CN109633001A - The fingerprint atlas detection method of the wine fruit of glossy privet - Google Patents
The fingerprint atlas detection method of the wine fruit of glossy privet Download PDFInfo
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- G—PHYSICS
- G01—MEASURING; TESTING
- G01N—INVESTIGATING OR ANALYSING MATERIALS BY DETERMINING THEIR CHEMICAL OR PHYSICAL PROPERTIES
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Abstract
The invention discloses the detection method of wine fruit of glossy privet finger-print, wine fruit of glossy privet finger-print establishes the preparation the following steps are included: step 1, test solution；The preparation of step 2, mixed reference substance solution: step 3, accurate test solution of drawing injects liquid chromatograph respectively, records chromatogram；Step 4, the wine fruit of glossy privet finger-print instrument obtained in step 3 is exported, and imports similarity evaluation, select in the chromatogram of the different batches wine fruit of glossy privet existing for chromatographic peak as shared peak；The reference fingerprint of the wine fruit of glossy privet is generated with mean value calculation method；Calculate relative retention time, the relative peak area at each shared peak.Wine fruit of glossy privet finger-print provided by the present invention objectively can characterize the quality of the wine fruit of glossy privet comprehensively.The detection method of finger-print provided by the invention has method simplicity, stablizes, precision height, high repeatability and other advantages.
Description
Technical field
The invention belongs to Chinese medicine detection technique fields, specifically, being related to a kind of finger-print detection side of wine fruit of glossy privet
Method.
Background technique
The fruit of glossy privet is the dry mature fruit of Oleaceae plants glossy privet Ligustrum lucidum Ait..Its property is sweet, bitter,
It is cool.Return liver and kidney channel.There is the effect of nourishing liver and kidney, improving eyesight black hair.For the deficiency of liver-yin and kidney-yin, dizziness and tinnitus, soreness and weakness of waist and knees, beard and hair morning
White, mesh is secretly unknown, Heat Diabetes, osteopyrexia and fever.Wine steams the conventional concocting method that method is the fruit of glossy privet, and Glossy Privet Fruit Wine product nourishes liver
Kidney acts on more preferably compared with health product.
With the extensive use of Chinese medicine, validity, safety issue are attracted wide attention, and establish the quality of high-quality
Standard is a difficult task for a long time with the quality for guaranteeing medicinal material.Currently, the method for traditional Chinese medicine quality control is only to wherein few
Number analyzed by principal component, can not embody the globality feature of traditional Chinese medicine, it is necessary to which the new method for developing traditional Chinese medicine quality control is built
The new system of vertical modern mass control standard, traditional Chinese medicine fingerprint technology are come into being.Traditional Chinese medicine fingerprint can analyze Chinese medicine
The information of the type of middle effective component and invalid components and the distribution of its amount, the characteristics of meeting traditional Chinese medicine globality and ambiguity.
In the existing correlation drug standards, only there is assay to this single component of Specnuezhenide in wine fruit of glossy privet medicine materical crude slice,
Therefore establishing a kind of wine fruit of glossy privet finger-print using high performance liquid chromatography has the quality for accurately controlling the wine fruit of glossy privet
Significance.
Summary of the invention
Goal of the invention: the purpose of the present invention is overcome the deficiencies in the prior art, develop a kind of finger-print of wine fruit of glossy privet
Detection method can guarantee the quality stability, consistency and controllability of the wine fruit of glossy privet by means of the present invention, so that it is guaranteed that
The safety and validity of the wine fruit of glossy privet.
