CN104237415B - The detection method of a kind of yellow incense drug compositions and preparation thereof - Google Patents
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Abstract
The invention discloses the detection method of a kind of yellow incense drug compositions and preparation thereof, the method comprises HPLC characteristic spectrum detection method and/or TLC differentiates detection method.The method sets up a stack features peak by HPLC method and simple gradient elution, and testing result and standard feature peak is contrasted.The method also discloses the TLC chromatographic identification of yellow incense drug compositions and preparation thereof.Detection method of the present invention is easy and simple to handle, quick, testing cost is low, favorable reproducibility, contain much information, and the HPLC characteristic peak of gained sample is obvious, and comparison is easy, and can reflect the formula composition of yellow incense drug compositions and preparation thereof more comprehensively.
Description
Technical field
The present invention relates to the detection method of a kind of yellow incense drug compositions and preparation thereof, belong to medical art.
Background technology
Modern pharmacological research finds, rheum officinale has effect for reducing blood fat significantly; Pogostemon cablin is the aromatic damp-resolving drug commonly used clinically, its taste is pungent, tepor, have the effect of eliminating dampness with aromatics, particularly its volatile oil component has pharmacologically active extremely significantly, and the fragrant particle of the Huang according to traditional ancient prescription achieves good curative effect clinical for high fat of blood card.Yellow fragrant particle records in national drug standards part (internal medicine feels concerned about fascicle), standard number: WS-10902 (ZD-0902)-2002-2012Z, yellow fragrant particle consist of rheum officinale 200g, Pogostemon cablin 200g and sucrose.
Current said preparation quality standard only has the discriminating of rheum officinale and patchouli alcohol and emodin content to measure item, its testing result can not embody yellow fragrant preparation total quality completely, and complex operation, do not find overall method for measuring and technology are carried out for the fragrant particle of Huang in retrieval prior art yet.
HPLC characteristic spectrum detection method have easy and simple to handle, quick, testing cost is low, favorable reproducibility and the advantage such as to contain much information, the detection for pharmaceutical composition has great importance.The characteristic spectrum detection method simultaneously detecting rheum officinale and Pogostemon cablin is not found in prior art, but it is a lot of to the characteristic spectrum detection method of rheum officinale or Pogostemon cablin, as the comparative studies of HPLC characteristic spectrum of processed product " rheum officinale different " (volume the 3rd phase March the 31st in 2011 " Hunan University of Traditional Chinese Medicine's journal ") also with methyl alcohol-0.05% phosphate aqueous solution for mobile phase establishes the characteristic spectrum detection method of rheum officinale, but the change of its graded is complicated, methanol ratio changes to 90% gradually from 10%, T.T. 80min, reference substance reaches 8 kinds, and experimental implementation is loaded down with trivial details." HPLC sets up the methodological study of Pogostemon cablin characteristic spectrum " (" Chinese patent drug " 27 volume 12 phases in 2005) also establish the characteristic spectrum detection method of Pogostemon cablin, also with methyl alcohol-0.05% phosphate aqueous solution for mobile phase, with 26 detected peaks for index, comparison difficulty, experimental implementation is loaded down with trivial details, requires higher.
Summary of the invention
For the deficiencies in the prior art, the invention discloses the detection method of a kind of yellow incense drug compositions and preparation thereof, the method comprises HPLC characteristic spectrum detection method and/or TLC differentiates detection method.
Term illustrates:
Yellow fragrant particle is the nomenclature of drug that national drug standards part (internal medicine feels concerned about fascicle) is recorded.
The preparation that yellow incense drug compositions and preparation thereof comprise yellow fragrant particle medicinal composition and prepare with yellow fragrant particulate material medicine composition.
