CN102759585A - Method for controlling full-time interval multi-wavelength fused fingerprint quality of qi stagnation and stomachache granules - Google Patents

Method for controlling full-time interval multi-wavelength fused fingerprint quality of qi stagnation and stomachache granules Download PDF

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CN102759585A
CN102759585A CN2012102233064A CN201210223306A CN102759585A CN 102759585 A CN102759585 A CN 102759585A CN 2012102233064 A CN2012102233064 A CN 2012102233064A CN 201210223306 A CN201210223306 A CN 201210223306A CN 102759585 A CN102759585 A CN 102759585A
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wavelength
reference substance
quality
granules
qizhi weitong
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CN102759585B (en
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孟宪生
潘英
韩凌
包永睿
何晓霞
姚东
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Liaoning Huarun Benxi Sanyao Co Ltd
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Liaoning Huarun Benxi Sanyao Co Ltd
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Abstract

The invention discloses a method for controlling the full-time interval multi-wavelength fused fingerprint quality of qi stagnation and stomachache granules. The method combines a fingerprint technology with a computer information fusion technology, so different compound chromatographic and spectral information is effectively fused, the preparation quality reflection incompleteness of a single wavelength and a single indicator is eliminated, and furthermore, the preparation quality can be comprehensively and clearly evaluated. The method for controlling quality has convenience, an accurate result and better reproducibility, and can be used for traditional Chinese medicine quality evaluation, traditional Chinese medicine quality control and research and development of new traditional Chinese medicines. Particularly, the method can be used as one indicator for quality control and authentication of the qi stagnation and stomachache granules.

