CN105241996A - Thin-layer chromatography identification method of carbonized herb processed product - Google Patents

Thin-layer chromatography identification method of carbonized herb processed product Download PDF

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CN105241996A
CN105241996A CN201510758058.7A CN201510758058A CN105241996A CN 105241996 A CN105241996 A CN 105241996A CN 201510758058 A CN201510758058 A CN 201510758058A CN 105241996 A CN105241996 A CN 105241996A
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charcoal
medicinal material
processed product
solution
control medicinal
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谭登平
程学仁
朱德全
林振东
刘丽萍
王闽予
陈向东
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Guangdong Yifang Pharmaceutical Co Ltd
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Guangdong Yifang Pharmaceutical Co Ltd
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Abstract

The invention discloses a thin-layer chromatography identification method of a carbonized herb processed product. The method comprises the steps that 1, sample powder is taken, hydrochloric acid is added, heating is conducted for hydrolysis, filtration is conducted, filtrate is extracted through ethyl acetate or ethyl ether, extract liquor is evaporated to dryness, and residues are dissolved through methyl alcohol to serve as a test sample solution; 2, reference medicinal materials are taken, and then a reference medicinal material solution is prepared through the method for preparing a test sample; 3, the test sample solution and the reference medicinal material solution are sucked and dripped on a same silica gel GF254 thin-layer plate, developing is conducted by taking methylbenzene, ethyl formate and formic acid as developing solvents according to the ratio of 2-8 to 2-8 to 0.1-1, and the thin-layer plate is taken out and dried in the air; 4, the thin-layer plate is viewed under a 254 nm ultraviolet lamp, and principal spots with the same color are showed on the positions, corresponding to the chromatography of the reference medicinal materials, in the test sample chromatography. The identification method is rapid, comprehensive and high in specificity, the requirements of the carbonizing drug characteristic of the carbonized herb product can be embodied, and a certain reference basis is provided for establishment of quality standards of the carbonized herb products.

Description

A kind of TLC Identification of charcoal drug processed product
Technical field
The invention belongs to traditional Chinese medicine quality detection technique field, be specifically related to a kind of TLC Identification of charcoal drug processed product.
Background technology
The use history of existing more than 2,000 year so far of Charcoal of Chinese Drugs, that a kind of purposes is comparatively wide, the Chinese medicine preparation product of determined curative effect, so far tens of kinds are still had to be commonly used by clinical, especially the treatment of hemorrhagic disease is more common in, as carbonized hair, charred HERBA CIRSII JAPONICI, field thistle charcoal, charred RADIX SANGUISORBAE, charred RADIX RUBIAE, charred POLLEN TYPHAE etc.
Chinese medicine is for reaching through the object of charcoal processing: the proper property changing medicine; Strengthen the merit of astringing to arrest bleeding, stopping diarrhea with astringents; Relax, reduce effect of drug toxicity etc.In concocting process, owing to being subject to heating-up temperature, time and the degree of process of preparing Chinese medicine, toxicity medicine special processing is with the impact of the factors such as attenuation synergistic, and physicochemical property there occurs change in various degree, and then causes the change of drug effect.The control of modern study to the process of preparing Chinese medicine degree of charcoal drug is the proterties according to frying mostly, and put in pot by medicinal material and fry to outer in black with moderate heat or intense fire, interior is that burnt brown etc. describes as quality standard.Fry charcoal drug and need the performance keeping original medicine, so-called " sustainability " is also." book on Chinese herbal medicine covers bamboo fish trap " of Chen Jiamo is said: " pharmacy is valued for moderate, and too late then effect difficulty is asked, and too then smell is counter loses.”
The process of preparing Chinese medicine degree of modern scholar's centering medicine charcoal drug and quality control quantitative target concentrate on the several aspect such as assay measuring content of tannin, clotting time, calcium ion content, determination of extractives, thin-layer chromatography and index composition.Coagulation time test is wasted time and energy, and other several assay method specificities are poor, and the thin-layer chromatography of index composition and assay lack specificity equally, because the plant of same kind is generally containing identical index components.