Technical solution: in order to achieve the above object, the technical solution adopted by the present invention are as follows:
A kind of fingerprint atlas detection method of the wine fruit of glossy privet, comprising the following steps:
The preparation of step 1, wine fruit of glossy privet test solution:
It is stand-by to weigh wine fruit of glossy privet medicine materical crude slice, beats powder, weighs powder and be placed in stuffed conical flask, methanol, weighing, ultrasound is added
Supply weightlessness after processing, supernatant taken to be filtered after centrifugation with 0.45 μm of organic miillpore filter, take subsequent filtrate to get；
The preparation of step 2, reference substance solution:
Take Specnuezhenide, rhodioside, tyrosol, galuteolin, rutin and acteoside reference substance appropriate respectively, it is accurate
It is weighed, it is respectively placed in volumetric flask, methanol is added to be made into reference substance stock solution respectively；Then the accurate Specnuezhenide, red drawn respectively
Red-spotted stonecrop glycosides, tyrosol, galuteolin, the reference substance solution of rutin and acteoside are appropriate, add methanol constant volume to 20ml, spy is made
Ligustrum lucidum Ait, rhodioside, tyrosol, galuteolin, rutin and acteoside mixed reference substance solution；
Step 3, the respectively accurate wine fruit of glossy privet test solution of aspiration step 1 and the mixed reference substance solution of step 2, note
Enter high performance liquid chromatograph, records chromatogram；
Step 4, the finger-print of the wine fruit of glossy privet test solution obtained in step 3 is exported, and imports Chinese medicine chromatography
Fingerprint similarity evaluation system 2004A；Select in the chromatogram of the different batches wine fruit of glossy privet existing chromatographic peak as
Shared peak；The reference fingerprint of the wine fruit of glossy privet is generated with mean value calculation method, calculate each shared peak relative retention time and
Relative peak area；And according to the retention time of mixed reference substance solution chromatogram mark reference fingerprint in peak chemistry at
Point.
Preferably, the fingerprint atlas detection method of above-described a kind of wine fruit of glossy privet, which is characterized in that
Step 1, wine fruit of glossy privet test solution the preparation method comprises the following steps:
It takes wine fruit of glossy privet medicine materical crude slice stand-by, beats powder, precision weighed the powder 1.0g of No. 4 sieves (65 mesh), was placed in tool plug taper
In bottle, methanol 25ml is added in precision, and weighed quality, ultrasonic extraction 30min is placed at room temperature for, then weighed quality, supplies mistake with methanol
Weight, 12000r/min are centrifuged 3min, take supernatant, cross 0.45 μm of organic miillpore filter to get.
Preferably, the fingerprint atlas detection method of above-described a kind of wine fruit of glossy privet, step 2, mixing control
The preparation of product solution: take Specnuezhenide, rhodioside, tyrosol, galuteolin, rutin and acteoside reference substance suitable respectively
Amount, it is accurately weighed, it is placed in 10ml volumetric flask, adding methanol to be made into concentration is respectively the Specnuezhenide of 290 μ g/ml, 117 μ g/ml
Rhodioside, the tyrosol of 143 μ g/ml, the galuteolin of 285 μ g/ml, the rutin of 276 μ g/ml, 540 μ g/ml feltwort
The reference substance stock solution of glucosides；Accurate Specnuezhenide, rhodioside, tyrosol, galuteolin, rutin and acteoside pair respectively
It is appropriate according to product solution, add methanol constant volume to 20ml, every 1ml is made containing 14.5 μ g of Specnuezhenide, 6.8 μ g of rhodioside, tyrosol 7.2
The mixed reference substance solution of μ g, 14.2 μ g of galuteolin, 13.8 μ g of rutin, 27.0 μ g of acteoside.
Preferably, the fingerprint atlas detection method of above-described a kind of wine fruit of glossy privet, step 3, efficient liquid phase
The chromatographic condition of chromatograph detection are as follows: using octadecylsilane chemically bonded silica as filler, using 0.1% phosphoric acid water as mobile phase
A, using acetonitrile as Mobile phase B, gradient elution, flow velocity be 0.5~1.5mlmin-1,25~40 DEG C of column temperature, Detection wavelength 200~
360nm；
Preferably, a kind of fingerprint atlas detection method of above-described wine fruit of glossy privet, which is characterized in that step
The chromatographic condition of 3 high performance liquid chromatographs detection are as follows: using octadecylsilane chemically bonded silica as filler, to contain 0.1% phosphoric acid
Water is as mobile phase A, using acetonitrile as Mobile phase B, gradient elution, and flow velocity 0.8mlmin-1,30 DEG C of column temperature, Detection wavelength
254nm。
Preferably, a kind of fingerprint atlas detection method of above-described wine fruit of glossy privet, which is characterized in that gradient
Elution is preferably as follows:
| Time/min | Mobile phase A percent by volume | Mobile phase B percent by volume |
| 0 | 95 | 5 |
| 20 | 88 | 12 |
| 40 | 83 | 17 |
| 55 | 77 | 23 |
| 95 | 67 | 33 |
| 105 | 0 | 100 |
Preferably, the fingerprint atlas detection method of above-described a kind of wine fruit of glossy privet, chromatographic column is chromatographic column
For Purospher STAR LP RP-18endcapped, 4.6*250mm, 5 μm.