Description

Qizhi weitong granules all the period of time multi-wavelength merges fingerprint pattern quality control method
Technical field
The present invention relates to a kind of control method of Chinese medicine preparation quality, is that a kind of qizhi weitong granules all the period of time multi-wavelength merges fingerprint pattern quality control method specifically.
Background technology
The electuary for stomachache caused by qi stagnation prescription is: radix bupleuri, long-pending shell, the root of herbaceous peony, Radix Glycyrrhizae, rhizoma cyperi, corydalis tuber etc. and its prescription derives from " Sini Tang " in the treatise on Febrile Diseases. and we are main with radix bupleuri, transfer to reach irritability, unclog and readjust the stagnation of the circulation of vital energy. the Fructus Aurantii regulating the flow of QI to ease the stomach; Dissipate-swelling removes full, spleen benefiting and stimulating the appetite. the pain relieving of root of herbaceous peony astringe yin, nourishing blood and liver; The benefit spleen is let out wood in soil. and the Radix Glycyrrhizae coordinating the drug actions of a prescription is for making, rhizoma cyperi assistance radix bupleuri regulating the function of the liver and spleen in addition, regulating qi-flowing for relieving pain. the act like a bully good medicine of promoting blood circulation and stopping pain of unit; All medicines are harmonious, and reach the effect of dispersing stagnated hepatoqi pain relieving jointly. and qizhi weitong granules at clinical indication is: epigastric pain, have a pain to attack support; Gastral cavity connects the characteristics of the side of body bitterly, and is uncomfortable with the gastral cavilty turgor, instigates gas frequent; Every bad because of feelings will, angry then turgor pain increases the weight of. the modern clinical treatment of diseases such as chronic gastritis, acute gastritis, gastric ulcer, enterogastritis that are usually used in.There is experimental study to prove that further qizhi weitong granules has significant analgesic effect simultaneously, and can obviously suppresses mouse gastric emptying and intestines propulsion functions; Show that in body bowel movement experiment this medicine does not have obvious influence to the wriggling number of times of intestines, but the wriggling wave amplitude is obviously increased, explain that this medicine can obviously increase the intensity of enterocinesia under the situation that does not increase the enterocinesia number of times.Show that thus this medicine is its function of scalable when gastrointestinal function is hyperfunction, to reach the effect of spasmolysis and analgesia.Tentative ulcer and hydrochloric acid in gastric juice, pepsic analysis show that this medicine has antiulcer, suppress gastric secretion, reduce the effect of hydrochloric acid in gastric juice and pepsin activity.Recent study finds that also the qizhi weitong granules drug combination has many new effects, like treatment coronary heart disease, ephritis and hypertension etc., all is common disease and high morbidity.
Along with science and technology development, modern good analysis and detecting instrument is popularized, and the information processing technology is ripe day by day, Chinese medicine preparation check and analysis level has been had significantly improve, and the Chinese medicine preparation method of quality control is constantly perfect.Wherein fingerprint pattern technology is brought into play more and more vital role as a kind of quality assessment pattern in the Chinese medicine preparation quality control.Finger-print is to adopt analysis detection meanss such as chromatogram, spectrum and wave spectrum that the material base of Chinese crude drug or Chinese patent drug is detected, and formation can be reacted the ensemble of communication of Chinese crude drug and Chinese patent drug quality.Information fusion technology can carry out reasonable integration with multi-source information, to obtain by the reasonable dismissal of integrate information or description.Make full use of the modern good bulk information that analysis and detecting instrument obtained and the powerful information processing function of computing machine, can obtain a kind of complete and effective method of quality control comparatively.
Summary of the invention
The purpose of this invention is to provide a kind of qizhi weitong granules all the period of time multi-wavelength and merge fingerprint pattern quality control method, a kind of comprehensive, stable and reliable evaluation method can be provided for the quality control of qizhi weitong granules.
The present invention realizes through following technical scheme:
Qizhi weitong granules all the period of time multi-wavelength merges the method for quality control of finger-print, it is characterized in that comprising step down:
(1) preparation of need testing solution: get these article qizhi weitong granules porphyrize, get 5-6g, the accurate title, decide, and puts in the tool plug conical flask, the accurate distilled water 100mL that adds; Close plug is claimed to decide weight, and sonicated (power 250W, frequency 33kHZ) 60-120 minute is taken out; Put coldly, claim again decide weight, supply the weight that subtracts mistake, shake up filtration with distilled water; The accurate filtrating 25ml that draws is added on the AB-8 resin column (0.3-1.25mm, 20g, internal diameter 1.5cm), washs with distilled water 150ml; Use the 200ml95% ethanol elution again, collect ethanol eluate, evaporate to dryness, residue add 20% acetonitrile to be made dissolving and is transferred in the 10ml volumetric flask; Add 20% acetonitrile and be settled to scale, shake up, filter, get filtrating and promptly get;
(2) preparation of reference substance solution: it is an amount of that precision takes by weighing RADIX PAEONIAE ALBA glycosides reference substance, Paeoniflorin reference substance and mono-ammonium glycyrrhizinate reference substance; Adding methyl alcohol processes every 1mL respectively and contains RADIX PAEONIAE ALBA glycosides reference substance 0.266mg, Paeoniflorin reference substance 0; The solution of 428mg and mono-ammonium glycyrrhizinate reference substance 0.1536mg promptly gets;
(3) chromatographic condition and system suitability test: use the Agilent TC-C of octadecylsilane chemically bonded silica as filling agent 18(4.6mm * 250 mm, 5 μ m) chromatographic column; With 0.02% formic acid water is mobile phase A, is Mobile phase B with the acetonitrile, carries out gradient elution; Flow velocity 1.0 mL/min; 30 ℃ of column temperatures; The DAD detecting device detects under wavelength 230 nm, 254nm simultaneously; Sample size 10 μ L; Theoretical cam curve is calculated, and should be not less than 3000;