After prepared slices of Chinese crude drugs charcoal processing, proterties and effective constituent are all destroyed seriously, and composition is imprecise, and the uncertainty of charcoal drug material base constrains the unification of its quality standard, the product quality of the lack of checks on power of quality standard charcoal drug medicine materical crude slice and Clinical practice.The charcoal drug of separate standards is had only to have charred HERBA CIRSII JAPONICI, carbonized hair, charred schizonepeta, ching-chieh charcoal and thick wood-fern rhizome charcoal in 2015 editions Chinese Pharmacopoeias.On market, charcoal drug prepared slice quality is uneven, concocts degree varies, and lacks the discriminating item for charcoal drug medicine materical crude slice in Chinese Pharmacopoeia, greatly constrain the use of charcoal drug medicine materical crude slice; Therefore a kind of objective, quick, easy, thoroughly evaluating charcoal drug processed product method of quality control of research is needed.
Summary of the invention
The object of the present invention is to provide a kind of TLC Identification of charcoal drug processed product, the method fast, comprehensively, specificity is strong and can embody charcoal drug " stir-baked the crude drugs into black on outside and brown in inside " requirement.
The present invention is achieved by the following technical solutions:
A TLC Identification for charcoal drug processed product, comprises the steps:
The preparation of a, need testing solution
Get charcoal drug processed product sample powder, add hydrochloric acid heating hydrolysis, filter, filtrate ethyl acetate or extracted with diethyl ether, preferred ether, gets ethyl acetate or ether extraction liquid evaporate to dryness, and residue adds methyl alcohol and dissolves, as need testing solution;
The preparation of b, control medicinal material solution
Get corresponding control medicinal material, add finite concentration hydrochloric acid heating hydrolysis, filter, filtrate ethyl acetate or extracted with diethyl ether, preferred ether, ethyl acetate or ether extraction liquid evaporate to dryness, residue adds methyl alcohol and dissolves, medicinal material solution in contrast;
C, unfolding condition
Draw above-mentioned need testing solution and control medicinal material solution, put in same silica G F respectively 254on thin layer plate, with toluene: ethyl formate: formic acid is 2 ~ 8:2 ~ 8:0.1 ~ 1 for developping agent launches by volume, takes out, dries;
D, to inspect
Inspect under thin layer plate being put 254nm ultraviolet lamp, in test sample chromatogram, on the position corresponding to control medicinal material chromatogram, the principal spot of aobvious same color, or spray with chromogenic reagent more clear, in test sample chromatogram, on the position corresponding to control medicinal material chromatogram, the principal spot of aobvious same color.
Preferably, the TLC Identification of described charcoal drug processed product, specifically comprises the steps:
The preparation of a, need testing solution
Get charcoal drug processed product sample powder 2 ~ 5g, add hydrochloric acid 15 ~ 30ml heating hydrolysis 30 ~ 90 minutes, by ethyl acetate or extracted with diethyl ether 1 ~ 3 time, preferred ether, each 10 ~ 30ml, combined ethyl acetate or ether extraction liquid, evaporate to dryness, residue adds methyl alcohol 1ml makes dissolving, as need testing solution;
The preparation of b, control medicinal material solution
Get corresponding control medicinal material 1 ~ 3g, add finite concentration hydrochloric acid 15 ~ 30ml heating hydrolysis 30 ~ 90 minutes, by ethyl acetate or extracted with diethyl ether 1 ~ 3 time, preferred ether, each 10 ~ 30ml, combined ethyl acetate or ether extraction liquid, evaporate to dryness, residue adds methyl alcohol 1ml makes dissolving, medicinal material solution in contrast;
C, unfolding condition
Draw above-mentioned need testing solution and each 3 ~ 15 μ l of control medicinal material solution, put respectively in same silica G F 254on thin layer plate, with toluene: ethyl formate: formic acid is 4 ~ 6:4 ~ 6:0.1 ~ 1 for developping agent launches by volume, takes out, dries;
D, to inspect
Inspect under thin layer plate being put 254nm ultraviolet lamp, in test sample chromatogram, on the position corresponding to control medicinal material chromatogram, the principal spot of aobvious same color, or spray with 10% phosphomolybdic acid ethanol solution, ferric trichloride test solution or 10% ethanol solution of sulfuric acid again, be heated to spot development at 105 DEG C clear, in test sample chromatogram, on the position corresponding to control medicinal material chromatogram, the principal spot of aobvious same color.
