CN102297912B - Building method of licorice medicinal material whole-time multi-wavelength fusion fingerprint chromatogram - Google Patents
Building method of licorice medicinal material whole-time multi-wavelength fusion fingerprint chromatogram Download PDFInfo
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Abstract
The invention discloses a creation method of a licorice medicinal material whole-time multi-wavelength fusion fingerprint chromatogram, which combines modern analysis detection means with information processing means, effectively fuses the chromatogram information of traditional Chinese medicine index components, can overcome the disadvantage of insufficient information content during single-wavelength single-index detection, and thus can perfectly reflect the internal quality of the traditional Chinese medicinal material. The quality control method of the invention has simple operation, is stable and reliable, has good reproducibility, and is applicable to quality evaluation and control of traditional Chinese medicinal materials and new medicine research and development of traditional Chinese medicine. Especially, the invention can be used as one of the indexes for licorice medicinal material quality control and identification.
Description
Invention field
The invention belongs to the technical field that adopts modern analysis detection means and information processing means that the quality of Chinese crude drug is detected, the control method that relates to a kind of Chinese crude drug quality says a kind of method for building up of licorice medicinal materials all the period of time multi-wavelength fusion finger-print more specifically.
Background technology
According to record of Pharmacopoeia of People's Republic of China version in 2010: this product is dry root and the rhizome of glycyrrhizic legume, glycyrrhiza inflate bat or glycyrrhiza glabra.Begin to be stated from Sheng Nong's herbal classic, classify as top grade.The gentle current twelve regular channels of this product property of medicine, traditional medicine are thought the effects such as its useful gas bowl spares, clearing heat and detoxicating, expelling phlegm and arresting coughing, relieving spasm to stop pain, coordinating the drug actions of a prescription has saying of " ten side's nine grass ".The clinical treatment that is mainly used in the diseases such as chronic hepatitis cirrhosis, canker, onset EA, pernicious vomiting severe, dysmenorrheal caused by qi stagnation and blood stasis, protrusion of lumber intervertebral disc and the chronic liver disease liver histological improves, chronic liver disease liver cancer becomes inhibition etc.In China, Radix Glycyrrhizae mainly originates in the areas such as the Inner Mongol, Gansu, Xinjiang, northeast, Shanxi.Mainly contain triterpenes and flavones ingredient in Radix Glycyrrhizae, wherein triterpenes components mainly contains glycyrrhizic acid, enoxolone etc.; Flavones ingredient mainly contains liquiritin, 4',7-Dihydroxyflavanone, isoliquiritin etc.
Along with the development of science and technology, the generally use of modern advanced analysis detecting instrument and the gradual perfection of the information processing technology have had the Analysis of Chinese Traditional Medicine detection level and significantly improve, and the traditional Chinese medicine quality control method is updated.By setting up finger-print, the Chinese crude drug index components is carried out a kind of development trend that assay becomes traditional Chinese medicine quality control and estimates in recent years.Traditional Chinese medicine fingerprint refers to some Chinese crude drug or Chinese patent drug through after suitably processing, spectrogram or the chromatogram that can manifest Chinese crude drug or pcm chemical feature that utilize present information acquisition technique and quality analysis means to obtain.Can't realize fingerprint of licorice is carried out comprehensively and the overall evaluation owing to using different pre-treating methods that Radix Glycyrrhizae glycosides, isoliquiritin and mono-ammonium glycyrrhizinate are detected respectively under two different chromatographic conditions, therefore, follow the information maximization principle and set up licorice medicinal materials all the period of time multi-wavelength fusion finger-print and its index components carried out assay can obtain a kind of comparatively effectively method of quality control, thereby guarantee the safe, stable and reliable of licorice medicinal materials quality.
Licorice medicinal materials occupies very consequence in Chinese crude drug.At present, commercially available licorice medicinal materials quality is uneven, so the stability of licorice medicinal materials is difficult to guarantee.The assay of 2010 editions Chinese Pharmacopoeia regulations: this product is pressed dry product and is calculated, and contains liquiritin and must not be less than 0.50%; Glycyrrhizic acid must not be less than 2.0% in ammonium glycyrrhetate.