Table 1 eluent gradient wash-out table
Time (min) Mobile phase A (%) Mobile phase B (%)
0 95 5
10 90 10
61 63 27
70 60 40
90 50 50
(4) multi-wavelength merges all the period of time: utilize computer software to carry out all the period of time fusion spectral data 230nm and two wavelength of 254nm under, obtain after the fusion that can reflect two wavelength simultaneously chromatogram and set of diagrams and compose data.
(5) sample size is measured: use the finger-print data after merging, the content of index property composition in the calculation sample.
(6) above-mentioned definite content assaying method is carried out efficiency evaluation, comprising specificity, accuracy, precision, repeatability, stability, linearity, scope and durability.
The good effect that qizhi weitong granules all the period of time multi-wavelength of the present invention merges fingerprint pattern quality control method is:
(1) the present invention discloses qizhi weitong granules all the period of time multi-wavelength fusion fingerprint pattern quality control method first, can control the quality of qizhi weitong granules comprehensively and effectively through this method.
(2) the present invention utilizes the modern analysis detecting instrument, and chemical constitution complicated in the qizhi weitong granules is carried out analyzing and testing, has obtained a large amount of chromatogram and spectral informations about chemical constitution in the qizhi weitong granules.
(3) the present invention utilizes information fusion technology, and a large amount of chromatograms and the spectral information that obtains effectively merged, and on the basis of not losing original characteristic information, obtains reflecting the finger-print chromatogram and the spectrum data of the qizhi weitong granules quality of the pharmaceutical preparations.
(4) the present invention adopts qizhi weitong granules all the period of time multi-wavelength to merge the fingerprint qualitative analysis that the finger-print chromatogram can be used for qizhi weitong granules; Spectrum data is used for the quantitative test of qizhi weitong granules multi-target ingredient; The perfect quality control standard of qizhi weitong granules; Thereby effectively guaranteed safety, the homogeneous, stable, effective, controlled of qizhi weitong granules, guaranteed the standardization of technology and the stable and consistent of quality.
(5) method of quality control of the present invention, its advantage be easy, stable, precision is high, favorable reproducibility, be easy to grasp, and can hold its quality situation from the global feature looks of qizhi weitong granules.
Description of drawings
Fig. 1 is reference substance RADIX PAEONIAE ALBA glycosides under the 230nm wavelength, Paeoniflorin and mono-ammonium glycyrrhizinate chromatic graph spectrum.
Fig. 2 is reference substance RADIX PAEONIAE ALBA glycosides under the 254nm wavelength, Paeoniflorin and mono-ammonium glycyrrhizinate chromatic graph spectrum.
Fig. 3 is the UV scanning figure of RADIX PAEONIAE ALBA glycosides.
Fig. 4 is the UV scanning figure of Paeoniflorin.
Fig. 5 is the UV scanning figure of mono-ammonium glycyrrhizinate.
Fig. 6 is a HPLC finger-print under the qizhi weitong granules 230nm wavelength.
Fig. 7 is a HPLC finger-print under the qizhi weitong granules 254nm wavelength.
Fig. 8 is chromatogram and the fingerprint peaks that qizhi weitong granules all the period of time multi-wavelength merges.
Embodiment
Qizhi weitong granules all the period of time multi-wavelength merges the method for quality control of finger-print, may further comprise the steps:
1, the preparation of need testing solution: get these article qizhi weitong granules porphyrize, get 5g, the accurate title, decide, and puts in the tool plug conical flask, the accurate distilled water 100mL that adds; Close plug is claimed to decide weight, and sonicated (power 250W, frequency 33kHZ) 60 minutes is taken out; Put coldly, claim again decide weight, supply the weight that subtracts mistake, shake up filtration with distilled water; The accurate filtrating 25ml that draws is added on the AB-8 resin column (0.3-1.25mm, 20g, internal diameter 1.5cm), washs with distilled water 150ml; Use the 200ml95% ethanol elution again, collect ethanol eluate, evaporate to dryness, residue add 20% acetonitrile to be made dissolving and is transferred in the 10ml volumetric flask; Add 20% acetonitrile and be settled to scale, shake up, filter, get filtrating and promptly get;
Use the Agilent TC-C of octadecylsilane chemically bonded silica as filling agent 18(4.6mm * 250 mm, 5 μ m) chromatographic column; With 0.02% formic acid water is mobile phase A, is Mobile phase B with the acetonitrile, carries out gradient elution by the regulation in the table 1; Flow velocity 1.0 mL/min; 30 ℃ of column temperatures; The DAD detecting device detects under wavelength 230 nm, 254nm simultaneously; Sample size 10 μ L; Theoretical cam curve is calculated, and should be not less than 3000;
Table 1 eluent gradient wash-out table
Time (min) Mobile phase A (%) Mobile phase B (%)
0 95 5
10 90 10
61 63 27
70 60 40
90 50 50
Qizhi weitong granules method of quality control of the present invention; With the spectral data under 230nm and two wavelength of 254nm by deriving in the analysis and detecting instrument; Utilize computer information processing software that the spectrum data under two wavelength is carried out all the period of time and merge, obtain chromatogram after the fusion that can reflect two wavelength simultaneously.Wherein chromatogram is seen Fig. 8.
Qizhi weitong granules method of quality control of the present invention is with obtaining set of diagrams spectrum data after the fusion of the spectral data under 230nm and two wavelength of 254nm.Wherein the fingerprint peaks spectrum data is seen table 2.
Table 2 fingerprint peaks spectrum data
The peak preface Retention time Peak height Peak area
1 27.810 228.9209 3381.9391
2 28.851 33.5450 503.8468
3 30.912 582.9306 10010.9945
4 40.026 175.5672 3706.2866
5 43.934 38.4946 737.5128
6 46.173 111.2008 1830.7798
7 48.823 1076.819 17686.4292
8 52.930 563.8185 9883.1455
9 67.945 95.1786 1669.6594
10 79.322 86.7376 1085.3113
Qizhi weitong granules method of quality control of the present invention, the finger-print spectrogram that obtains can be used for the fingerprint qualitative analysis of qizhi weitong granules.

