CN108169345A - Anaesthetic radix gentiane dahuvicae fingerprint and quality evaluating method - Google Patents
Anaesthetic radix gentiane dahuvicae fingerprint and quality evaluating method Download PDFInfo
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Abstract
The present invention relates to a kind of method for building up of anaesthetic radix gentiane dahuvicae finger-print, including：1) preparation of test solution：Medicinal powder 0.4g is taken, is put in 150mL conical flask with cover, adds 40% methanol 25mL, weighs, ultrasonic extraction after being placed into room temperature, is re-weighed, and the weight of less loss is supplied with solvent, filtration, and filtrate is taken to be filtered with 0.45 μm of micropore, filter membrane；2) chromatographic condition：Chromatographic column：Thermo SCIENTIFIC Hypersil GOLD；Mobile phase：0.1% aqueous formic acid of acetonitrile (A) (containing 0.05% tetrahydrofuran) (B), using gradient elution 95%B (0min)~95%B (5min)~90%B (10min)~87%B (30min)~80%B (50min)~78%B (60min)~75%B (65min)~65%B (90min)；Flow velocity：1.0mL/min；Testing conditions：DAD detectors, Detection wavelength：245nm；Column temperature：25℃；Sample size：20μL.The present invention establishes anaesthetic radix gentiane dahuvicae finger-print using HPLC, provides a kind of method compared with thoroughly evaluating anaesthetic radix gentiane dahuvicae quality of medicinal material.
Description
Technical field
The present invention relates to Pharmaceutical Analysis fields, and in particular to medicinal materials fingerprint method for building up and evaluation of medical materials' quality side
Method.
Background technology
In recent years, growing day by day to the attention degree of ethnic drug both at home and abroad, there is an urgent need to the quality standard progress to drug
Control, to ensure that research medication is more reliable and more stable.Due to understanding insufficient (Ji Yuan, pick and process, the agents area to anaesthetic
Deng), lead to kind confusion in the market, so fully and effectively method of quality control is imperative for foundation, ensure, with to medicine, to make good use of
Medicine.
Radix gentiane dahuvicae is Gentianaceae (Gentianaceae) Gentiana (Gentiana) bark of ash group Da Wuli bark of ash
The dry flower of (Gentiana dahurica Fisch.), be distributed widely in Shaanxi, Gansu, Ningxia, the Inner Mongol, Xinjiang, Shanxi,
The ground such as Hebei are grown on field at, roadside, river shoal, ditch, the ground such as endroit more.Radix gentiane dahuvicae enters anaesthetic, and anaesthetic is entitled to exhale
With-Zhu Ligen-its wooden lattice, there is heat-clearing, removing toxic substances, cough-relieving, eliminating the phlegm, cure mainly cough with lung heat, throat is warm, abscess of throat,
It is scorchingly hot, the diseases such as pest heat.
Radix gentiane dahuvicae be Mongolian medicine's clinic common medicine, record in《Drug Standard of Ministry of Public Health of the Peoples Republic of China》(anaesthetic point
Volume), and microscopical characters and chemical discrimination method are only limitted under quality standard item, the assay of pertinent literature report also only has dragon
The iridoids constituents such as courage hardship glycosides do not ensure that safety and the validity of medication.Fingerprint pattern technology is as crude drug
The method of quality control of object extract and its preparation has reached international consensus, is a kind of identification of means of synthesis, specificity is strong, surely
It is qualitative, reproducible, it can more comprehensively evaluate authenticity, the Optimality of medicinal material.Therefore, the present invention utilizes high performance liquid chromatography
The finger-print of anaesthetic radix gentiane dahuvicae is constructed, and analysis is carried out to the multiple batches of radix gentiane dahuvicae of different sources, the medicinal material is determined
Standard finger-print, establish a kind of reliable and stable anaesthetic radix gentiane dahuvicae method of quality control.
