WO2005088295A1 - Procede de controle de qualite destine aux pilules a avaler composees de danshen - Google Patents

Procede de controle de qualite destine aux pilules a avaler composees de danshen Download PDF

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Publication number
WO2005088295A1
WO2005088295A1 PCT/CN2005/000332 CN2005000332W WO2005088295A1 WO 2005088295 A1 WO2005088295 A1 WO 2005088295A1 CN 2005000332 W CN2005000332 W CN 2005000332W WO 2005088295 A1 WO2005088295 A1 WO 2005088295A1
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Prior art keywords
rsd
peak
compound danshen
fingerprint
dripping pills
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PCT/CN2005/000332
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English (en)
Chinese (zh)
Inventor
Yiyu Cheng
Zhengliang Ye
Yongjiang Wu
Xiaohui Fan
Yi Wang
Yuxia Sun
Shuju Li
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Tianjin Tasly Pharmaceutical Co., Ltd.
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Publication of WO2005088295A1 publication Critical patent/WO2005088295A1/fr

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    • A—HUMAN NECESSITIES
    • A61—MEDICAL OR VETERINARY SCIENCE; HYGIENE
    • A61K—PREPARATIONS FOR MEDICAL, DENTAL OR TOILETRY PURPOSES
    • A61K36/00—Medicinal preparations of undetermined constitution containing material from algae, lichens, fungi or plants, or derivatives thereof, e.g. traditional herbal medicines
    • A61K36/18—Magnoliophyta (angiosperms)
    • A61K36/185—Magnoliopsida (dicotyledons)
    • A61K36/53—Lamiaceae or Labiatae (Mint family), e.g. thyme, rosemary or lavender
    • A61K36/537—Salvia (sage)
    • 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
    • G01N30/86—Signal analysis
    • G01N30/8675—Evaluation, i.e. decoding of the signal into analytical information
    • G01N30/8686—Fingerprinting, e.g. without prior knowledge of the sample components

Definitions

  • the invention relates to a method for quality control of fangshen dripping pills, in particular to control the quality of the compound danshen dripping pills by using a fingerprint pattern detection method.
  • Cardiovascular and cerebrovascular diseases are common diseases that seriously endanger humans.
  • cardiovascular and cerebrovascular diseases have been on the rise.
  • Compound Danshen preparations are mostly used to treat cardiovascular and cerebrovascular diseases, such as Compound Danshen Tablets, Compound danshen Drop Pills, and Guanxin Danshen Drop Pills.
  • Salvia miltiorrhiza is the dry roots and rhizomes of Salvia miltiorrhiza Bge. It is produced in most parts of the country. Because the quality of Salvia miltiorrhiza varies due to different varieties, places of production, and harvesting time, it is difficult to guarantee the stability of a wide range of manufactured products. At present, the identification of salvia miltiorrhiza and its compound preparations is usually to determine the content of one or two active ingredients or index ingredients of salvia miltiorrhiza, and determine the quality based on its content.
  • tanshinone ⁇ A content (58 pages of Chinese Pharmacopoeia 2000 edition) or danshensu content (Zhang Youqin et al., Chinese Journal of Traditional Chinese Medicine, 2000, 28 (3): 68) are used to identify the quality of danshen medicinal materials; Panaxone to determine Salvia miltiorrhiza variety and origin (Zhi Feijun, China Modern Applied Pharmacy, 1998, 15 (5): 16; Hu Shilin et al., Chinese Journal of Chinese Materia Medica, 1999, 24 (12): 721); using danshensu content ( Yan Changkai et al., Chinese Journal of Hospital Pharmacy, 2000, 20 (10): 600), Protocatechuic aldehyde content (Zheng Mojing et al., China Pharmaceutical Affairs, 2000, 14 (4): 254) or Tanshinone IIA content (Lin Weizhong Et al., Chinese Patent Medicine, 2000, 22 (11): 766) etc.