Claims (2)

1. qizhi weitong granules all the period of time multi-wavelength merges fingerprint pattern quality control method, it is characterized in that this method comprises step down:
(1) preparation of need testing solution: get these article qizhi weitong granules porphyrize, get 5g, the accurate title, decide, and puts in the tool plug conical flask, the accurate distilled water 100mL that adds; Close plug is claimed to decide weight, uses power to be 250W, and frequency is the 33KHZ ultrasound wave, sonicated 60 minutes; Take out, put coldly, claim again to decide weight, supply the weight that subtracts mistake, shake up with distilled water; Filter, the accurate filtrating 25ml that draws is added in 0.3-1.25mm, and 20g is on the AB-8 resin column of internal diameter 1.5cm; With distilled water 150ml washing, use 200ml 95% ethanol elution again, collect ethanol eluate, evaporate to dryness, residue add 20% acetonitrile to be made dissolving and is transferred in the 10ml volumetric flask; Add 20% acetonitrile and be settled to scale, shake up, filter, get filtrating and promptly get;
(2) preparation of reference substance solution: it is an amount of that precision takes by weighing RADIX PAEONIAE ALBA glycosides reference substance, Paeoniflorin reference substance and mono-ammonium glycyrrhizinate reference substance; Adding methyl alcohol processes every 1mL respectively and contains RADIX PAEONIAE ALBA glycosides reference substance 0.266mg, Paeoniflorin reference substance 0; The solution of 428mg and mono-ammonium glycyrrhizinate reference substance 0.1536mg promptly gets;
(3) chromatographic condition and system suitability test: use the Agilent TC-C of octadecylsilane chemically bonded silica as filling agent 18Chromatographic column, chromatographic column specification are 4.6mm * 250 mm, 5 mm; With 0.02% formic acid water is mobile phase A, is Mobile phase B with the acetonitrile, carries out gradient elution;
The gradient elution technique parameter is:
Time min Mobile phase A % Mobile phase B % 0 95 5 10 90 10 61 63 27 70 60 40 90 50 50
Flow velocity 1.0 mL/min; 30 ℃ of column temperatures; The DAD detecting device detects under wavelength 230 nm, 254nm simultaneously; Sample size 10 μ L; Theoretical cam curve is calculated, and should be not less than 3000;
(4) multi-wavelength merges all the period of time: utilize computer software to carry out all the period of time fusion spectral data 230nm and two wavelength of 254nm under, obtain after the fusion that can reflect two wavelength simultaneously chromatogram and set of diagrams and compose data;
(5) sample size is measured: use the finger-print data after merging, the content of index property composition in the calculation sample;
(6) above-mentioned definite content assaying method is carried out efficiency evaluation, comprising specificity, accuracy, precision, repeatability, stability, linearity, scope and durability.
2. qizhi weitong granules all the period of time multi-wavelength according to claim 1 merges fingerprint pattern quality control method, it is characterized in that: this method can the identical or close any formulation that contains the qizhi weitong granules composition of Detection and Extraction method.
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Cited By (8)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
CN105467051A (en) * 2014-09-11 2016-04-06 富力 Dachuanxiong tablet whole-time multi-wavelength fusion fingerprint quality control method
CN105758950A (en) * 2016-02-26 2016-07-13 辽宁中医药大学 Quality control method based on dose-effect color card for anti-inflammatory and analgesia action of qi-stagnation and stomachache granules
CN105758949A (en) * 2016-02-26 2016-07-13 辽宁中医药大学 Quality control method of gastrointestinal motility promoting power of qi-stagnation and stomachache granules based on dose-effect color card
CN106770001A (en) * 2016-11-11 2017-05-31 本溪国家中成药工程技术研究中心有限公司 Method and application using extract solution concentration process in the preparation process of near infrared spectroscopy quick detection qizhi weitong granules
CN109932432A (en) * 2017-12-15 2019-06-25 富力 The method of quality control of Shenyi capsule bulk pharmaceutical chemicals all the period of time multi-wavelength fusion finger-print
CN113325115A (en) * 2021-07-08 2021-08-31 辽宁华润本溪三药有限公司 Method for establishing characteristic spectrum of qi stagnation stomachache granules and application thereof
CN113433245A (en) * 2021-07-08 2021-09-24 辽宁华润本溪三药有限公司 Method for determining content of saikosaponin in qi stagnation stomachache granules and application thereof
CN116124911A (en) * 2022-08-04 2023-05-16 山东省食品药品检验研究院 Quality evaluation method for Chinese patent medicine based on multisource information fusion