Invention content
The present invention proposes a kind of method for building up of radix gentiane dahuvicae finger-print, includes the following steps：
1) preparation of test solution：Medicinal powder is taken, it is accurately weighed, it puts in 150mL conical flask with cover, precision adds in 0
~100% methanol 25mL, weighs, and 20~60min of ultrasonic extraction after being placed into room temperature, is re-weighed, and the weight of less loss is supplied with solvent
Amount, filtration, takes filtrate to be filtered with 0.45 μm of miillpore filter, spare；
2) test solution is injected in high performance liquid chromatograph, the chromatographic condition that uses for：Chromatographic column：Octadecyl silicon
Alkane bonded silica gel chromatographic column；Mobile phase is selected from methanol-water, acetonitrile-water, acetonitrile-phosphoric acid water, acetonitrile-formic acid water, acetonitrile-formic acid
One kind in tetrahydrofuran aqueous solution, wherein the most preferably aqueous solution of -0.1% formic acid of acetonitrile (A) and 0.05% tetrahydrofuran
(B)；Gradient：95%B (0min)~95%B (5min)~90%B (10min)~87%B (30min)~80%B
(50min)~78%B (60min)~75%B (65min)~65%B (90min)；Testing conditions：DAD detectors, Detection wavelength
230~400nm；Column temperature：20~35 DEG C；Sample size：10~20 μ L.
Preferably, chromatographic column uses specification as 250mm × 4.6mm, 5 μm
Thermo SCIENTIFIC Hypersil GOLD、Hypersil ODS2、KromasilTM C18And Agilent
Eclipse Plus C18Chromatographic column.
It is further to be preferably, in step 1), medicinal powder about 0.4g is taken, accurately weighed, 40% methanol 25mL of addition surpasses
Sound extracts 30min, after being placed into room temperature, is re-weighed, the weight of less loss is supplied with solvent, filters, takes filtrate with 0.45 μm of micropore
Filter membrane filters.
It is highly preferred that flow velocity is 1.0mL/min；Using DAD detectors, Detection wavelength 245nm；25 DEG C of column temperature；Sample size
20μL。
The present invention also provides a kind of method using finger-print evaluation radix gentiane dahuvicae quality of medicinal material, including the following contents：
Finger-print is established, including：A) preparation of test solution：The radix gentiane dahuvicae style product test sample of 10 different batches is prepared respectively
Solution takes medicinal powder (No. 4 sieves) 0.1~0.4g, accurately weighed, puts in 150mL conical flask with cover, precision adds in 0~100%
Methanol 25mL, weighs, and 20~60min of ultrasonic extraction after being placed into room temperature, is re-weighed, and the weight of less loss is supplied with solvent, filter
It crosses, filtrate is taken to be filtered with 0.45 μm of miillpore filter, it is spare；B) preparation of reference substance solution：Weigh 1) 5- hydroxyls -2- pyridine carboxylics
Acid, 2) 5- hydroxyls furfural, 3) 2- furancarboxylic acids, 4) loganin, 5) m-hydroxybenzoic acid, 6) gentiamarin, 7) cyanidenon -6-C- β -
D-Glucose -7-O- β-D-Glucose glycosides, 8) sweroside, 9) apiolin -6-C- β-D-Glucose -7-O- β-D-Glucose
The totally 11 kinds of controls of glycosides, 10) cyanidenon -6-C- β-D- glucopyranosides, 11) apiolin -6-C- β-D- glucopyranosides
Product dissolve constant volume with methanol, and certain density single contrast solution is made, and 0.45 μm of filtration of miillpore filter is spare；C) successively will
In each test solution and reference substance solution injection high performance liquid chromatograph, chromatographic condition is：Chromatographic column：Octadecylsilane key
Close silica gel chromatographic column；Chromatographic condition：Mobile phase：Methanol-water, acetonitrile-water, acetonitrile-phosphoric acid water, acetonitrile-formic acid water, acetonitrile-first
Sour water (contains tetrahydrofuran), using gradient elution 95%B (0min)~65%B (90min)；Testing conditions：DAD detectors, inspection
Survey 230~400nm of wavelength；Column temperature：20~35 DEG C；Flow velocity：0.8~1.2mL/min；Sample size：10~20 μ L；D) 10 batches are utilized
Secondary sample establishes finger-print, and calculates its similarity with similarity evaluation software.
Further, the finger-print includes following 19 shared peaks, and the retention time at each peak is respectively：4.00
8.20,10.46,11.76,12.00,12.69,14.79,18.52,19.93,22.04,22.62,23.40,23.89,25.64,
30.61,32.40,41.32,54.25,58.33.