Preferably, in step a and b, the method adding hydrochloric acid heating hydrolysis adopts and adds hot reflux or heating water bath, preferred heating water bath, and wherein heating reflux temperature is 110 ± 2 DEG C, and water bath reflux temperature is 98 ± 2 DEG C.
Preferably, in step a and b, the mass concentration of described hydrochloric acid is 5% ~ 30%, more preferably 10% ~ 20%.
Preferably, in step c, described developping agent is toluene: ethyl formate: formic acid=5: 5: 0.5 or toluene: ethyl formate: formic acid=5:4:1.
Charcoal drug processed product of the present invention is that the charcoal class prepared slices of Chinese crude drugs meeting 2015 editions Chinese Pharmacopoeias are fried to meeting relevant imperial charcoal drug processed product according to stir-fry charcoal method appendix II D.
Preferably, described charcoal drug processed product is the charcoal drug processed product containing 254nm fluorescent absorption material, is specially charred RADIX RUBIAE, charred CACUMEN PLATYCLADI, charred HERBA CIRSII JAPONICI, field thistle charcoal, charred RADIX SANGUISORBAE, charred POLLEN TYPHAE, vinegar Chinese mugwort charcoal, glutinous rehmannia charcoal or crinis trachycarpi etc.
The present invention compared with prior art, has following beneficial effect:
1. the present invention establishes a kind of TLC Identification of charcoal drug processed product, and after charcoal fried by the prepared slices of Chinese crude drugs, proterties and effective constituent are all destroyed seriously, and composition is imprecise, therefore mostly lacks the TLC distinguish item to charcoal drug medicine materical crude slice in statutory standards; The present invention adopt generally acknowledged directly perceived, fast thin-layer identification method charcoal drug processed product is differentiated, meet the requirement of statutory standards and enterprise's production quick test, can be used in the daily quality inspection work that scientific research and enterprise thereof produce;
2. thin-layer identification method of the present invention selects corresponding crude drug in contrast, differentiates that specificity is stronger, more comprehensively; Compared with other thin layer chromatographies of charcoal drug processed product, the present invention selects its " non-fluorescence composition " ester dissolubility position to carry out discrimination test uniquely, adopts acid hydrolysis reducing process, adopts silica G F 254fluorescent quenching thin layer plate, then observe in conjunction with the colour developing of characteristic component, specificity is stronger, and testing result is more comprehensive, the quality requirements of " stir-baked the crude drugs into black on outside and brown in inside " after having embodied prepared slices of Chinese crude drugs charcoal processing;
3. the basic guidance method of TLC distinguish of the present invention can be used as the discrimination method of multiple charcoal drug processed product, solve a great problem that charcoal drug processed product is differentiated, fill up the blank differentiating the quality control of charcoal drug processed product, set up for the quality standard controlling charcoal drug processed product and provide certain reference frame.
Accompanying drawing explanation
Fig. 1 is charred CACUMEN PLATYCLADI TLC distinguish chromatogram (UV254nm).
Fig. 2 is charred CACUMEN PLATYCLADI TLC distinguish chromatogram (daylight).
Fig. 3 is charred RADIX SANGUISORBAE TLC distinguish chromatogram (UV254nm).
Fig. 4 is charred RADIX SANGUISORBAE TLC distinguish chromatogram (daylight).
Fig. 5 is vinegar Chinese mugwort charcoal TLC distinguish chromatogram (UV254nm).
Fig. 6 is vinegar Chinese mugwort charcoal TLC distinguish chromatogram (daylight).
Fig. 7 is charred POLLEN TYPHAE TLC distinguish chromatogram (UV254nm).
Fig. 8 is charred POLLEN TYPHAE TLC distinguish chromatogram (daylight).
Fig. 9 is charred HERBA CIRSII JAPONICI TLC distinguish chromatogram (UV254nm).