Preferably, the fingerprint atlas detection method of above-described a kind of wine fruit of glossy privet, the obtained wine fruit of glossy privet
There are 10 shared peaks in finger-print, the retention time that the retention time at each shared peak is respectively as follows: shared peak 1 is 25.385min；
The retention time at shared peak 2 is 27.623min；The retention time at shared peak 3 is 37.849min；The retention time at shared peak 4 is
48.670min；The retention time at shared peak 5 is 57.478min；The retention time at shared peak 6 is 58.276min；Shared peak 7
Retention time is 59.004min；The retention time at shared peak 8 is 61.698min；The retention time at shared peak 9 is
80.021min；The retention time at shared peak 10 is 85.180min.
Wherein, No. 1 peak is rhodioside, and No. 2 peaks are tyrosol, and No. 5 peaks are rutin, and No. 6 peaks are galuteolin, and No. 7 peaks are
Acteoside, No. 8 peaks are Specnuezhenide.
The optimization of finger-print testing conditions is tested:
(1) selection of different mobile phases:
The present invention has screened pure water-acetonitrile, pure water-methanol, 0.1% phosphoric acid water-acetonitrile, 0.1% phosphorus by many experiments
Sour water-methanol, 0.1% glacial acetic acid water-flow phase systems such as acetonitrile and 0.1% glacial acetic acid water-methanol are detected, testing result
Display select water containing 0.1% volume phosphoric acid and acetonitrile as mobile phase, system baseline steadily, peak shape, each peak separating degree situation
It is best.Therefore select using the water containing 0.1% phosphoric acid volume as mobile phase A, it take Mobile phase B as optimal flow phase of acetonitrile；True
On the basis of determining mobile phase, in order to reach better separating degree, the present invention has screened gradient elution mode, the experimental results showed that, no
With gradient elution mode, the separating degree of each compound is influenced it is big, the present invention by adjusting separating degree in different time periods and
Chromatographic peak number preferably obtains optimal gradient elution mode are as follows: the ratio of Mobile phase B changes are as follows: 0~20min, 5%~
12% acetonitrile；20~40min, 12%~17% acetonitrile；40~55min, 17%~23% acetonitrile；55~95min, 23%~
33% acetonitrile；95~105min, 33%~100% acetonitrile.
(2) selection of different Detection wavelengths:
The present invention has screened chromatography testing result under different wave length 230nm, 254nm, 280nm by many experiments, detection
Each feature peak intensity is preferable at 254nm as the result is shown, therefore selects 254nm as Detection wavelength, as shown in Figure 1.
(3) selection different in flow rate:
The present invention is respectively in flow velocity 0.8mlmin-1、1.0ml·min-1、1.2ml·min-1Under detected, detection knot
Fruit shows flow velocity in 0.8mlmin-1Under each characteristic peak separating degree it is preferable, therefore select flow velocity for 0.8mlmin-1。
The beneficial effects of the present invention are:
(1) wine fruit of glossy privet finger-print established by the present invention can effectively characterize the quality of the wine fruit of glossy privet, be conducive to complete
The quality of face monitoring drug.
(2) finger-print that the present invention establishes can focus on each tandem and correlation for constituting fingerprint characteristic peak,
Focus on whole facial feature, not only can avoid determining the one-sidedness of wine glossy privet protonatomic mass because measuring individual chemical ingredient, but also can subtract
A possibility that artificially being handled for requisite quality less.
(3) the method for the present invention has the advantages that method is easy, stablizes, precision is high, favorable reproducibility.
Detailed description of the invention
Fig. 1 is chromatogram of the wine fruit of glossy privet test sample at 254nm.
Fig. 2 is chromatogram of the reference substance solution at 254nm.
Specific embodiment
Embodiment of the present invention is described in detail below in conjunction with embodiment, actual conditions are not specified in embodiment
Person carries out according to conventional conditions or manufacturer's recommended conditions.Reagents or instruments used without specified manufacturer, being can be with
Conventional products that are commercially available.