Further, wherein, the relative peak area at 19 shared peaks is respectively 2.929,0.177,5.354,
0.122,0.189,0.438,1.000,1.791,0.822,0.401,0.578,0.161,0.280,0.534,0.306,
0.902,0.692,0.414,0.678.
The present invention establishes anaesthetic radix gentiane dahuvicae HPLC finger-prints for the first time, identifies 11 peaks in 19 shared peaks.
This method is easy to operate, and separating degree is high, favorable reproducibility, and the true and false quality for fully and effectively reflection radix gentiane dahuvicae anther material provides one kind
Technical support can comprehensively and effectively reflect radix gentiane dahuvicae quality of medicinal material, and foundation is provided for the control of radix gentiane dahuvicae quality of medicinal material.
Description of the drawings
Fig. 1 is the finger-print obtained according to the method for the present invention；
What Fig. 2 showed 11 single reference substances and finger-print compares collection of illustrative plates；
Fig. 3 is 10 crowdes of radix gentiane dahuvicae Herbal HPLC Fingerprint stacking charts.
Specific embodiment
The preparation of test solution
The dry radix gentiane dahuvicae to constant weight is taken, crush and crosses No. 4 sieves, takes sieving powder, precision adds in the methanol of calculation amount
Solution is ultrasonically treated, places to room temperature, and solvent supplies weightlessness, shakes up, and filtration takes subsequent filtrate, crosses 0.45 μm of miillpore filter, makees
For test solution.
In the present invention, using methanol aqueous solution as test sample solvent, preferably the concentration range of methanol solution 30~
Between 50%, most preferably 40% methanol solution；Extracting method is reflux or ultrasonic extraction, preferably ultrasonic extraction, is carried
20~60min of time is taken, preferably extracts 30min；Sampling amount can be in the range of 0.1~0.4g, final preferred sampling 0.4g.
Therefore, the preparation method of the most preferred radix gentiane dahuvicae test solution of the present invention is：Medicinal powder about 0.4g is taken, essence
It is close weighed, it puts in 150mL conical flask with cover, precision adds in 40% methanol 25mL, ultrasonic extraction 30min, after being placed into room temperature, then
Weigh, the weight of less loss supplied with solvent, filter, take filtrate with the filtration of 0.45 μm of miillpore filter to get.The preparation method is in color
Peak number, peak height, peak area and the separating degree aspect of spectrogram are put up the best performance.
The preparation of reference substance solution
Precision weighs each reference substance, and methanol is added to dissolve and is diluted to scale, is shaken up, a certain concentration reference substance solution is made,
It is filtered before sample introduction with 0.45 μm of miillpore filter.Reference substance is that its knot is obtained and identified in radix gentiane dahuvicae chemical constitution study
Structure, following 11 kinds：
1) 5- hydroxyls -2-Pyridinecarboxylic Acid
2) 5- hydroxyls furfural
3) 2- furancarboxylic acids
4) loganin
5) m-hydroxybenzoic acid
6) gentiamarin
7) cyanidenon -6-C- β-D-Glucose -7-O- β-D-Glucose glycosides
8) sweroside
9) apiolin -6-C- β-D-Glucose -7-O- β-D-Glucose glycosides
10) cyanidenon -6-C- β-D- glucopyranosides
11) apiolin -6-C- β-D- glucopyranosides
Chromatographic condition
The chromatographic condition used in the present invention is preferably：Chromatographic column：Octadecylsilane chemically bonded silica chromatographic column；Mobile phase
It can be selected from one in methanol-water, acetonitrile-water, acetonitrile-phosphoric acid water, acetonitrile-formic acid water, acetonitrile-formic acid tetrahydrofuran aqueous solution
Kind, using gradient elution 95%B (0min)~65%B (90min)；Testing conditions：DAD detectors, Detection wavelength 230~
400nm；Column temperature：20~35 DEG C；Flow velocity：0.8~1.2mL/min；Sample size：10~20 μ L；
Present invention determine that the optimal chromatographic condition of radix gentiane dahuvicae HPLC fingerprint map analyzings is：Chromatographic column：Thermo
SCIENTIFIC Hypersil GOLD；Mobile phase：- 0.1% aqueous formic acid of acetonitrile (A) (containing 0.05% tetrahydrofuran) (B),
Using gradient elution 95%B (0min)~95%B (5min)~90%B (10min)~87%B (30min)~80%B
(50min)~78%B (60min)~75%B (65min)~65%B (90min)；Flow velocity：1.0mL/min；Detection wavelength
245nm；25 DEG C of column temperature；20 μ L of sample size.Using the chromatographic column, flow phase system and elution ratio, peak shape and separating degree are good, peak
Number is more, and flow velocity, column temperature and sample size are also adjusted such index；Detection wavelength uses 245nm to determine best peak height
And peak area.Protrusion is needed, selection contains 0.1% formic acid and 0.05% tetrahydrofuran to the present invention in a preferred embodiment
Aqueous solution as Mobile phase B solvent, can clearly pull open each peak.And use other mobile phases, then analytical effect
It is poor.