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Cited By (11)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
CN105467051A (en) * 2014-09-11 2016-04-06 富力 Dachuanxiong tablet whole-time multi-wavelength fusion fingerprint quality control method
CN105467051B (en) * 2014-09-11 2017-07-28 富力 The method of quality control of big Ligusticum wallichii piece all the period of time multi-wavelength fusion finger-print
CN105758950A (en) * 2016-02-26 2016-07-13 辽宁中医药大学 Quality control method based on dose-effect color card for anti-inflammatory and analgesia action of qi-stagnation and stomachache granules
CN105758949A (en) * 2016-02-26 2016-07-13 辽宁中医药大学 Quality control method of gastrointestinal motility promoting power of qi-stagnation and stomachache granules based on dose-effect color card
CN105758949B (en) * 2016-02-26 2018-02-06 辽宁中医药大学 Qizhi weitong granules based on dose-effect colour atla promotees gastroenteritic power method of quality control
CN105758950B (en) * 2016-02-26 2018-02-06 辽宁中医药大学 Qizhi weitong granules anti-inflammatory and antalgic method of quality control based on dose-effect colour atla
CN106770001A (en) * 2016-11-11 2017-05-31 本溪国家中成药工程技术研究中心有限公司 Method and application using extract solution concentration process in the preparation process of near infrared spectroscopy quick detection qizhi weitong granules
CN109932432A (en) * 2017-12-15 2019-06-25 富力 The method of quality control of Shenyi capsule bulk pharmaceutical chemicals all the period of time multi-wavelength fusion finger-print
CN113325115A (en) * 2021-07-08 2021-08-31 辽宁华润本溪三药有限公司 Method for establishing characteristic spectrum of qi stagnation stomachache granules and application thereof
CN113433245A (en) * 2021-07-08 2021-09-24 辽宁华润本溪三药有限公司 Method for determining content of saikosaponin in qi stagnation stomachache granules and application thereof
CN116124911A (en) * 2022-08-04 2023-05-16 山东省食品药品检验研究院 Quality evaluation method for Chinese patent medicine based on multisource information fusion

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