  • Panax notoginseng is the dried root of the Panaxnotoginseng (Burk.) FH Chen plant of the Araliaceae family, which is mainly produced in Yunnan, Guangxi, and Sichuan. It is a precious specialty medicinal material in China and is commonly used in traditional Chinese medicine.
  • Panax notoginseng mainly contains chemical constituents such as soap ring, polysaccharides, amino acids, etc.
  • the saponin part is the material basis for the effect of activating blood circulation and removing blood stasis, and is the main effective ingredient of panax notoginseng.
  • These ingredients belong to the Dammarane type of tetracyclic triterpenoid saponins, among which ginsenosides R bl and R g personallynotoginsenosides! ⁇ Is the highest content of the three ingredients, notoginsenosides are the most representative compounds of notoginseng.
  • the fingerprint of traditional Chinese medicine refers to the chromatogram or spectrum of a certain type or several types of components that are common in a certain Chinese herbal medicine or proprietary Chinese medicine.
  • the active ingredients of Chinese medicine must never In most cases, the fingerprint of traditional Chinese medicine is of great significance to effectively control the quality of traditional Chinese medicine or proprietary Chinese medicines.
  • the major manufacturers of Japanese traditional Chinese medicine in the 1980s have already adopted high-performance liquid-phase fingerprints to control the quality within the company.
  • high-performance liquid fingerprints were also used method.
  • the current standard for the quality evaluation of traditional Chinese medicines is the identification and determination of one or more active ingredients, active ingredients or index components, as well as routine inspection items prescribed by the Pharmacopoeia, by means of spectrum or chromatography.
  • the 2000 edition of the Chinese Pharmacopoeia [1] contains a total of 602 medicinal materials and proprietary medicines. Among them, 992 were identified by thin layer chromatography, and 308 varieties were determined by content [volume method, spectrometry, liquid color pan method, gas chromatography, and thin layer chromatography scanning method]. Most varieties have general inspection items. Obviously, these quality standards are set to mimic the model of chemicals.
  • Coptis chinensis, Phellodendron amurense and the three needles all contain trabeine, and they are generally used as the detection target, but their functional indications are quite different.
  • the situation with compound preparations is even more complicated.
  • This kind of non-linear one-on-one theory and practice of traditional Chinese medicine shows that the quality of traditional Chinese medicine should adopt some kind of macroscopic and comprehensive quality evaluation method.
  • Fufang Danshen Diwan is a drip preparation made from Danshen and Sanqi as the main raw materials. It is clinically used to treat various diseases caused by cardiovascular and cerebrovascular diseases, coronary heart disease, angina pectoris, myocardial ischemia, and microcirculation disorders. Its therapeutic effect has been clinically verified, and whether the quality of the drug and the content of active ingredients in the compound Danshen dripping pills can be guaranteed is the basis for determining the efficacy of the compound Danshen dripping pills. If one or two active ingredients of Danshen are used to explain the intrinsic quality of Fufang Danshen Diwan, it has a certain one-sidedness, not to mention the non-medicinal index component.
  • the object of the present invention is to provide a method for quality control of compound Danshen dripping pills, by which the quality of compound Danshen dripping pills can be controlled.
  • the purpose of the present invention is to establish a method for quality control of traditional Chinese medicine compound preparations. Under a certain condition, the present invention uses a large number of experiments to compare the fingerprint of a compound Danshen dripping pill control sample with the fingerprint of a Danshen medicinal material and the fingerprint of a compound Danshen dripping pill intermediate.
  • the invention can be implemented by the following steps:
  • the above reference solution was sucked and injected into a liquid chromatograph, and the measurement was performed using high performance liquid chromatography to obtain a comparative fingerprint of the compound Danshen dripping pills.