Embodiment 1
Following embodiment instrument
Japanese Shimadzu Corporation Shimadzu LC-20AB highly effective liquid phase chromatographic system, including on-line degassing machine, automatic sampling
Device Prominence SIL-20A, diode array detector SPD-M20A and column oven CTO-20A；ME204E electronic analysis day
Flat (Mei Tele-support benefit Internaional, Inc, be accurate to ten a ten thousandths)；BSM220.4 assay balance (the tall and erect essence in Shanghai
Company is accurate to a ten thousandth)；GVS type ultrasonic cleaner (Gou Wei Science and Technology Ltd., Shenzhen)；TGL-16C high speed platform
Formula centrifuge (Anting Scientific Instrument Factory, Shanghai).
Reagent used in following instance is as follows: Specnuezhenide analytical standard product (lot number 5937, purity 99.5%), rhodioside
Reference substance (lot number 4256, purity 99.7%), tyrosol reference substance (lot number 1487, purity 99.7%) are purchased from Shanghai poem pellet moral mark
Quasi- Technology Service Co., Ltd.Rutin, Quercetin, galuteolin, that luteolin acteoside reference substance is purchased from Nanjing is gloomy
Bei Jia Biotechnology Co., Ltd.Acetonitrile is chromatographically pure, and water is ultrapure water, and phosphoric acid is that analysis is pure.The wine fruit of glossy privet is (in the Hai Yuan of Nanjing
Medicine medicine materical crude slice Co., Ltd, lot number 180509,180409,180309,180109,171209,171109,171010,170910,
170810,170710), other reagents (analysis is pure).
Embodiment 1
A kind of fingerprint atlas detection method of the wine fruit of glossy privet comprising following steps:
(1) preparation of test solution
Take respectively 10 batches of wine fruit of glossy privets to be measured (Nanjing Hai Yuan prepared slices of Chinese crude drugs Co., Ltd, lot number 180509,180409,
180309, powder 180109,171209,171109,171010,170910,170810,170710) for use, is beaten, it is close to weigh No. 4
The powder 1.0g for sieving (65 mesh), is placed in stuffed conical flask, and methanol 25ml, weighed quality, in power 250w, frequency is added in precision
It is ultrasonically treated 30min under conditions of 40KHz, is placed at room temperature for, then weighed quality, supplies weightlessness, 12000r/min centrifugation with methanol
3min, takes supernatant, cross 0.45 μm of organic miillpore filter to get.
(2) preparation of reference substance solution
Take Specnuezhenide, rhodioside, tyrosol, galuteolin, rutin and acteoside reference substance appropriate respectively, it is accurate
It is weighed, it is placed in 10ml volumetric flask, methanol is added to be made into the root of kirilow rhodiola that concentration is respectively the Specnuezhenide of 290 μ g/ml, 117 μ g/ml
Glycosides, the tyrosol of 143 μ g/ml, the galuteolin of 285 μ g/ml, the rutin of 276 μ g/ml, 540 μ g/ml acteoside pair
According to product stock solution；Accurate Specnuezhenide, rhodioside, tyrosol, galuteolin, rutin and acteoside reference substance solution respectively
In right amount, add methanol constant volume to 20ml, every 1ml is made containing 14.5 μ g of Specnuezhenide, 6.8 μ g of rhodioside, 7.2 μ g of tyrosol, sweet-scented osmanthus
The mixed reference substance solution of careless 14.2 μ g of glycosides, 13.8 μ g of rutin, 27.0 μ g of acteoside.
(3) mixed reference substance solution of 10 batches of wine fruit of glossy privet test solutions and step 2 of the accurate aspiration step 1 of difference,
High performance liquid chromatograph is injected, chromatogram is recorded；
(4) finger-print of obtain in step 3 10 batches of wine fruit of glossy privet test solutions is exported, and imports Chinese medicine chromatography
Fingerprint similarity evaluation system 2004A；Select in the chromatogram of the 10 batch wine fruit of glossy privets existing chromatographic peak as being total to
There is peak；The reference fingerprint of the wine fruit of glossy privet is generated with mean value calculation method, similarity evaluation the results are shown in Table 2.It calculates each shared
The relative retention time and relative peak area at peak；And (shown in Fig. 2, rhodioside retains according to mixed reference substance solution chromatogram
Time is 26.300min, tyrosol retention time is 28.666min, rutin retention time is 57.377min, galuteolin retains
Time is 58.991min, acteoside retention time is 59.624min, Specnuezhenide 61.699min) retention time mark
Infuse the chemical component at peak in reference fingerprint.