Summary of the invention
The object of the invention is to adopt modern analysis detection means and information processing means to set up the brand-new finger-print of licorice medicinal materials, and take this finger-print as the basis all the period of time multi-wavelength fusion content assaying method, easier, reasonable, reliable with the method for quality control of guaranteeing licorice medicinal materials.
The present invention is achieved by the following technical solutions:
The method for building up of licorice medicinal materials all the period of time multi-wavelength fusion finger-print is characterized in that the method carries out as follows:
(1) preparation of need testing solution: the extracting Radix Glycyrrhizae medicinal powder is 5g approximately, and is accurately weighed, puts in round-bottomed flask, precision adds entry 100mL, and weighed weight added hot reflux 2 hours, let cool, weighed weight again, water is supplied the weight of less loss, shakes up, filter, the accurate subsequent filtrate 20mL that draws is added on the AB-8 resin column, with distilled water 120mL washing, use again the 100mL95% ethanol elution, collect ethanol eluate, evaporate to dryness, residue add 20% acetonitrile to be made and dissolves and be transferred in the 10mL measuring bottle, add 20% acetonitrile and be settled to scale, shake up, filter, get subsequent filtrate and get final product;
(2) preparation of reference substance solution: it is appropriate that precision takes mono-ammonium glycyrrhizinate reference substance, liquiritin reference substance and isoliquiritin reference substance, add methyl alcohol and make respectively the solution that every 1mL contains mono-ammonium glycyrrhizinate reference substance 0.154mg, liquiritin reference substance 0.587mg and isoliquiritin reference substance 0.362mg, and get final product;
(3) chromatographic condition and system suitability: be the Agilent TC-C of filling agent with octadecyl silane
18Chromatographic column; Take 0.2 ‰ formic acid water as mobile phase A, take acetonitrile as Mobile phase B, gradient elution: 0 ~ 10min is 5% ~ 10%B, and 10 ~ 61min is 10% ~ 27%B, and 61 ~ 70min is 27% ~ 40%B, and 70 ~ 90min is 40% ~ 50%B; Flow velocity 1.0mL/min; 30 ℃ of column temperatures; The DAD detecting device detects under wavelength 254nm, 279nm and 362 nm simultaneously; Sample size 10 μ L; Theoretical cam curve is calculated, and should be not less than 3000;
(4) all the period of time multi-wavelength fusion: adopt the multi-wavelength fusion fingerprint pattern technology that the spectral data under 254nm, 279nm and three wavelength of 362 nm is carried out all the period of time and merge, obtain a chromatogram that can comprise simultaneously three wavelength information.
(5) sample size is measured: use the finger-print data after merging, the content of index components in 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 method for building up of licorice medicinal materials all the period of time multi-wavelength fusion finger-print of the present invention, the preparation of preferred need testing solution: the extracting Radix Glycyrrhizae medicinal powder is 5g approximately, accurately weighed, put in round-bottomed flask, precision adds entry 100mL, weighed weight, added hot reflux 2 hours, let cool, weighed weight again, water is supplied the weight of less loss, shake up, filter, the accurate subsequent filtrate 20mL that draws, be added on the AB-8 resin column, wash with distilled water 120mL, use again the 100mL95% ethanol elution, collect ethanol eluate, evaporate to dryness, residue adds 20% acetonitrile to be made and dissolves and be transferred in the 10mL measuring bottle, add 20% acetonitrile and be settled to scale, shake up, filter, get subsequent filtrate and get final product,
The method for building up of licorice medicinal materials all the period of time multi-wavelength fusion finger-print of the present invention, preferred detection method: be the Agilent TC-C of filling agent with octadecyl silane
18Chromatographic column; Take 0.2 ‰ formic acid water as mobile phase A, take acetonitrile as Mobile phase B, gradient elution: 0 ~ 10min is 5% ~ 10%B, and 10 ~ 61min is 10% ~ 27%B, and 61 ~ 70min is 27% ~ 40%B, and 70 ~ 90min is 40% ~ 50%B; Flow velocity 1.0mL/min; 30 ℃ of column temperatures; The DAD detecting device detects under wavelength 254nm, 279nm and 362 nm simultaneously; Sample size 10 μ L; Theoretical cam curve is calculated, and should be not less than 3000;
The method for building up of Radix Glycyrrhizae all the period of time multi-wavelength fusion finger-print of the present invention, obtain spectral data under 254nm, 279nm and three wavelength of 362 nm by analysis and detecting instrument, exploit information is processed the spectral data under three wavelength of means all the period of time fusion, obtains a chromatogram that can comprise simultaneously three wavelength information.