Technical scheme of the present invention is as follows:
Bulk drug consists of rheum officinale 200 weight portion, the yellow incense drug compositions of Pogostemon cablin 200 weight portion and a detection method for preparation thereof, and the method comprises following HPLC characteristic spectrum detection method and/or TLC differentiates detection method:
HPLC characteristic spectrum detection method:
A) chromatographic condition and system suitability: take octadecylsilane chemically bonded silica as filling agent; With methyl alcohol-volume parts than 0.5% phosphate aqueous solution for mobile phase, by following condition gradient elution: 0 → 30 minute methyl alcohol volume ratio, 40% → 80%, 30 → 60 minutes methyl alcohol volume ratios keep 80%; Determined wavelength is 280 ~ 300nm; Flow velocity: 0.8 ~ 1.2ml/min; Analysis time: 60 minutes; Number of theoretical plate calculates by archen peak and is not less than 2000;
B) preparation of reference substance solution: get archen reference substance, adds methyl alcohol and makes the solution of every 1ml containing archen 0.2mg, to obtain final product;
C) preparation of need testing solution: get powder 1-5g after yellow incense drug compositions or its preparation porphyrize, add methyl alcohol 10-50ml, ultrasonic process 30-40 minute, lets cool, filters, gets subsequent filtrate, to obtain final product;
D) detect: accurate absorption reference substance solution and each 5 ~ 15 μ l of need testing solution respectively, inject high performance liquid chromatograph, record the chromatogram in 60 minutes; Gained collection of illustrative plates comprises the characteristic peak of yellow incense drug compositions or its preparation, and each characteristic peak relative retention time error is no more than 10%;
TLC differentiates detection method:
Get yellow incense drug compositions or its preparation 2-5g, add boiling range 60-90 DEG C of sherwood oil 10-30ml, ultrasonic process 30min, lets cool, and filter, filtrate evaporate to dryness, residue adds boiling range 60-90 DEG C of sherwood oil 2ml makes dissolving, as need testing solution; Get rheum officinale control medicinal material 1g, obtain rheum officinale control medicinal material solution with legal system; Get Pogostemon cablin control medicinal material 1g, obtain Pogostemon cablin control medicinal material solution with legal system; According to Chinese Pharmacopoeia thin-layered chromatography, draw each 10 μ l of above-mentioned three kinds of solution, put respectively in same silica G chromatographic sheet, with volume parts ratio for the boiling range 60-90 DEG C of sherwood oil-ethyl formate-formic acid supernatant of 3-5:0.5-2:0.2-1 is for developping agent, launch, take out, dry, inspect under putting 365nm ultraviolet lamp; In test sample chromatogram, on the position corresponding to control medicinal material chromatogram, the fluorescence spot of aobvious same color.
The present invention is preferred, the detection method of a kind of yellow incense drug compositions and preparation thereof, and wherein in HPLC characteristic spectrum detection method, the characteristic peak of yellow incense drug compositions or its preparation is 11, wherein No. 9 peak archens are base peak, and the relative retention time at 11 peaks is respectively 0.195,0.208,0.271,0.428,0.505,0.531,0.587,0.827,1.000,1.114,1.335.
The present invention is preferred, the detection method of a kind of yellow incense drug compositions and preparation thereof, and the determined wavelength wherein in HPLC characteristic spectrum detection method is 290nm; Flow velocity is 1.0ml/min; Sample size is 10 μ l.
The present invention is preferred, the detection method of a kind of yellow incense drug compositions and preparation thereof, and wherein TLC differentiates that detection method developping agent boiling range 60-90 DEG C of sherwood oil-ethyl formate-formic acid supernatant volume portion rate is 4:1:0.5.