Figure 10 is setose thistle TLC distinguish chromatogram (daylight).
Figure 11 is field thistle charcoal TLC distinguish chromatogram (UV254nm).
Figure 12 is charred RADIX RUBIAE TLC distinguish chromatogram (UV254nm).
In figure, 1-3 is charcoal drug processed product sample, and 4 is control medicinal material.
Embodiment
Further illustrate the present invention below by embodiment, following examples are the concrete embodiment of the present invention, but embodiments of the present invention are by the restriction of following embodiment.
Control medicinal material: (Nat'l Pharmaceutical & Biological Products Control Institute provides cacumen biotae control medicinal material; Lot number: 121396-200401), (Nat'l Pharmaceutical & Biological Products Control Institute provides garden burnet control medicinal material; Lot number: 121286-200402), (Nat'l Pharmaceutical & Biological Products Control Institute provides tarragon control medicinal material; Lot number: 121345-201002), (Nat'l Pharmaceutical & Biological Products Control Institute provides cattail pollen control medicinal material; Lot number: 121225-201003), (Nat'l Pharmaceutical & Biological Products Control Institute provides setose thistle control medicinal material; Lot number: 121411-201101), (Nat'l Pharmaceutical & Biological Products Control Institute provides field thistle control medicinal material; Lot number: 121436-201102), (Nat'l Pharmaceutical & Biological Products Control Institute provides madder control medicinal material; Lot number: 121049-201003);
Following charcoal drug processed product: be Guangdong Yifang Pharmaceutical Co., Ltd's buying crude drug and fry charcoal method (appendix II D) stir-fry to meeting relevant imperial charcoal drug processed product through concocting according to 2015 editions Chinese Pharmacopoeias.
the TLC distinguish of experimental example 1 charred CACUMEN PLATYCLADI
Get charred CACUMEN PLATYCLADI powder 4.0g, be placed in conical flask, add 15% hydrochloric acid solution 30ml, put in 98 DEG C of water-baths and heat 60 minutes, let cool, filter; Filtrate is by extracted with diethyl ether 2 times, and each 20ml, merges ether solution, evaporate to dryness; Residue adds methyl alcohol 1ml makes dissolving, as need testing solution.Separately get cacumen biotae control medicinal material 1.0g, make control medicinal material solution with test sample preparation method.According to thin-layered chromatography (" Chinese Pharmacopoeia " version in 2010 annex VI B) test, draw need testing solution, each 5 μ l of control medicinal material solution, put respectively in same silica G F 254on thin layer plate, with toluene-ethyl formate-formic acid (5:5:0.5) for developping agent, launch, take out, dry, inspect under putting ultraviolet lamp (254nm); As Fig. 1 ~ 2, in test sample chromatogram, on the position corresponding to control medicinal material chromatogram chromatogram, the principal spot of aobvious same color; Spray with 10% phosphomolybdic acid ethanol solution again, be heated to spot development at 105 DEG C clear.In test sample chromatogram, on the position corresponding to reference substance chromatogram, the principal spot of aobvious same color.
the TLC distinguish of experimental example 2 charred RADIX SANGUISORBAE
Get charred RADIX SANGUISORBAE powder 3.0g, be placed in conical flask, add 20% hydrochloric acid solution 30ml, 110 DEG C add hot reflux 45 minutes, let cool, and filter; Filtrate is by extracted with diethyl ether 2 times, and each 20ml, merges ether solution, evaporate to dryness; Residue adds methyl alcohol 1ml makes dissolving, as need testing solution.Separately get garden burnet control medicinal material 1.0g, make control medicinal material solution with test sample preparation method.According to thin-layered chromatography (" Chinese Pharmacopoeia " version in 2010 annex VI B) test, draw need testing solution, each 5 μ l of control medicinal material solution, put respectively in same silica G F 254on thin layer plate, with toluene-ethyl formate-formic acid (5:5:0.5) for developping agent, launch, take out, dry, inspect under putting ultraviolet lamp (254nm); As Fig. 3 ~ 4, in test sample chromatogram, on the position corresponding to control medicinal material chromatogram chromatogram, the principal spot of aobvious same color; Spray, with 5% iron chloride ethanolic solution, is heated to spot development at 105 DEG C clear, inspects under putting daylight lamp.In test sample chromatogram, on the position corresponding to reference substance chromatogram, the principal spot of aobvious same color.