The calibration at shared peak
Different sources and 10 batches of radix gentiane dahuvicae anther materials of time acquisition are collected, according to the above-mentioned operating method having built up point
Sample introduction is analyzed, obtains the HPLC finger-prints of medicinal material, and determine 19 shared peaks, forms common pattern.Wherein No. 7 peaks (S)
For with reference to peak, relative retention time and relative peak area are 1.000, other peaks calculate in contrast relative retention time and
Relative peak area is shown in Table 1.
The relative retention time and relative peak area at peak are shared in 1 radix gentiane dahuvicae finger-print of table
The foundation of standard finger-print
Above-mentioned 10 parts of sample collection of illustrative plates of acquisition are imported in similarity evaluation software, similarity is calculated with average method, therefrom
The finger-print of a similarity maximum is selected as standard finger-print (Fig. 1).Reference substance is compared with standard finger-print, knot
Fruit such as Fig. 2 identifies 1,2,4,7,10,11,12,13,15,16, No. 17 peak.
Using aforementioned most preferably condition, finger-print is obtained, it includes 19 shared peaks, retention time and opposite peak face
Product is respectively：4.00 2.929；8.20 0.177；10.46 5.354；11.76 0.122；12.00 0.189；12.69,
0.438；14.79 1.000；18.52 1.791；19.93 0.822；22.04 0.401；22.62 0.578；23.40,
0.161；23.89 0.280；25.64 0.534；30.61 0.306；32.40 0.902；41.32 0.692；54.25,
0.414；58.33 0.678.The reference substance solution prepared is identified with the same terms sample introduction in 19 shared peaks simultaneously
11, this 11 peaks are corresponding with peak number in finger-print as follows：
No. 1 5- hydroxyls -2-Pyridinecarboxylic Acid
No. 2 5- hydroxyl furfurals
No. 4 2- furancarboxylic acids
No. 7 loganins
No. 10 m-hydroxybenzoic acids
No. 11 gentiamarins
No. 12 cyanidenon -6-C- β-D-Glucose -7-O- β-D-Glucose glycosides
No. 13 swerosides
No. 15 apiolin -6-C- β-D-Glucose -7-O- β-D-Glucose glycosides
No. 16 cyanidenon -6-C- β-D- glucopyranosides
No. 17 apiolin -6-C- β-D- glucopyranosides
The 10 batches of radix gentiane dahuvicae anther material information in this invention
2 10 batches of radix gentiane dahuvicae anther materials of table
Radix gentiane dahuvicae evaluation of medical materials' quality
The evaluation software that the present invention uses is the chromatographic fingerprints of Chinese materia medica similarity evaluation that Chinese Pharmacopoeia Commission is recommended
System (2004A editions), using the condition that above-mentioned finger-print is established by sample to be evaluated and established standard finger-print into
Row compares, and is evaluated with similarity evaluation software, and similarity meets the requirements more than 0.90.
Methodology validation
The investigation of precision
S8 samples are prepared according to the preparation method of test solution, sample introduction is repeated 6 times with determining optimal chromatographic condition, is surveyed
Each shared peak relative retention time and relative peak area RSD values respectively 0.01~0.18% and 0.46~2.87% it
Between, show that instrument precision is good, meet the technology requirement of finger-print, be shown in Table 3.Study on the stability
S8 samples are prepared according to the preparation method of determining test solution, are existed respectively with determining optimal chromatographic condition
0th, 2,4,6,8,10, sample introduction is analyzed by 12h, measures the relative retention time at each shared peak and the RSD values of relative peak area 0.01
Between~0.22% and 0.64~2.94%, show that test solution is good in 12h internal stabilities, be shown in Table 4.