Further preferred, a kind of bulk drug consists of the detection method of the fragrant particle of Huang of rheum officinale 200 weight portion, Pogostemon cablin 200 weight portion, and the method comprises following HPLC characteristic spectrum detection method and/or TLC differentiates detection method:
HPLC characteristic spectrum detection method:
A) chromatographic condition and system suitability: take octadecylsilane chemically bonded silica as filling agent; With methyl alcohol-volume parts than 0.5% phosphate aqueous solution for mobile phase, by following condition gradient elution: 0 → 30 minute methyl alcohol volume ratio, 40% → 80%, 30 → 60 minutes methyl alcohol volume ratios keep 80%; Determined wavelength is 290nm; Flow velocity: 1.0ml/min; Analysis time: 60 minutes; Number of theoretical plate calculates by archen peak and is not less than 2000;
B) preparation of reference substance solution: get archen reference substance, adds methyl alcohol and makes the solution of every 1ml containing archen 0.2mg, to obtain final product;
C) preparation of need testing solution: get powder 4g after yellow fragrant particle porphyrize, add methyl alcohol 50ml, ultrasonic process 30 minutes, lets cool, filters, gets subsequent filtrate, to obtain final product;
D) detect: accurate absorption reference substance solution and each 10 μ l of need testing solution respectively, inject high performance liquid chromatograph, record the chromatogram in 60 minutes; Gained collection of illustrative plates comprises the characteristic peak of yellow incense drug compositions or its preparation, and each characteristic peak relative retention time error is no more than 10%;
TLC differentiates detection method:
Get yellow fragrant particle 3g, add boiling range 60-90 DEG C of sherwood oil 25ml, ultrasonic process 30min, lets cool, and filter, filtrate evaporate to dryness, residue adds boiling range 60-90 DEG C of sherwood oil 2ml makes dissolving, as need testing solution; Get rheum officinale control medicinal material 1g, obtain rheum officinale control medicinal material solution with legal system; Get Pogostemon cablin control medicinal material 1g, obtain Pogostemon cablin control medicinal material solution with legal system; According to Chinese Pharmacopoeia thin-layered chromatography, draw each 10 μ l of above-mentioned three kinds of solution, put respectively in same silica G chromatographic sheet, with volume parts ratio for the boiling range 60-90 DEG C of sherwood oil-ethyl formate-formic acid supernatant of 4:1:0.5 is for developping agent, launch, take out, dry, inspect under putting 365nm ultraviolet lamp; In test sample chromatogram, on the position corresponding to control medicinal material chromatogram, the fluorescence spot of aobvious same color.
Preparation of the present invention refers to gets yellow fragrant particulate material medicine, technique routinely, adds customary adjuvant and is prepared into clinical acceptable any one formulation, include but not limited to pill, micropill, dripping pill, tablet, capsule, medicine materical crude slice, dispersing tablet.
The unit corresponding relation of the weight portion described in this instructions and parts by volume is g/ml or kg/l.
The beneficial effect of the invention:
Detection method of the present invention is easy and simple to handle, quick, testing cost is low, favorable reproducibility, contain much information, and the HPLC characteristic peak of gained sample is obvious, and comparison is easy, and can reflect the formula composition of yellow incense drug compositions and preparation thereof more comprehensively.
Accompanying drawing explanation
Fig. 1 is the HPLC standard feature collection of illustrative plates of yellow fragrant particle;
Fig. 2 is the HPLC collection of illustrative plates of archen standard items;
Fig. 3 is that the TLC of yellow fragrant particle differentiates collection of illustrative plates.
Wherein, the horizontal ordinate of Fig. 1, Fig. 2 is the time, unit: minute (min); Ordinate is voltage, unit: volt (Volts).In Fig. 3,1 is rheum officinale control medicinal material, and 2 is yellow fragrant particle, and 3 is Pogostemon cablin control medicinal material.
Embodiment
Following experimental example and embodiment are used for further illustrating but are not limited to the present invention.