Chromatographic condition and system suitability
Chromatographic column: Purospher STAR LP RP-18endcapped, 4.6*250mm, 5 μm.
Mobile phase: A phase: 0.1 volume % phosphoric acid water；B phase: acetonitrile；Detection wavelength: 254nm, flow velocity: 0.8mlmin-1,
Column temperature: 30 DEG C；Gradient elution program such as the following table 1:
1 gradient elution program of table
| Time/min | Mobile phase A percent by volume | Mobile phase B percent by volume |
| 0 | 95 | 5 |
| 20 | 88 | 12 |
| 40 | 83 | 17 |
| 55 | 77 | 23 |
| 95 | 67 | 33 |
| 105 | 0 | 100 |
。
2 10 batches of wine fruit of glossy privet test solution similarity evaluation results of table
The finger-print of acquisition shares 10 shared peaks, by detecting simultaneously to reference substance solution and test solution, respectively
The retention time at shared peak is respectively as follows: shared peak 1, retention time 25.385min；Shared peak 2, retention time are
27.623min；Shared peak 3, retention time 37.849min；Shared peak 4, retention time 48.670min；Shared peak 5, is protected
Staying the time is 57.478min；Shared peak 6, retention time 58.276min；Shared peak 7, retention time 59.004min；Altogether
There are peak 8, retention time 61.698min；Shared peak 9, retention time 80.021min；Shared peak 10, retention time are
85.180min.Wherein, No. 1 peak is rhodioside, and No. 2 peaks are tyrosol, and No. 5 peaks are rutin, and No. 6 peaks are galuteolin, No. 7 peaks
For acteoside, No. 8 peaks are Specnuezhenide.
The methodological study of 2 finger-print of embodiment detection:
1, methodological study
1.1 precision are investigated
Taking lot number is the 180509 wine fruit of glossy privet, and preparation method of test article in accordance with the above-mentioned embodiment 1 is prepared for examination
Product solution continuous sample introduction 6 times, each 10 μ L of sample volume, is detected by 1 chromatographic condition of above-described embodiment, measures its HPLC chromatogram,
10 shared fingerprint peaks in chromatogram are investigated, the results showed that, the retention time RSD of shared fingerprint peaks is respectively less than 2.5%,
Shared peak peak area RSD is respectively less than 2.6%, illustrates that instrument precision is preferable.
1.2 study on the stability
Taking lot number is the 180509 wine fruit of glossy privet, and it is molten that preparation method of test article in accordance with the above-mentioned embodiment 1 prepares test sample
Liquid, by the chromatographic condition in above-described embodiment 1 respectively at 0,2,4,8,12, sample introduction, records chromatogram, in chromatogram 10 for 24 hours
A shared fingerprint peaks are investigated, the results showed that, the retention time RSD of shared fingerprint peaks is respectively less than 2.0%, shares peak peak area
RSD is respectively less than 2.4%, illustrates that test solution is preferable in internal stability for 24 hours.
1.3 repeatability are investigated
Taking lot number is 180,509 6 parts of wine glossy privet subsample, and preparation method of test article preparation is for examination in accordance with the above-mentioned embodiment 1
Product solution, measures respectively, records chromatogram, investigates to 6 shared fingerprint peaks in chromatogram, the results showed that, share fingerprint
The retention time RSD at peak is respectively less than 2.1%, and shared peak peak area RSD is respectively less than 2.0%, illustrates that this method repeatability is good.
By above the experimental results showed that, the wine fruit of glossy privet fingerprint atlas detection method that the present invention establishes, precision, stability
With it is reproducible, can effectively characterize the quality of the wine fruit of glossy privet, be conducive to its quality of overall monitor.
