-layer identification method of coptidis flos |
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| CN109187841A true CN109187841A (en) | 2019-01-11 |
| CN109187841B CN109187841B (en) | 2020-11-13 |
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Citations (6)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| JP2001270835A (en) * | 2000-03-15 | 2001-10-02 | Korea Yakult Co Ltd | Extract of perilla frutescens var. acuta kudo effective for prophylaxis and therapy of gastric ulcer, its use and process for obtaining berberine from the extract |
| JP2001302525A (en) * | 2000-02-16 | 2001-10-31 | Shiseido Co Ltd | External preparation for skin care |
| EP1454993A1 (en) * | 2003-03-05 | 2004-09-08 | Max-Planck-Gesellschaft Zur Förderung Der Wissenschaften E.V. | Method for identifying the function of a gene |
| CN1733105A (en) * | 2005-08-18 | 2006-02-15 | 贵阳云岩西创药物科技开发有限公司 | Preparation for treating gynecological disease, its preparation process and quality control method |
| CN101928285A (en) * | 2010-08-05 | 2010-12-29 | 重庆市中药研究院 | Method for extracting major alkaloids from rhizoma coptidis |
| CN104478878A (en) * | 2014-11-08 | 2015-04-01 | 吕梁学院 | Method for separation and preparation of alkaloids from walnut green seedcase |
-
2018
- 2018-08-31 CN CN201811009945.4A patent/CN109187841B/en active Active
Patent Citations (6)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| JP2001302525A (en) * | 2000-02-16 | 2001-10-31 | Shiseido Co Ltd | External preparation for skin care |
| JP2001270835A (en) * | 2000-03-15 | 2001-10-02 | Korea Yakult Co Ltd | Extract of perilla frutescens var. acuta kudo effective for prophylaxis and therapy of gastric ulcer, its use and process for obtaining berberine from the extract |
| EP1454993A1 (en) * | 2003-03-05 | 2004-09-08 | Max-Planck-Gesellschaft Zur Förderung Der Wissenschaften E.V. | Method for identifying the function of a gene |
| CN1733105A (en) * | 2005-08-18 | 2006-02-15 | 贵阳云岩西创药物科技开发有限公司 | Preparation for treating gynecological disease, its preparation process and quality control method |
| CN101928285A (en) * | 2010-08-05 | 2010-12-29 | 重庆市中药研究院 | Method for extracting major alkaloids from rhizoma coptidis |
| CN104478878A (en) * | 2014-11-08 | 2015-04-01 | 吕梁学院 | Method for separation and preparation of alkaloids from walnut green seedcase |
Non-Patent Citations (4)
| Title |
|---|
| COICHI KURONO 等: "Analysis of Constituents in crude drugs by Thin-layer Chromatography.I. Studiers on the quantitative Analysis of berberine in Coptis japonica MAKINO by Thin-layer Chromatography", 《YAKUGAKU ZASSHI》 * |
| 刘法锦 等: "黄连吴茱萸药对化学成分的薄层色谱定性研究", 《中国实验方剂学杂志》 * |
| 方周伯 等: "中国黄连愈伤组织的诱导与次生代谢产物", 《西南农业学报》 * |
| 朱天明等: "盐酸小檗碱及其片剂中有关物质检查方法的探讨", 《中国药品标准》 * |
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