Experimental example 1: the foundation of yellow incense drug compositions characteristic spectrum
Test apparatus: high performance liquid chromatograph: Hitachi L-2100 pump L-2400 UV-detector
Electronic balance: Shimadzu AUW-220D type
Ultraviolet spectrophotometer: Shimadzu UV-2450 type
Reference substance: archen reference substance (Nat'l Pharmaceutical & Biological Products Control Institute) lot number: 110756-200110
Test sample: yellow fragrant particle (Jin He Tibetan medicine incorporated company) lot number: 20100105,20100806,20110204,20110902,20120103,20120704,20130207,20130906,20140102,20140503
Chromatographic condition and system suitability: take octadecylsilane chemically bonded silica as filling agent; With methyl alcohol (A)-volume parts than 0.5% phosphate aqueous solution (B) for mobile phase, gradient elution: methyl alcohol rose to 80% by 40% in 0 ~ 30 minute, 30 ~ 60 minutes methyl alcohol keeps 80%; Determined wavelength is 290nm; Column temperature: 35 DEG C; Flow velocity: 1.0ml/min; Analysis time: 60 minutes.Number of theoretical plate calculates should be not less than 2000 by archen peak;
The preparation of reference substance solution: get archen reference substance appropriate, adds methyl alcohol and makes the solution of every 1ml containing archen 0.2mg, to obtain final product;
The preparation of need testing solution: get powder 2g after yellow incense drug compositions or its preparation porphyrize, add methyl alcohol 25ml, ultrasonic process 30 minutes, lets cool, filters, gets subsequent filtrate, to obtain final product.
Determined wavelength is selected: obtain need testing solution by the preparation method by need testing solution, scan in 190-400nm wavelength coverage, according to ultraviolet absorpting spectrum, selected 290nm is determined wavelength.
High effective liquid chromatography for measuring standard feature collection of illustrative plates: get 10 batches of fragrant particles of Huang and obtain need testing solution by the preparation method of need testing solution, the high-efficient liquid phase chromatogram of 10 batches of fragrant granular preparations of Huang is obtained by above-mentioned chromatographic condition, comparative evaluation is carried out with the HPLC collection of illustrative plates of these 10 batches of fragrant particles of Huang, set up the standard feature collection of illustrative plates of yellow fragrant particle, be specially characteristic peak 11, wherein No. 9 peak archens are base peak, and the relative retention time at 11 peaks is respectively 0.195,0.208,0.271,0.428,0.505,0.531,0.587,0.827,1.000,1.114,1.335.
Experimental example 2: the adaptability of characteristic spectrum detection method is investigated
1, precision test
Getting lot number is 20140503 batches of fragrant particulate samples of Huang, empirically the preparation method of example 1 need testing solution obtains need testing solution portion, under experimental example 1 chromatographic condition, continuous sample introduction measures for 5 times, and result shows: characteristic spectrum detection method precision provided by the invention is good.Measurement result is in table 1.
The yellow fragrant particle liquid phase characteristic spectrum precision of table 1 investigates result (relative retention time)
2, replica test
Getting lot number is 20140503 batches of fragrant particulate samples of Huang, empirically preparation method's operation repetitive six times of example 1 need testing solution, obtain need testing solution six parts, under experimental example 1 chromatographic condition, sample introduction measures, and result shows: characteristic spectrum detection method repeatability provided by the invention is good.Measurement result is in table 2.
The yellow fragrant particle liquid phase characteristic spectrum repeatability of table 2 investigates result (relative retention time)
3, stability test
Getting lot number is 20140503 batches of fragrant particulate samples of Huang, empirically the preparation method of example 1 need testing solution obtains need testing solution portion, measure at 0 hour, 1 hour, 2 hours, 4 hours, 6 hours, 8 hours sample introductions respectively under experimental example 1 chromatographic condition, result shows: characteristic spectrum detection method provided by the invention has good stability.Measurement result is in table 3.
Yellow fragrant particle liquid phase characteristic spectrum study on the stability result (relative retention time) of table 3
The choice experiment of the developping agent of experimental example 3, thin-layer chromatography
For the developping agent that rheum officinale is differentiated in prior art, the upper solution of conventional sherwood oil (30-60 DEG C)-ethyl formate-formic acid (15:5:1), yellow fragrant particle contains rheum officinale and Pogostemon cablin, therefore the present invention also once selected this developping agent, but find that final expansion separating effect is not satisfactory, launch the hangover of spot overlap serious, also once strengthened the ratio of formic acid to promote the polarity of developping agent, but result is not improved.After through experiment find, change the sherwood oil of high boiling range (60-90 DEG C) into, gained separating effect is ideal, and within the scope of ratio 3-5:0.5-2:0.2-1, gained launches collection of illustrative plates all can meet requirement of experiment, but ideal developping agent ratio is 4:1:0.5.