  • Chromatographic parts The column was filled with octadecylsilane bonded silica gel; Mobile phase A is an aqueous phosphoric acid solution; mobile phase B is an acetonitrile phosphoric acid aqueous solution; the detection wavelength is 275-285nm;
  • the preferred method of the invention comprises the following steps:
  • a more preferred method of the present invention includes the following steps:
  • the column is filled with octadecylsilane bonded silica;
  • the mobile phase A is 0.02% phosphoric acid aqueous solution;
  • the mobile phase B is 80% acetonitrile 0.02% phosphoric acid aqueous solution;
  • the gradient elution procedure is as follows:
  • mobile phase A is 90% 0.02% phosphoric acid aqueous solution
  • mobile phase B is 10% 80% acetonitrile 0.02% phosphoric acid aqueous solution
  • the mobile phase A is 78% 0.02% phosphoric acid in water
  • the mobile phase B is
  • mobile phase A is 74% 0.02% phosphoric acid aqueous solution
  • mobile phase B is 26% 80% acetonitrile 0.02% phosphoric acid aqueous solution
  • mobile phase A is 48% 0.02% phosphoric acid aqueous solution
  • mobile phase B is 52% 80% acetonitrile 0.02% phosphoric acid aqueous solution
  • the flow rate is 1.000ml / min
  • the detection wavelength is 280nm
  • the column temperature is 30 ° C. Volume 10 ⁇ l;
  • the preparation ratio of the mobile phase A solution is prepared by volume ratio
  • the preparation ratio of the mobile phase B solution is prepared by volume ratio
  • Peak No. 1 average retention time RT is 6.04min, RSD is 0.31%, peak area is 1627.92, RSD is 5.91%; Peak No. 2, with an average retention time RT of 9.90 ⁇ , RSD of 0.25%, a peak area of 2575.54, and an RSD of 13.53%;
  • Peak No. 8 the average retention time RT is 31.02min, the RSD is 1.18%, the peak area is 1852.33, and the RSD is 14.84%;
  • Peak No. 1 average retention time RT is 6.04min, RSD is 0.31%, peak area is 1627.92, RSD is 5.91%;
  • Peak No. 2 with an average retention time RT of 9.90 min, an RSD of 0.25%, and a peak area of
  • Peak No. 6 with an average retention time RT of 23.74min, an RSD of 0.76%, a peak area of 555.35, and an RSD of 10.48%;
  • Peak No. 8 with an average retention time RT of 31.02min, an RSD of 1.18%, a peak area of 1852.33, and an RSD of 14.84%;
  • Peak No. 1 average retention time RT is 6.04miii, RSD is 0.31%, peak area is 1627.92, RSD is 5.91%;
  • Peak No. 2 with an average retention time RT of 9.90 min, RSD of 0.25%, a peak area of 2575.54, and an RSD of 13.53%;
  • Peak No. 3 with an average retention time RT of 16.89 min, an RSD of 0.61%, a peak area of 366.89, and an RSD of 10.92%;
  • Peak No. 4 average retention time RT is 17.84min, RSD is 0.07%, peak area is 381.40, RSD is 13.81%;
  • Peak No. 5 with an average retention time RT of 20.31 min, an RSD of 0.96%, a peak area of 186.08, and an RSD of 12.04%;
  • Peak No. 6 with an average retention time of 23.74 min, RSD of 0.76%, peak area of 555.35, and RSD ⁇ 10.48%;
  • Peak 7 the average retention time RT was 27.73min, the RSD was 0.50%, the peak area was 281.91, and the RSD was 18.08%;
  • the following methods are used to control the quality of Fufang Danshen Dripping Pills, the Fufang Danshen Dripping Pills to be tested are taken, and the preparation method, chromatographic conditions, and measuring methods of Fufang Danshen Dripping Pills are exactly the same, and the fingerprint is obtained. Compare the fingerprint of the product of the compound Danshen dripping pills with the fingerprint of the compound danshen dripping pills. When the fingerprints of the two have three or more identical chromatographic peaks, the quality of the compound Danshen dripping pills is determined. qualified.
  • the fingerprint of the product of the compound Danshen dripping pill is compared with the fingerprint of the compound Danshen dripping pill. If the fingerprints of the two have 5 or more identical chromatographic peaks, the quality of the product of the compound Danshen dripping pill is considered to be qualified. .