Repetitive test
6 parts of S8 samples are prepared according to the preparation method of determining test solution is parallel, with aforementioned determining optimal color
Sample introduction is analyzed respectively for spectral condition, measure the relative retention time at each shared peak and the RSD values of relative peak area 0.02~
Between 0.33% and 0.73~2.89%, show that this method repeatability is good, be shown in Table 5.
10 batches of radix gentiane dahuvicae style product similarity evaluations
10 batches of radix gentiane dahuvicae anther timber-used methods same as before obtain the HPLC collection of illustrative plates of each batch of medicinal material, utilize " Chinese medicine chromatography
19 shared peaks in each chromatogram are analyzed and evaluated in fingerprint similarity evaluation system (2004A editions) ", with average
Method calculates similarity, obtains the similar degrees of data (table 6) of 10 batches of medicinal materials, and each batch sample HPLC collection of illustrative plates stacking charts see Fig. 3.
Claims (10)
1. a kind of method for building up of anaesthetic radix gentiane dahuvicae finger-print, includes the following steps：
1) preparation of test solution：Medicinal powder is taken, it is accurately weighed, it puts in 150mL conical flask with cover, precision addition 0~
100% methanol 25mL, weighs, and 20~60min of ultrasonic extraction after being placed into room temperature, is re-weighed, and the weight of less loss is supplied with solvent
Amount, filtration, takes filtrate to be filtered with 0.45 μm of miillpore filter, spare；
2) chromatographic condition：Chromatographic column：Octadecylsilane chemically bonded silica chromatographic column；
Mobile phase：It is water-soluble selected from methanol-water, acetonitrile-water, acetonitrile-phosphoric acid water, acetonitrile-formic acid water, acetonitrile-formic acid tetrahydrofuran
One kind in liquid, using gradient elution 95%B (0min)~65%B (90min)；Testing conditions：DAD detectors, Detection wavelength
230~400nm；Column temperature：20~35 DEG C；Flow velocity：0.8~1.2mL/min；Sample size：10~20 μ L.
2. processing method described in claim 1, wherein, chromatographic column uses specification as 250mm × 4.6mm, 5 μm of Thermo
SCIENTIFIC Hypersil GOLD、Hypersil ODS2、KromasilTM C18With Agilent Eclipse Plus C18
Chromatographic column.
3. processing method described in claim 1, wherein, in step 1), medicinal powder about 0.4g is taken, accurately weighed, precision adds
Enter 40% methanol 25mL, weigh, ultrasonic extraction 30min after being placed into room temperature, is re-weighed, and the weight of less loss is supplied with solvent, filter
It crosses, filtrate is taken to be filtered with 0.45 μm of miillpore filter.
4. processing method described in claim 1, wherein, mobile phase：Acetonitrile (A) 0.05% tetrahydrofuran of -0.1% formic acid is water-soluble
Liquid (B)；Gradient：95%B (0min)~95%B (5min)~90%B (10min)~87%B (30min)~80%B
(50min)~78%B (60min)~75%B (65min)~65%B (90min)；Flow velocity is 1.0mL/min；It is detected using DAD
Device, Detection wavelength 245nm；25 DEG C of column temperature；20 μ L of sample size.