Following embodiment all can realize the effect described in above-mentioned experimental example.
Below in conjunction with embodiment, detailed elaboration is done to the present invention, but be not limited to these embodiments specifically recorded.The yellow incense drug compositions detected be gold scold Tibetan medicine medicine company incorporated company produce sell.
Embodiment 1: the detection method of yellow fragrant particle
Comprise HPLC characteristic spectrum detection method and TLC detection method, wherein,
HPLC characteristic spectrum detection method is:
Chromatographic condition and system suitability: take octadecylsilane chemically bonded silica as filling agent; With methyl alcohol (A)-volume parts than 0.5% phosphate aqueous solution (B) for mobile phase, according to following condition gradient elution: within 0 ~ 30 minute, methyl alcohol rises to 80% by 40%, 30 ~ 60 minutes methyl alcohol keeps 80%; Determined wavelength is 290nm; Column temperature: 35 DEG C; Flow velocity: 1.0ml/min; Analysis time: 60 minutes.Number of theoretical plate calculates should be not less than 2000 by archen peak;
The preparation of reference substance solution: get archen reference substance appropriate, adds methyl alcohol and makes the solution of every 1ml containing archen 0.2mg, to obtain final product;
The preparation of need testing solution: get powder 4g after yellow fragrant particle porphyrize, add methyl alcohol 50ml, ultrasonic process 30 minutes, lets cool, filters, gets subsequent filtrate, to obtain final product.
Detect: accurate absorption reference substance solution and each 10 μ l of need testing solution respectively, inject high performance liquid chromatograph, record the chromatogram in 60 minutes; Gained collection of illustrative plates comprises 11 characteristic spectrum peaks of yellow incense drug compositions, the equal < 5% of each characteristic peak relative retention time error; The relative retention time at 11 peaks is specially 0.194, and 0.208,0.271,0.429,0.504,0.531,0.587,0.826,1.000,1.114,1.334.
TLC detection method is:
Get yellow fragrant particle 3g, add sherwood oil (60-90 DEG C) 25ml, ultrasonic process 30min, lets cool, and filter, filtrate evaporate to dryness, residue adds sherwood oil (60-90 DEG C) 2ml makes dissolving, as need testing solution; Get rheum officinale control medicinal material 1g, obtain rheum officinale control medicinal material solution with legal system; Get Pogostemon cablin control medicinal material 1g, obtain Pogostemon cablin control medicinal material solution with legal system; Test according to thin-layered chromatography (Chinese Pharmacopoeia version in 2010 annex VI B), draw each 10 μ l of above-mentioned three kinds of solution, put respectively in same silica G chromatographic sheet, with volume parts ratio for sherwood oil (the 60-90 DEG C)-ethyl formate-formic acid supernatant of 4:1:0.5 is for developping agent, launch, take out, dry, inspect under putting 365nm ultraviolet lamp; In test sample chromatogram, on the position corresponding to control medicinal material chromatogram, the fluorescence spot of aobvious same color.