The method for building up of licorice medicinal materials all the period of time multi-wavelength fusion finger-print of the present invention will can obtain one group of spectral data after the spectral data all the period of time fusion under 254nm, 279nm and three wavelength of 362nm.
The method for building up of licorice medicinal materials all the period of time multi-wavelength fusion finger-print of the present invention, the finger-print data that obtain can be used for the fingerprint qualitative analysis of licorice medicinal materials.
The method for building up of licorice medicinal materials all the period of time multi-wavelength fusion finger-print of the present invention, the finger-print data that obtain can be used for the quantitative test of licorice medicinal materials index components.
The method for building up of licorice medicinal materials all the period of time multi-wavelength fusion finger-print of the present invention is compared with the assay method of existing Chinese Pharmacopoeia regulation the good effect that has and is:
(1) the present invention is open by setting up licorice medicinal materials all the period of time multi-wavelength fusion finger-print and its index components being carried out the method for assay first, the method is to same sample heterogeneity multi-wavelength qualitative and quantitative analysis simultaneously, thus the perfect method for building up of licorice medicinal materials all the period of time multi-wavelength fusion finger-print.
(2) the present invention adopts modern advanced analysis detection technique, and a plurality of index components of licorice medicinal materials are carried out analyzing and testing, thereby obtains extremely abundant quantity of information.
(3) the present invention carries out all the period of time fusion by information processing means with the chromatogram under the licorice medicinal materials multi-wavelength, under the prerequisite that guarantees the data message loss reduction, obtains the chromatogram of a plurality of wavelength information of simultaneous reactions.
(4) method for building up of quality all the period of time multi-wavelength fusion finger-print of the present invention, its advantage is simple to operate, and is reliable and stable, precision, repeatability, the recovery all reach the quantitative test requirement, can comprehensively analyze on a macro scale the quality of licorice medicinal materials.
(5) the present invention is by setting up licorice medicinal materials all the period of time multi-wavelength fusion finger-print, each constituents in licorice medicinal materials is carried out the fingerprint qualitative and quantitative analysis, disclose truly the inherent quality feature of licorice medicinal materials comprehensively, thereby guaranteed the safe, effective, reliable, stable of licorice medicinal materials, guaranteed the equalization stable of its quality and the standardization of technique.
Description of drawings
Fig. 1 is reference substance liquiritin under the 254nm wavelength, isoliquiritin, mono-ammonium glycyrrhizinate chromatogram.
Fig. 2 is reference substance liquiritin under the 279nm wavelength, isoliquiritin, mono-ammonium glycyrrhizinate chromatogram.
Fig. 3 is reference substance liquiritin under the 362nm wavelength, isoliquiritin, mono-ammonium glycyrrhizinate chromatogram.
Fig. 4 is the UV scanning figure of liquiritin.
Fig. 5 is the UV scanning figure of isoliquiritin.
Fig. 6 is the UV scanning figure of mono-ammonium glycyrrhizinate.
Fig. 7 is HPLC finger-print under licorice medicinal materials 254nm wavelength.
Fig. 8 is HPLC finger-print under licorice medicinal materials 279nm wavelength.
Fig. 9 is HPLC finger-print under licorice medicinal materials 362nm wavelength.
Figure 10 is the chromatogram of licorice medicinal materials all the period of time multi-wavelength fusion and merges the peak.