  • the fingerprint of the product of the compound Danshen dripping pill is compared with the fingerprint of the compound Danshen dripping pill.
  • the fingerprints of the two have 7 or more identical chromatographic peaks, the quality of the product of the compound Danshen dripping pill is determined. qualified.
  • the fingerprint of the product of the compound Danshen dripping pill is compared with the fingerprint of the compound Danshen dripping pill.
  • the fingerprints of the two have the same color borrowing peaks, the product of the compound Danshen dripping pill is considered to be qualified.
  • the method for determining the high-performance liquid standard fingerprint of chemical constituents in Salvia miltiorrhiza is as follows: Preparation of Salvia miltiorrhiza standard specimens: Crush the salvia miltiorrhiza, place it in a flask, add water, heat to reflux, let cool, collect the reflux solution, and add water to the residue Heating and refluxing, cooling, collecting the refluxing liquid, combining the two refluxing liquids, adjusting the volume, and filtering, as the standard sample solution of Salvia miltiorrhiza;
  • Chromatographic conditions The column uses octadecylsilane bonded silica as a filler; gradient elution is used, and mobile phase A is ringworm acid ⁇ water solution; mobile phase B is acetonitrile phosphoric acid aqueous solution, flow rate LOOOml / min, detection wavelength 280nm, column temperature 30. C;
  • the preferred method for determining the chemical composition of Salvia miltiorrhiza by high-performance liquid fingerprints is as follows: Preparation of Salvia miltiorrhiza standard sample: Take 2.5 g of crushed salvia miltiorrhiza, place it in a flask, add 50 ml of water, heat under reflux for 1.5 hours, and let cool. Collect the reflux solution, add 50 ml of water to the residue, and heat reflux for 1 hour, let it cool, collect the reflux solution, combine the two decoction reflux solutions in a 100 ml volumetric flask, make up the volume, and filter as the standard sample of Salvia miltiorrhiza.
  • the column uses octadecylsilane bonded silica as the filler; gradient elution is used, and the mobile phase A phase is 0.02% phosphoric acid aqueous solution; the mobile phase B phase is 80% acetonitrile 0.02% phosphoric acid aqueous solution; color i ⁇
  • the mobile phase elution gradient is as follows:
  • mobile phase A is 90% 0.02% phosphoric acid aqueous solution
  • mobile phase B is 10% 80% acetonitrile 0.02% phosphoric acid aqueous solution
  • mobile phase A is 78% 0.02% phosphoric acid aqueous solution
  • mobile phase B is 22% 80% acetonitrile 0.02% phosphoric acid aqueous solution
  • mobile phase A is 74% 0.02% phosphoric acid aqueous solution
  • mobile phase B 26% 80% acetonitrile 0.02% phosphoric acid aqueous solution
  • mobile phase A is 48% 0.02% aqueous solution of plaque acid
  • mobile phase B is 52% 80% acetonitrile 0.02% phosphoric acid aqueous solution
  • the flow rate is 1.000ml / min
  • the detection wavelength is 280nm
  • the column temperature is 30 ° C.