Embodiment 2: the detection method of yellow fragrant particle
HPLC characteristic spectrum detection method:
Chromatographic condition and system suitability: take octadecylsilane chemically bonded silica as filling agent; With methyl alcohol (A)-volume parts than 0.5% phosphate aqueous solution (B) for mobile phase, according to following condition gradient elution: within 0 ~ 30 minute, methyl alcohol rises to 80% by 40%, 30 ~ 60 minutes methyl alcohol keeps 80%; Determined wavelength is 290nm; Column temperature: 35 DEG C; Flow velocity: 1.0ml/min; Analysis time: 60 minutes.Number of theoretical plate calculates should be not less than 2000 by archen peak;
The preparation of reference substance solution: get archen reference substance appropriate, adds methyl alcohol and makes the solution of every 1ml containing archen 0.2mg, to obtain final product;
The preparation of need testing solution: get powder 1g after yellow fragrant particle porphyrize, add methyl alcohol 10ml, ultrasonic process 40 minutes, lets cool, filters, gets subsequent filtrate, to obtain final product.
Detect: accurate absorption reference substance solution and each 5 μ l of need testing solution respectively, inject high performance liquid chromatograph, record the chromatogram in 60 minutes; Gained collection of illustrative plates comprises 11 characteristic spectrum peaks of yellow incense drug compositions, the equal < 5% of each characteristic peak relative retention time error; The relative retention time at 11 peaks is specially 0.194, and 0.208,0.271,0.429,0.504,0.531,0.587,0.826,1.000,1.114,1.334.
Embodiment 3: the detection method of yellow fragrant particle
TLC detection method is as follows:
Get yellow fragrant particle 2g, add sherwood oil (60-90 DEG C) 10ml, ultrasonic process 30min, lets cool, and filter, filtrate evaporate to dryness, residue adds sherwood oil (60-90 DEG C) 2ml makes dissolving, as need testing solution; Get rheum officinale control medicinal material 1g, obtain rheum officinale control medicinal material solution with legal system; Get Pogostemon cablin control medicinal material 1g, obtain Pogostemon cablin control medicinal material solution with legal system; Test according to thin-layered chromatography (Chinese Pharmacopoeia version in 2010 annex VI B), draw each 10 μ l of above-mentioned three kinds of solution, put respectively in same silica G chromatographic sheet, with volume parts ratio for sherwood oil (the 60-90 DEG C)-ethyl formate-formic acid supernatant of 3:0.5:0.2 is for developping agent, launch, take out, dry, inspect under putting 365nm ultraviolet lamp; In test sample chromatogram, on the position corresponding to control medicinal material chromatogram, the fluorescence spot of aobvious same color.
Embodiment 4: the detection method of yellow fragrant particle
TLC detection method is as follows:
Get yellow fragrant particle 5g, add sherwood oil (60-90 DEG C) 30ml, ultrasonic process 30min, lets cool, and filter, filtrate evaporate to dryness, residue adds sherwood oil (60-90 DEG C) 2ml makes dissolving, as need testing solution; Get rheum officinale control medicinal material 1g, obtain rheum officinale control medicinal material solution with legal system; Get Pogostemon cablin control medicinal material 1g, obtain Pogostemon cablin control medicinal material solution with legal system; Test according to thin-layered chromatography (Chinese Pharmacopoeia version in 2010 annex VI B), draw each 10 μ l of above-mentioned three kinds of solution, put respectively in same silica G chromatographic sheet, with volume parts ratio for sherwood oil (the 60-90 DEG C)-ethyl formate-formic acid supernatant of 5:2:1 is for developping agent, launch, take out, dry, inspect under putting 365nm ultraviolet lamp; In test sample chromatogram, on the position corresponding to control medicinal material chromatogram, the fluorescence spot of aobvious same color.