Claims (1)
1. the method for building up of licorice medicinal materials all the period of time multi-wavelength fusion finger-print is characterized in that the method carries out as follows:
(1) preparation of need testing solution: the extracting Radix Glycyrrhizae medicinal powder is 5g approximately, and is accurately weighed, puts in round-bottomed flask, precision adds entry 100mL, and weighed weight added hot reflux 2 hours, let cool, weighed weight again, water is supplied the weight of less loss, shakes up, filter, the accurate subsequent filtrate 20mL that draws is added on the AB-8 resin column, with distilled water 120mL washing, use again the 100mL95% ethanol elution, collect ethanol eluate, evaporate to dryness, residue add 20% acetonitrile to be made and dissolves and be transferred in the 10mL measuring bottle, add 20% acetonitrile and be settled to scale, shake up, filter, get subsequent filtrate and get final product;
(2) preparation of reference substance solution: it is appropriate that precision takes mono-ammonium glycyrrhizinate reference substance, liquiritin reference substance and isoliquiritin reference substance, add methyl alcohol and make respectively the solution that every 1mL contains mono-ammonium glycyrrhizinate reference substance 0.154mg, liquiritin reference substance 0.587mg and isoliquiritin reference substance 0.362mg, and get final product;
(3) chromatographic condition and system suitability: be filling agent Agilent TC-C with octadecyl silane
18Chromatographic column; Take 0.2 ‰ formic acid water as mobile phase A, take acetonitrile as Mobile phase B, gradient elution: 0 ~ 10min is 5% ~ 10%B, and 10 ~ 61min is 10% ~ 27%B, and 61 ~ 70min is 27% ~ 40%B, and 70 ~ 90min is 40% ~ 50%B; Flow velocity 1.0mL/min; 30 ℃ of column temperatures; The DAD detecting device detects under wavelength 254nm, 279nm and 362 nm simultaneously; Sample size 10 μ L; Theoretical cam curve is calculated, and should be not less than 3000;
(4) all the period of time multi-wavelength fusion: adopt the multi-wavelength fusion fingerprint pattern technology that the spectral data under 254nm, 279nm and three wavelength of 362 nm is carried out all the period of time and merge, obtain a chromatogram that can comprise simultaneously three wavelength information;
(5) sample size is measured: use the finger-print data after merging, the content of index components in calculation sample;
(6) above-mentioned definite content assaying method is carried out efficiency evaluation, comprising specificity, accuracy, precision, repeatability, stability, linearity, scope and durability.
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| CN102539576A (en) * | 2012-01-30 | 2012-07-04 | 辽宁中医药大学 | Control method for simultaneously detecting content of nine components through five wavelength merging method for licorice medicinal materials |
| CN102680628B (en) * | 2012-05-18 | 2015-01-14 | 新疆全安药业有限公司 | Method for establishing fingerprint of An Weiyang |
| CN102680629B (en) * | 2012-05-18 | 2014-08-06 | 新疆全安药业有限公司 | Method for establishing Anweiyang capsule fingerprint spectrum |
| CN102692460A (en) * | 2012-05-22 | 2012-09-26 | 辽宁中医药大学 | Process for determining content of four components of honeysuckle during full-time-interval three-wavelength fusion |
| CN102692461B (en) * | 2012-05-22 | 2013-12-18 | 辽宁中医药大学 | Whole-time three-wavelength fusion method for simultaneously determining contents of four ingredients in Flos Carthami |
| CN102759585B (en) * | 2012-07-02 | 2013-12-04 | 辽宁华润本溪三药有限公司 | Method for controlling full-time interval multi-wavelength fused fingerprint quality of qi stagnation and stomachache granules |
| 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 |
| 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 |
| CN110274970B (en) * | 2018-12-28 | 2021-11-05 | 吉林三九金复康药业有限公司 | Method for establishing melting difference fingerprint spectrum and application of melting difference fingerprint spectrum in quality control of Yixuesheng capsules |
| CN111443154B (en) * | 2020-05-21 | 2023-03-07 | 贵州中医药大学 | Research method of medicinal genetic relationship of glycyrrhiza |
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