the TLC distinguish of experimental example 3 vinegar Chinese mugwort charcoal
Get vinegar Chinese mugwort carbon powder 4.0g, be placed in conical flask, add 15% hydrochloric acid solution 30ml, put in 100 DEG C of water-baths and heat 60 minutes, let cool, filter; Filtrate is by extracted with diethyl ether 2 times, and each 20ml, merges ether solution, evaporate to dryness; Residue adds methyl alcohol 1ml makes dissolving, as need testing solution.Separately get tarragon control medicinal material 1.0g, make control medicinal material solution with test sample preparation method.According to thin-layered chromatography (" Chinese Pharmacopoeia " version in 2010 annex VI B) test, draw need testing solution, each 5 μ l of control medicinal material solution, put respectively in same silica G F 254on thin layer plate, with toluene-ethyl formate-formic acid (5:5:0.5) for developping agent, launch, take out, dry, inspect under putting ultraviolet lamp (254nm); As Fig. 5 ~ 6, in test sample chromatogram, on the position corresponding to control medicinal material chromatogram chromatogram, the principal spot of aobvious same color; Spray, with 10% vanillin-sulfuric acid solution, is heated to spot development at 105 DEG C clear, inspects under putting daylight lamp.In test sample chromatogram, on the position corresponding to reference substance chromatogram, the principal spot of aobvious same color.
the TLC distinguish of experimental example 4 charred POLLEN TYPHAE
Get charred POLLEN TYPHAE powder 4.0g, be placed in conical flask, add 15% hydrochloric acid solution 30ml, put in 98 DEG C of water-baths and heat 60 minutes, let cool, filter; Filtrate is by extracted with diethyl ether 2 times, and each 20ml, merges ether solution, evaporate to dryness; Residue adds methyl alcohol 1ml makes dissolving, as need testing solution.Separately get cattail pollen control medicinal material 1.5g, make control medicinal material solution with test sample preparation method.According to thin-layered chromatography (" Chinese Pharmacopoeia " version in 2010 annex VI B) test, draw need testing solution, each 5 μ l of control medicinal material solution, put respectively in same silica G F 254on thin layer plate, with toluene-ethyl formate-formic acid (5:5:0.5) for developping agent, launch, take out, dry, inspect under putting ultraviolet lamp (254nm); As Fig. 7 ~ 8, in test sample chromatogram, on the position corresponding to control medicinal material chromatogram chromatogram, the principal spot of aobvious same color; Spray, with 5% iron chloride ethanolic solution, is heated to spot development at 105 DEG C clear, inspects under putting daylight lamp.In test sample chromatogram, on the position corresponding to reference substance chromatogram, the principal spot of aobvious same color.
the TLC distinguish of experimental example 5 charred HERBA CIRSII JAPONICI
Get charred HERBA CIRSII JAPONICI powder 2.0g, be placed in conical flask, add 15% hydrochloric acid solution 30ml, put in 98 DEG C of water-baths and heat 30 minutes, let cool, filter; Filtrate is by extracted with diethyl ether 2 times, and each 20ml, merges ether solution, evaporate to dryness; Residue adds methyl alcohol 1ml makes dissolving, as need testing solution.Separately get setose thistle control medicinal material 1.0g, make control medicinal material solution with test sample preparation method.According to thin-layered chromatography (" Chinese Pharmacopoeia " version in 2010 annex VI B) test, draw need testing solution 5 μ l, control medicinal material solution 10 μ l, put respectively in same silica G F 254on thin layer plate, with toluene-ethyl formate-formic acid (5:4:1) for developping agent, launch, take out, dry, inspect under putting ultraviolet lamp (254nm); As Fig. 9 ~ 10, in test sample chromatogram, on the position corresponding to control medicinal material chromatogram chromatogram, the principal spot of aobvious same color; Spray, with 5% iron chloride ethanolic solution, is heated to spot development at 105 DEG C clear, inspects under putting daylight lamp.In test sample chromatogram, on the position corresponding to reference substance chromatogram, the principal spot of aobvious same color.