Claims (9)
1. a kind of fingerprint atlas detection method of the wine fruit of glossy privet, which comprises the following steps:
The preparation of step 1, wine fruit of glossy privet test solution:
It is stand-by to weigh wine fruit of glossy privet medicine materical crude slice, beats powder, weighs powder and be placed in stuffed conical flask, methanol is added, weighs, ultrasonic treatment
After supply weightlessness, take supernatant to be filtered after centrifugation with 0.45 μm of organic miillpore filter, take subsequent filtrate to get；
The preparation of step 2, reference substance solution:
Take Specnuezhenide, rhodioside, tyrosol, galuteolin, rutin and acteoside reference substance appropriate respectively, precision claims
It is fixed, it is respectively placed in volumetric flask, methanol is added to be made into reference substance stock solution respectively；Then accurate respectively to draw Specnuezhenide, red scape
Its glycosides, tyrosol, galuteolin, the reference substance solution of rutin and acteoside are appropriate, add methanol constant volume to 20ml, special female is made
Loyal glycosides, rhodioside, tyrosol, galuteolin, rutin and acteoside mixed reference substance solution；
Step 3, the accurate wine fruit of glossy privet test solution of aspiration step 1 and the mixed reference substance solution of step 2, injection are high respectively
Effect liquid phase chromatogram instrument records chromatogram；
Step 4, the finger-print of the wine fruit of glossy privet test solution obtained in step 3 is exported, and imports Chinese medicine chromatographic fingerprint
Map similarity evaluation system 2004A；Select in the chromatogram of the different batches wine fruit of glossy privet existing chromatographic peak as sharing
Peak；The reference fingerprint of the wine fruit of glossy privet is generated with mean value calculation method, calculates the relative retention time at each shared peak and opposite
Peak area；And the chemical component at peak in reference fingerprint is marked according to the retention time of mixed reference substance solution chromatogram.
2. a kind of fingerprint atlas detection method of wine fruit of glossy privet according to claim 1, which is characterized in that
Step 1, wine fruit of glossy privet test solution the preparation method comprises the following steps:
It takes wine fruit of glossy privet medicine materical crude slice stand-by, beats powder, precision weighed the powder 1.0g of No. 4 sieves, and was placed in stuffed conical flask, and precision adds
Enter methanol 25ml, weighed quality, ultrasonic extraction 30min is placed at room temperature for, then weighed quality, supplies weightlessness, 12000r/ with methanol
Min is centrifuged 3min, takes supernatant, cross 0.45 μm of organic miillpore filter to get.
3. a kind of fingerprint atlas detection method of wine fruit of glossy privet according to claim 1, which is characterized in that
The preparation of step 2, mixed reference substance solution:
Take Specnuezhenide, rhodioside, tyrosol, galuteolin, rutin and acteoside reference substance appropriate respectively, precision claims
It is fixed, it is placed in 10ml volumetric flask, methanol is added to be made into the root of kirilow rhodiola that concentration is respectively the Specnuezhenide of 290 μ g/ml, 117 μ g/ml
Glycosides, the tyrosol of 143 μ g/ml, the galuteolin of 285 μ g/ml, the rutin of 276 μ g/ml, 540 μ g/ml acteoside pair
According to product stock solution；Accurate Specnuezhenide, rhodioside, tyrosol, galuteolin, rutin and acteoside reference substance solution respectively
In right amount, add methanol constant volume to 20ml, every 1ml is made containing 14.5 μ g of Specnuezhenide, 6.8 μ g of rhodioside, 7.2 μ g of tyrosol, sweet-scented osmanthus
The mixed reference substance solution of careless 14.2 μ g of glycosides, 13.8 μ g of rutin, 27.0 μ g of acteoside.
4. a kind of fingerprint atlas detection method of wine fruit of glossy privet according to claim 1, which is characterized in that
The chromatographic condition that step 3, high performance liquid chromatograph detect are as follows:
It is flowing with acetonitrile using the water containing 0.1% phosphoric acid as mobile phase A using octadecylsilane chemically bonded silica as filler
Phase B, gradient elution, flow velocity are 0.5~1.5mlmin-1, 25~40 DEG C of column temperature, 200~360nm of Detection wavelength.
5. a kind of fingerprint atlas detection method of wine fruit of glossy privet according to claim 4, which is characterized in that
The chromatographic condition of step 3 high performance liquid chromatograph detection are as follows: using octadecylsilane chemically bonded silica as filler, to contain
The water of 0.1% phosphoric acid is as mobile phase A, using acetonitrile as Mobile phase B, gradient elution, and flow velocity 0.8mlmin-1, 30 DEG C of column temperature,
Detection wavelength 254nm.
6. a kind of fingerprint atlas detection method of wine fruit of glossy privet according to claim 4 or 5, which is characterized in that gradient is washed
It is de- to be preferably as follows:
。
7. a kind of fingerprint atlas detection method of wine fruit of glossy privet according to claim 6, which is characterized in that chromatographic column is color
Composing column is Purospher STAR LP RP-18 endcapped, 4.6*250mm, 5 μm.