5. a kind of method using finger-print evaluation radix gentiane dahuvicae quality of medicinal material includes the following steps：
Standard finger-print is established, including：A) preparation of test solution：The radix gentiane dahuvicae style of 10 different batches is prepared respectively
Product test solution takes sample powder, accurately weighed, puts in 150mL conical flask with cover, and precision adds in 0~100% methanol
25mL weighs, and 20~60min of ultrasonic extraction after being placed into room temperature, is re-weighed, and the weight of less loss is supplied with solvent, and filtration takes
Filtrate is filtered with 0.45 μm of miillpore filter, spare；B) preparation of reference substance solution：Weigh 1) 5- hydroxyls -2-Pyridinecarboxylic Acid, 2) 5-
Hydroxyl furfural, 3) 2- furancarboxylic acids, 4) loganin, 5) m-hydroxybenzoic acid, 6) gentiamarin, 7) cyanidenon -6-C- β-D- grapes
Sugar -7-O- β-D-Glucose glycosides, 8) sweroside, 9) apiolin -6-C- β-D-Glucose -7-O- β-D-Glucose glycosides, 10) wood
Rhinoceros grass element -6-C- β-D- glucopyranosides, 11) apiolin -6-C- β-D- glucopyranosides totally 11 kinds of reference substances, use methanol
Constant volume is dissolved, certain density single contrast solution is made, 0.45 μm of filtration of miillpore filter is spare；C) chromatographic condition：Chromatography
Column：Octadecylsilane chemically bonded silica chromatographic column；Mobile phase：Methanol-water, acetonitrile-water, acetonitrile-phosphoric acid water, acetonitrile-formic acid water,
Acetonitrile-formic acid-tetrahydrofuran aqueous solution, using gradient elution 95%B (0min)~65%B (90min)；Testing conditions：DAD is examined
Survey device, 230~400nm of Detection wavelength；Column temperature：20~35 DEG C；Flow velocity：0.8~1.2mL/min；Sample size：10~20 μ L；d)
The similarity of 10 samples is calculated with similarity evaluation software, therefrom determines that a similarity is highest and is used as standard fingerprint figure
Spectrum；
The finger-print of a sample to be evaluated is obtained with above-mentioned identical mode；
The similarity of sample finger-print to be evaluated and the standard finger-print described in aforementioned similarity evaluation software evaluation,
Similarity judges that the sample quality to be evaluated meets the requirements more than 0.9.
6. the processing method described in claim 5, wherein, chromatographic column uses specification as 250mm × 4.6mm, 5 μm of Thermo
SCIENTIFIC Hypersil GOLD、Hypersil ODS2、KromasilTMC18、Agilent Eclipse Plus C18Color
Compose column.
7. the processing method described in claim 5, wherein, in step 1), medicinal powder about 0.4g is taken, accurately weighed, precision adds
Enter 40% methanol 25mL, weigh, ultrasonic extraction 30min after being placed into room temperature, is re-weighed, and the weight of less loss is supplied with solvent, filter
It crosses, filtrate is taken to be filtered with 0.45 μm of miillpore filter.
8. the processing method described in claim 5, wherein, mobile phase：Acetonitrile (A) 0.05% tetrahydrofuran of -0.1% formic acid is water-soluble
Liquid (B)；Gradient：95%B (0min)~95%B (5min)~90%B (10min)~87%B (30min)~80%B
(50min)~78%B (60min)~75%B (65min)~65%B (90min)；Flow velocity is 1.0mL/min；It is detected using DAD
Device, Detection wavelength 245nm；25 DEG C of column temperature；20 μ L of sample size.
9. method according to any one of claims 8, wherein, finger-print includes 19 shared peaks, and the retention time at each peak is respectively：
4.00,8.20,10.46,11.76,12.00,12.69,14.79,18.52,19.93,22.04,22.62,23.40,23.89,
25.64,30.61,32.40,41.32,54.25,58.33.
10. the method described in claim 9, wherein, the relative peak area at 19 shared peaks is respectively 2.929,0.177,
5.354,0.122,0.189,0.438,1.000,1.791,0.822,0.401,0.578,0.161,0.280,0.534,
0.306,0.902,0.692,0.414,0.678.
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Cited By (3)
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| CN113588648A (en) * | 2021-09-01 | 2021-11-02 | 石河子大学 | Quality detection method of gentiana macrophylla Huameng medicinal material |
| CN114002366A (en) * | 2020-07-27 | 2022-02-01 | 京津冀联创药物研究（北京）有限公司 | Large gentiana root decoction standard water extract, preparation and quality control evaluation method thereof |
| CN114184700B (en) * | 2021-12-06 | 2023-08-22 | 内蒙古民族大学 | Method for measuring chemical component content of Mongolian medicine costa |
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| CN113588648B (en) * | 2021-09-01 | 2024-01-02 | 石河子大学 | Quality detection method for gentiana macrophylla flower Mongolian medicinal material |
| CN114184700B (en) * | 2021-12-06 | 2023-08-22 | 内蒙古民族大学 | Method for measuring chemical component content of Mongolian medicine costa |
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