the TLC distinguish of experimental example 6 field thistle charcoal
Get field thistle charcoal powder 3.0g, be placed in conical flask, add 10% hydrochloric acid solution 30ml, put in 98 DEG C of water-baths and heat 60 minutes, let cool, filter; Filtrate is by extracted with diethyl ether 2 times, and each 20ml, merges ether solution, evaporate to dryness; Residue adds methyl alcohol 1ml makes dissolving, as need testing solution.Separately get field thistle control medicinal material 1.0g, make control medicinal material solution with test sample preparation method.According to thin-layered chromatography (" Chinese Pharmacopoeia " version in 2010 annex VI B) test, draw need testing solution, each 5 μ l of control medicinal material solution, put respectively in same silica G F 254on thin layer plate, with toluene-ethyl formate-formic acid (5:5:0.5) for developping agent, launch, take out, dry, inspect under putting ultraviolet lamp (254nm); As Figure 11, in test sample chromatogram, on the position corresponding to control medicinal material chromatogram chromatogram, the principal spot of aobvious same color.
the TLC distinguish of experimental example 7 charred RADIX RUBIAE
Get charred RADIX RUBIAE powder 3.0g, be placed in conical flask, add 15% hydrochloric acid solution 30ml, put in 98 DEG C of water-baths and heat 60 minutes, let cool, filter; Filtrate is by extracted with diethyl ether 2 times, and each 20ml, merges ether solution, evaporate to dryness; Residue adds methyl alcohol 1ml makes dissolving, as need testing solution.Separately get madder control medicinal material 1.0g, make control medicinal material solution with test sample preparation method.According to thin-layered chromatography (" Chinese Pharmacopoeia " version in 2010 annex VI B) test, draw need testing solution, each 5 μ l of control medicinal material solution, put respectively in same silica G F 254on thin layer plate, with toluene-ethyl formate-formic acid (5:4:1) for developping agent, launch, take out, dry, inspect under putting ultraviolet lamp (254nm); As Figure 12, in test sample chromatogram, on the position corresponding to control medicinal material chromatogram chromatogram, the principal spot of aobvious same color.

Claims (8)

1. a TLC Identification for charcoal drug processed product, is characterized in that, comprises the steps:
The preparation of a, need testing solution
Get charcoal drug processed product sample powder, add hydrochloric acid heating hydrolysis, filter, filtrate ethyl acetate or extracted with diethyl ether, preferred ether, gets ethyl acetate or ether extraction liquid evaporate to dryness, and residue adds methyl alcohol and dissolves, as need testing solution;
The preparation of b, control medicinal material solution
Get corresponding control medicinal material, add hydrochloric acid heating hydrolysis, filter, filtrate ethyl acetate or extracted with diethyl ether, preferred ether, ethyl acetate or ether extraction liquid evaporate to dryness, residue adds methyl alcohol and dissolves, medicinal material solution in contrast;
C, unfolding condition
Draw above-mentioned need testing solution and control medicinal material solution, put in same silica G F respectively 254on thin layer plate, with toluene: ethyl formate: formic acid is 2 ~ 8:2 ~ 8:0.1 ~ 1 for developping agent launches by volume, takes out, dries;
D, to inspect
Inspect under thin layer plate being put 254nm ultraviolet lamp, in test sample chromatogram, on the position corresponding to control medicinal material chromatogram, the principal spot of aobvious same color, or spray with chromogenic reagent more clear, in test sample chromatogram, on the position corresponding to control medicinal material chromatogram, the principal spot of aobvious same color.