  • the chemical composition of the salvia miltiorrhiza component in the salvia miltiorrhiza component has 9 chromatographic peaks, of which there are 9 chromatographic peaks whose single peak area exceeds 2% of the total peak area, respectively:
  • Peak No. 1 average retention time RT is 5.99min, RSD is 0.45%, peak area is 784.93, RSD is 7.34%;
  • Peak No. 2 has an average retention time RT of 9.85 min, an RSD of 0.47%, a peak area of 916.57, and an RSD of 6.06%;
  • Peak No. 3 with an average retention time RT of 20.13 min, an RSD of 0.46%, a peak area of 778.87, and an RSD of 8.78%;
  • Peak No. 4 with an average retention time of 22.37 min, an RSD of 0.77%, a peak area of 1165.13, and an RSD of 7.60%;
  • Peak No. 5 with an average retention time of 23.49min, RSD of 0.45%, peak area of 1076.7, and RSD of 3.70%;
  • Peak No. 6 with an average retention time RT of 24.51min, an RSD of 0.46%, a peak area of 802.43, and an RSD of 8.21%;
  • Peak 7 average retention time RT is 27.26min, RSD is 0.44%, peak area is 9017.8, RSD is 10.82%;
  • Peak No. 8 with an average retention time of 29.71 min, RSD of 0.32%, peak area of 539.37, and RSD of 13.30%;
  • the chemical composition of the salvia miltiorrhiza component in the salvia medicinal material has 9 color peaks, of which there are 7 chromatographic peaks with a single peak area exceeding 5% of the total peak area, which are:
  • Peak No. 1 average retention time RT is 5.99min, RSD is 0.45%, peak area is 784.93, RSD is 7.34%;
  • Peak No. 2 with an average retention time RT of 9.85min, RSD of 0.47%, peak area of 916.57, and RSD of 6.06%;
  • Peak No. 3 with an average retention time RT of 20.13 min, an RSD of 0.46%, a peak area of 778.87, and an RSD of 8.78%;
  • Peak No. 4 with an average retention time of 22.37min, an RSD of 0.77%, a peak area of 1165.13, and an RSD of 7.60%;
  • Peak No. 5 with an average retention time of 23.49 min, RSD of 0.45%, peak area of 1076.7, and RSD of 3.70%;
  • Peak No. 6 with an average retention time RT of 24.51min, an RSD of 0.46%, a peak area of 802.43, and an RSD of 8.21%;
  • the chemical constituents of Salvia miltiorrhiza in the Salvia miltiorrhiza component have 9 chromatographic peaks, of which there is 1 chromatographic peak with a single peak area exceeding 10% of the total peak area, and the peak is as follows:
  • Peak No. 7 had an average retention time RT of 27.26 min, an RSD of 0.44%, a peak area of 9017.8, and an RSD of 10.82%.
  • Chromatographic conditions The chromatographic column is filled with octadecylsilane bonded silica gel; gradient elution is adopted, and the mobile phase A phase is 0.02% phosphoric acid aqueous solution; the mobile phase B phase is 80% acetonitrile 0.02% phosphoric acid aqueous solution; chromatographic mobile phase
  • the elution gradient is as follows:
  • mobile phase A is 90% 0.02% phosphoric acid aqueous solution
  • mobile phase B is 10% 80% acetonitrile 0.02% phosphoric acid aqueous solution
  • mobile phase A is 78% 0.02% phosphoric acid aqueous solution
  • mobile phase B is 22% 80% acetonitrile 0.02% phosphoric acid aqueous solution
  • the mobile phase A is 74% 0.02% phosphoric acid aqueous solution
  • the mobile phase B is 26% 80% acetonitrile 0.02% steric acid aqueous solution
  • mobile phase A is 48% of 0.02% gramic acid aqueous solution
  • mobile phase B is 52% of 80% acetonitrile 0.02% phosphoric acid aqueous solution
  • the flow rate is 1.000 ml / min
  • the detection wavelength is 280 nm
  • the column temperature is 30 ° C.
  • the chemical composition of the salvia miltiorrhiza component in the compound danshen Diwan Intermediate has 8 chromatographic peaks, of which there are 8 chromatographic peaks whose single peak area exceeds 2% of the total peak area, respectively:
  • Peak No. 1 average retention time RT is 6.12min, RSD is 0.83%, peak area is 2554.6, RSD is 10.68%;
  • Peak No. 2 with an average retention time RT of 10,000 min, RSD of 0.77%, peak area of 4438.6, and RSD of 14.63%;
  • Peak No. 3 average retention time RT is 15.96min, RSD is 0.58%, peak area is 740.16, RS is 13.18%;
  • Peak No. 4 average retention time RT is 17.89min, RSD is 1.17%, peak area is 667.68, RSD is 13.47%;
  • Peak No. 5 with an average retention time RT of 20.27min, an RSD of 2.94%, a peak area of 654.73, and an RSD of 15.01%;
  • Peak No. 6 with an average retention time RT of 23.83 min, an RSD of 0.88%, a front area of 1140.51, and an RSD of 16.45%;
  • Peak 7 average retention time RT is 27.67min, RSD is 0.61%, peak area is 880.14, RSD is 11.49%;
  • Peak No. 8 had an average retention time RT of 30.93 min, an RSD of 0.47%, a peak area of 2965.29, and an RSD of 10.21%.