Claims (4)
1. bulk drug consists of rheum officinale 200 weight portion, the yellow incense drug compositions of Pogostemon cablin 200 weight portion and a detection method for preparation thereof, is characterised in that, the method comprises following HPLC characteristic spectrum detection method:
A) chromatographic condition and system suitability: take octadecylsilane chemically bonded silica as filling agent; With methyl alcohol-volume parts than 0.5% phosphate aqueous solution for mobile phase, by following condition gradient elution: 0 → 30 minute methyl alcohol volume ratio, 40% → 80%, 30 → 60 minutes methyl alcohol volume ratios keep 80%; Determined wavelength is 280 ~ 300nm; Flow velocity: 0.8 ~ 1.2ml/min; Analysis time: 60 minutes; Number of theoretical plate calculates by archen peak and is not less than 2000;
B) preparation of reference substance solution: get archen reference substance, adds methyl alcohol and makes the solution of every 1ml containing archen 0.2mg, to obtain final product;
C) preparation of need testing solution: get powder 1-5g after yellow incense drug compositions or its preparation porphyrize, add methyl alcohol 10-50ml, ultrasonic process 30-40 minute, lets cool, filters, gets subsequent filtrate, to obtain final product;
D) detect: accurate absorption reference substance solution and each 5 ~ 15 μ l of need testing solution respectively, inject high performance liquid chromatograph, record the chromatogram in 60 minutes; Gained collection of illustrative plates comprises the characteristic peak of yellow incense drug compositions or its preparation, and each characteristic peak relative retention time error is no more than 10%.
2. detection method according to claim 1, is characterised in that, wherein in HPLC characteristic spectrum detection method, the characteristic peak of yellow incense drug compositions or its preparation is 11, wherein No. 9 peak archens are base peak, and the relative retention time at 11 peaks is respectively 0.195,0.208,0.271,0.428,0.505,0.531,0.587,0.827,1.000,1.114,1.335.
3. detection method according to claim 1, is characterised in that, the determined wavelength wherein in HPLC characteristic spectrum detection method is 290nm; Flow velocity is 1.0ml/min; Sample size is 10 μ l.
4. bulk drug consists of the detection method of the fragrant particle of Huang for rheum officinale 200 weight portion, Pogostemon cablin 200 weight portion, and be characterised in that, the method comprises following HPLC characteristic spectrum detection method:
A) chromatographic condition and system suitability: take octadecylsilane chemically bonded silica as filling agent; With methyl alcohol-volume parts than 0.5% phosphate aqueous solution for mobile phase, by following condition gradient elution: 0 → 30 minute methyl alcohol volume ratio, 40% → 80%, 30 → 60 minutes methyl alcohol volume ratios keep 80%; Determined wavelength is 290nm; Flow velocity: 1.0ml/min; Analysis time: 60 minutes; Number of theoretical plate calculates by archen peak and is not less than 2000;
B) preparation of reference substance solution: get archen reference substance, adds methyl alcohol and makes the solution of every 1ml containing archen 0.2mg, to obtain final product;
C) preparation of need testing solution: get powder 4g after yellow fragrant particle porphyrize, add methyl alcohol 50ml, ultrasonic process 30 minutes, lets cool, filters, gets subsequent filtrate, to obtain final product;
D) detect: accurate absorption reference substance solution and each 10 μ l of need testing solution respectively, inject high performance liquid chromatograph, record the chromatogram in 60 minutes; Gained collection of illustrative plates comprises the characteristic peak of yellow incense drug compositions or its preparation, and each characteristic peak relative retention time error is no more than 10%.
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| 香桂化浊胶囊的数字化指纹图谱研究及其质量控制;张辰辰;《中国优秀硕士学位论文全文数据库医药卫生科技辑》;20140915(第9期);16页3.1-4.2节，17页第1-3节 * |
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Address after: 250101 Shandong city of Ji'nan province (Lixia District Shun) high wind Road No. 322 room 501-506 Applicant after: Shandong Jin He drug development research company limited Address before: 250101 Shandong city of Ji'nan province (Lixia District Shun) high wind Road No. 322 room 501-506 Applicant before: Shandong ARURA Pharmaceutical Research & Development Co., Ltd. |
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Effective date of registration: 20171011 Address after: 810003, No. two, No. 22, Xining Road, Qinghai, Qinghai Province Patentee after: JINHE TIBETAN MEDICINE CO., LTD. Address before: 250101 Shandong city of Ji'nan province (Lixia District Shun) high wind Road No. 322 room 501-506 Patentee before: Shandong Jin He drug development research company limited |