8. a kind of fingerprint atlas detection method of wine fruit of glossy privet according to claim 1, which is characterized in that obtained wine female
There are 10 shared peaks in loyal sub fingerprint map, the retention time that the retention time at each shared peak is respectively as follows: shared peak 1 is
25.385min；The retention time at shared peak 2 is 27.623min；The retention time at shared peak 3 is 37.849min；Shared peak 4
Retention time is 48.670min；The retention time at shared peak 5 is 57.478min；The retention time at shared peak 6 is
58.276min；The retention time at shared peak 7 is 59.004min；The retention time at shared peak 8 is 61.698min；Shared peak 9
Retention time is 80.021min；The retention time at shared peak 10 is 85.180min.
9. a kind of fingerprint atlas detection method of wine fruit of glossy privet according to claim 8, which is characterized in that wherein, No. 1 peak
For rhodioside, No. 2 peaks are tyrosol, and No. 5 peaks are rutin, and No. 6 peaks are galuteolin, and No. 7 peaks are acteoside, and No. 8 peaks are
Specnuezhenide.
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Cited By (5)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN110596277A (en) * | 2019-10-14 | 2019-12-20 | 天津中医药大学 | Method for identifying glossy privet fruit raw product and wine product |
| CN111366672A (en) * | 2020-04-24 | 2020-07-03 | 劲牌有限公司 | Detection method of health wine fingerprint |
| CN113640432A (en) * | 2021-10-13 | 2021-11-12 | 江西省药品检验检测研究院 | Quality evaluation method of loins strengthening and body building pills |
| CN114965732A (en) * | 2022-04-07 | 2022-08-30 | 陕西医药控股集团山海丹药业股份有限公司 | Construction method and application of HPLC fingerprint of Qitianfuzheng capsule |
| CN116036156A (en) * | 2022-12-26 | 2023-05-02 | 仲景宛西制药股份有限公司 | Processing method of wine glossy privet fruit |
Citations (1)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN108802217A (en) * | 2018-05-28 | 2018-11-13 | 南京中医药大学 | The quality control of Chinese medicine compound prescription and evaluation method |
-
2018
- 2018-12-26 CN CN201811600046.1A patent/CN109633001B/en active Active
Patent Citations (1)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN108802217A (en) * | 2018-05-28 | 2018-11-13 | 南京中医药大学 | The quality control of Chinese medicine compound prescription and evaluation method |
Non-Patent Citations (2)
| Title |
|---|
| LIFU SHI ET AL.: "Quantitative Determination of Salidroside and Specnuezhenide in the Fruits of Ligustrum lucidum Ait by High Performance Liquid Chromatography", 《BIOMEDICAL CHROMATOGRAPHY》 * |
| 吴修红 等: "酒女贞子HPLC指纹图谱的建立及多成分含量的测定", 《药物分析杂志》 * |
Cited By (9)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN110596277A (en) * | 2019-10-14 | 2019-12-20 | 天津中医药大学 | Method for identifying glossy privet fruit raw product and wine product |
| CN110596277B (en) * | 2019-10-14 | 2022-07-22 | 天津中医药大学 | Method for identifying glossy privet fruit raw product and wine product |
| CN111366672A (en) * | 2020-04-24 | 2020-07-03 | 劲牌有限公司 | Detection method of health wine fingerprint |
| CN111366672B (en) * | 2020-04-24 | 2021-06-22 | 劲牌有限公司 | Detection method of health wine fingerprint |
| CN113640432A (en) * | 2021-10-13 | 2021-11-12 | 江西省药品检验检测研究院 | Quality evaluation method of loins strengthening and body building pills |
| CN114965732A (en) * | 2022-04-07 | 2022-08-30 | 陕西医药控股集团山海丹药业股份有限公司 | Construction method and application of HPLC fingerprint of Qitianfuzheng capsule |
| CN114965732B (en) * | 2022-04-07 | 2023-12-22 | 陕西医药控股集团山海丹药业股份有限公司 | Construction method and application of HPLC fingerprint of Qitianfu body resistance strengthening capsule |
| CN116036156A (en) * | 2022-12-26 | 2023-05-02 | 仲景宛西制药股份有限公司 | Processing method of wine glossy privet fruit |
| CN116036156B (en) * | 2022-12-26 | 2024-01-26 | 仲景宛西制药股份有限公司 | Processing method of wine glossy privet fruit |
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