  • the chemical composition of the salvia miltiorrhiza component in the compound danshen Diwan Intermediate has 8 chromatographic peaks, of which there are 6 chromatographic peaks with a single peak area exceeding 5% of the total peak area, respectively:
  • Peak No. 1 average retention time RT is 6.12min, RSD is 0.83%, peak area is 2554.6, RSD is 10.68%;
  • Peak No. 3 average retention time RT is 15.96min, RSD is 0.58%, peak area is 740.16, RSD is 13.18%;
  • Peak No. 6 with an average retention time of 23.83 min, RSD of 0.88%, a peak area of 1140.51, and an RSD of 16.45%;
  • Peak No. 7 with an average retention time RT of 27.67min, an RSD of 0.61%, a peak area of 880.14, and an RSD of 11.49%;
  • Peak No. 8 had an average retention time RT of 30.93 min, an RSD of 0.47%, a peak area of 2965.29, and an RSD of 10.21%.
  • Peak No. 1 average retention time RT is 6.12min, RSD is 0.83%, peak area is 2554.6, RSD is 10.68%;
  • Peak No. 2 with an average retention time RT of 10.00mm, an RSD of 0.77%, a peak area of 4438.6, and an RSD of 14.63%;
  • Peak No. 8 had an average retention time RT of 30.93 min, an RSD of 0.47%, a peak area of 2965.29, and an RSD of 10.21%.
  • the quality control standard can objectively reflect the presence and content of the internal ingredients of the product in order to comprehensively control the quality of the product.
  • the present invention provides a new control standard for a complete and accurate evaluation of the quality of Fufang Danshen Diwan, and will contribute to improving the quality and efficacy of Fufang Danshen Diwan and other prescriptions with Danshen and Panax notoginseng as main ingredients.
  • the invention has the characteristics of simple method, stable, high precision, good reproducibility, and easy to handle.
  • the invention provides a method for identifying compound Danshen dripping pills, and the invention is a practical method obtained through a large number of experiments.
  • the high-performance liquid standard fingerprint fingerprints of the chemical components of Danshen in compound Danshen dripping pills obtained by high-performance liquid and under the same test conditions have the characteristics of good reproducibility, so it can be established by the above determination method.
  • the fingerprint of Compound Danshen Diwan pills is used as a standard fingerprint to identify traditional Chinese medicine preparations containing the active ingredients of Danshen and Panax notoginseng.
  • the fingerprints of chemical constituents in Salvia miltiorrhizae and the intermediates of Fufang Danshen Diwan are given below.
  • the fingerprints of the chemical components of Salvia miltiorrhiza, the fingerprints of the chemical components of Salvia miltiorrhiza in the compound danshen dripping pills, and the comparison of the HPLC fingerprints of the chemical components of Salvia miltiorrhiza from different sources are intended to further illustrate the present invention, but not to limit the present invention.
  • Example 5 (Preparation Example) Salvia weighed 116.35g, thirty-seven 58. 2 lg, add boiling water twice, four times the amount of water for the first time 2 hours, 3 times the amount of water a second time 1.5 hours, filtered and the filtrate were combined, concentrated to a specific gravity of 1.19- At 1.20 (75 ⁇ 1 ° C), add ethanol at a concentration of about 88% to an ethanol content of 66% (20 ° C), leave it for 10 hours, separate the supernatant, recover the ethanol, and concentrate to a relative density of 1.40. (55-60 ° C) to obtain Danshen Sanqi extract.