2. the TLC Identification of charcoal drug processed product according to claim 1, is characterized in that, specifically comprise the steps:
The preparation of a, need testing solution
Get charcoal drug processed product sample powder 2 ~ 5g, add hydrochloric acid 15 ~ 30ml heating hydrolysis 30 ~ 90 minutes, by ethyl acetate or extracted with diethyl ether 1 ~ 3 time, preferred ether, each 10 ~ 30ml, combined ethyl acetate or ether extraction liquid, evaporate to dryness, residue adds methyl alcohol 1ml makes dissolving, as need testing solution;
The preparation of b, control medicinal material solution
Get corresponding control medicinal material 1 ~ 3g, add hydrochloric acid 15 ~ 30ml heating hydrolysis 30 ~ 90 minutes, by ethyl acetate or extracted with diethyl ether 1 ~ 3 time, preferred ether, each 10 ~ 30ml, combined ethyl acetate or ether extraction liquid, evaporate to dryness, residue adds methyl alcohol 1ml makes dissolving, medicinal material solution in contrast;
C, unfolding condition
Draw above-mentioned need testing solution and each 3 ~ 15 μ l of control medicinal material solution, put respectively in same silica G F 254on thin layer plate, with toluene: ethyl formate: formic acid is 4 ~ 6:4 ~ 6:0.1 ~ 1 for developping agent launches by volume, takes out, dries;
D, to inspect
Inspect under thin layer plate being put 254nm ultraviolet lamp, in test sample chromatogram, on the position corresponding to control medicinal material chromatogram, the principal spot of aobvious same color, or spray with 10% phosphomolybdic acid ethanol solution, ferric trichloride test solution or 10% ethanol solution of sulfuric acid again, be heated to spot development at 105 DEG C clear, in test sample chromatogram, on the position corresponding to control medicinal material chromatogram, the principal spot of aobvious same color.
3. the TLC Identification of charcoal drug processed product according to claim 1 and 2, is characterized in that, in step a and b, the method adding hydrochloric acid heating hydrolysis adopts and adds hot reflux or heating water bath, preferred heating water bath, wherein heating reflux temperature is 110 ± 2 DEG C, and bath temperature is 98 ± 2 DEG C.
4. the TLC Identification of charcoal drug processed product according to claim 1 and 2, is characterized in that, in step a and b, the mass concentration of described hydrochloric acid is 5% ~ 30%, preferably 10% ~ 20%.
5. the TLC Identification of charcoal drug processed product according to claim 1 and 2, is characterized in that, in step c, described developping agent is toluene: ethyl formate: formic acid=5: 5: 0.5 or toluene: ethyl formate: formic acid=5:4:1.
6. the TLC Identification of charcoal drug processed product according to claim 1 and 2, is characterized in that, described charcoal drug processed product is the charcoal drug processed product containing 254nm fluorescent absorption material.
7. the TLC Identification of charcoal drug processed product according to claim 6, is characterized in that, described charcoal drug processed product is charred RADIX RUBIAE, charred CACUMEN PLATYCLADI, charred HERBA CIRSII JAPONICI, field thistle charcoal, charred RADIX SANGUISORBAE, charred POLLEN TYPHAE, vinegar Chinese mugwort charcoal, glutinous rehmannia charcoal or crinis trachycarpi.
8. the TLC Identification of charcoal drug processed product according to claim 1 and 2, it is characterized in that, described charcoal drug processed product is that the charcoal class prepared slices of Chinese crude drugs meeting 2015 editions Chinese Pharmacopoeias are fried to meeting relevant imperial charcoal drug processed product according to stir-fry charcoal method appendix II D.
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CN106265777A (en) * 2016-08-21 2017-01-04 贵州三泓药业股份有限公司 A kind of standardized processing method of the primary charcoal in side
CN106706793A (en) * 2016-12-29 2017-05-24 南京中医药大学 Quality control method for platycladi cacumen carbonisatum
CN114246888A (en) * 2018-05-21 2022-03-29 成都中医大华神药业有限责任公司 Detection method of folium artemisiae argyi charcoal
CN112414967A (en) * 2020-11-17 2021-02-26 南京中医药大学 Near-infrared quality control method for rapidly detecting processing of cattail pollen charcoal in real time
CN112414967B (en) * 2020-11-17 2023-08-18 南京中医药大学 Near infrared quality control method for rapidly detecting processing of cattail pollen charcoal in real time

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Application publication date: 20160113