  • Embodiment 7 Finger Danshen Diwan Pill Danshen Component Fingerprint Detection Example
  • Reagents acetonitrile (chromatographically pure, American Merck), phosphoric acid (superior pure), Wahaha purified water.
  • Preparation of control sample of compound Danshen dripping pills Take 10 tablets of compound Danshen dripping pills in each batch of Example 1, accurately weigh them, place them in a 10ml volumetric flask, add distilled water for 15 minutes, dissolve, make volume, and filter, which is the control. sample.
  • Salvia miltiorrhiza standard sample Take 2.5 g of salvia miltiorrhiza (crush), place it in a flask, add 50 ml of water, heat to reflux for 1.5 hours, let it cool, and collect the reflux solution. 50 ml of water was added to the residue, and the mixture was heated under reflux for 1 hour, allowed to cool, and the reflux solution was collected. The two decoction reflux solutions were combined in a 100 ml volumetric flask, and the volume was adjusted and filtered to obtain the standard sample.
  • phase A is 0.02% phosphoric acid aqueous solution
  • phase B is 80% acetonitrile 0.02% phosphoric acid aqueous solution.
  • the flow rate was 1.000 ml / min
  • the detection wavelength was 280 nm
  • the column temperature was 30 ° C
  • the injection volume was 10 ⁇ 1.
  • the chromatographic mobile phase elution gradient is as follows:
  • Peak No. 1 average retention time RT is 6.04min, RSD is 0.31%, peak area is 1627.92, RSD is 5.91%;
  • Peak No. 2 with an average retention time RT of 9.90 min, RSD of 0.25%, a peak area of 2575.54, and an RSD of 13.53%;
  • Peak No. 8 with an average retention time RT of 31.02min, an RSD of 1.18%, a peak area of 1852.33, and an RSD of 14.84%;
  • Peak No. 1 average retention time RT is 6.04min, RSD is 0.31%, peak area is 1627.92, RSD is 5.91%;
  • Peak No. 2 average retention time RT is 9.90min, RSD is 0.25%, peak area is
  • Peak No. 6 with an average retention time RT of 23.74min, an RSD of 0.76%, a peak area of 555.35, and an RSD of 10.48%;
  • Peak No. 8 with an average retention time RT of 31.02min, an RSD of 1.18%, a peak area of 1852.33, and an RSD of 14.84%;
  • Peak No. 1 average retention time RT is 6.04min, RSD is 0.31%, peak area is 1627.92, RSD is 5.91%; Peak No. 2, with an average retention time RT of 9.90 min, an RSD of 0.25%, a peak area of 2575.54, and an RSD of 13.53%;
  • Peak No. 3 with an average retention time RT of 16.89 min, an RSD of 0.61%, a peak area of 366.89, and an RSD of 10.92%;
  • Peak No. 4 with an average retention time RT of 17.84min, an RSD of 0.70%, a peak area of 381.40, and an RSD of 13.81%;
  • Peak No. 5 with an average retention time RT of 20.31 min, an RSD of 0.96%, a peak area of 186.08, and an RSD of 12.04%;
  • Peak No. 6 with an average retention time RT of 23.74min, an RSD of 0.76%, a peak area of 555.35, and an RSD of 10.48%;
  • Peak 7 average retention time RT is 27.73min, RSD is 0.50%, peak area is 281.91, RSD is 18.08%;
  • Peak No. 8 had an average retention time RT of 31.02 min, an RSD of 1.18%, a peak area of 1852.33, and an RSD of 14.84%.

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Abstract

L'invention concerne un procédé de contrôle de qualité destiné à des pilules à avaler composées de danshen, qui consiste: à obtenir l'empreinte digitale des pilules à avaler composées de danshen de conférence par HPLC dans des conditions décrites dans l'invention; dans ces même conditions, à obtenir l'empreinte digitale des pilules à avaler composées de danshen détecté par ce même procédé; à comparer ces deux empreintes digitales lorsqu'elles ont le même nombre chromatographique maximal en tant que valeur décrite dans cette invention, la qualité des pilules à avaler composées de danshen détecté étant considérée comme bonne.
PCT/CN2005/000332 2004-03-17 2005-03-17 Procede de controle de qualite destine aux pilules a avaler composees de danshen WO2005088295A1 (fr)

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CN200410018756.5 2004-03-17
CN200410018756 2004-03-17

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WO2005088295A1 true WO2005088295A1 (fr) 2005-09-22

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CN105486787A (zh) * 2015-12-04 2016-04-13 广东药学院 微乳色谱测定丹参有效成分指纹图谱的方法及应用
CN110632190A (zh) * 2019-08-28 2019-12-31 湖南先伟实业有限公司 迷迭香中迷迭香酸、鼠尾草酸、鼠尾草酚同时测定的方法
CN112946118A (zh) * 2021-02-01 2021-06-11 贵州金桥药业有限公司 一种药物指纹图谱的测定方法及其指纹图谱
CN114166958A (zh) * 2021-10-29 2022-03-11 合肥创新医药技术有限公司 中药复方苍藿平胃颗粒的指纹图谱的检测方法及其应用
CN114660194A (zh) * 2022-03-16 2022-06-24 西双版纳傣族自治州民族医药研究所(西双版纳傣族自治州傣医医院) 雅拢牛哈占波方剂的hplc指纹图谱构建方法及检测方法
CN114965726A (zh) * 2021-11-03 2022-08-30 葵花药业集团(佳木斯)有限公司 一种咀嚼片的指纹图谱检测方法及其指纹图谱
CN115184493A (zh) * 2022-07-06 2022-10-14 株洲市食品药品检验所 一种南方红豆杉药材及其中药饮片中活性成分的指纹图谱检测方法
CN115201364A (zh) * 2022-07-02 2022-10-18 浙江金大康动物保健品有限公司 一种降香药材的一板20余种成分信息斑点薄层鉴别方法

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CN105486787A (zh) * 2015-12-04 2016-04-13 广东药学院 微乳色谱测定丹参有效成分指纹图谱的方法及应用
CN110632190A (zh) * 2019-08-28 2019-12-31 湖南先伟实业有限公司 迷迭香中迷迭香酸、鼠尾草酸、鼠尾草酚同时测定的方法
CN112946118A (zh) * 2021-02-01 2021-06-11 贵州金桥药业有限公司 一种药物指纹图谱的测定方法及其指纹图谱
CN114166958A (zh) * 2021-10-29 2022-03-11 合肥创新医药技术有限公司 中药复方苍藿平胃颗粒的指纹图谱的检测方法及其应用
CN114166958B (zh) * 2021-10-29 2024-03-29 合肥创新医药技术有限公司 中药复方苍藿平胃颗粒的指纹图谱的检测方法及其应用
CN114965726A (zh) * 2021-11-03 2022-08-30 葵花药业集团(佳木斯)有限公司 一种咀嚼片的指纹图谱检测方法及其指纹图谱
CN114965726B (zh) * 2021-11-03 2024-01-30 葵花药业集团(佳木斯)有限公司 一种咀嚼片的指纹图谱检测方法及其指纹图谱
CN114660194A (zh) * 2022-03-16 2022-06-24 西双版纳傣族自治州民族医药研究所(西双版纳傣族自治州傣医医院) 雅拢牛哈占波方剂的hplc指纹图谱构建方法及检测方法
CN114660194B (zh) * 2022-03-16 2023-10-10 西双版纳傣族自治州民族医药研究所(西双版纳傣族自治州傣医医院) 雅拢牛哈占波方剂的hplc指纹图谱构建方法及检测方法
CN115201364A (zh) * 2022-07-02 2022-10-18 浙江金大康动物保健品有限公司 一种降香药材的一板20余种成分信息斑点薄层鉴别方法
CN115184493A (zh) * 2022-07-06 2022-10-14 株洲市食品药品检验所 一种南方红豆杉药材及其中药饮片中活性成分的指纹图谱检测方法

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