CN107045034A - A kind of DANHONG ZHUSHEYE interior metabolism product identifies detection method - Google Patents
A kind of DANHONG ZHUSHEYE interior metabolism product identifies detection method Download PDFInfo
- Publication number
- CN107045034A CN107045034A CN201710190629.0A CN201710190629A CN107045034A CN 107045034 A CN107045034 A CN 107045034A CN 201710190629 A CN201710190629 A CN 201710190629A CN 107045034 A CN107045034 A CN 107045034A
- Authority
- CN
- China
- Prior art keywords
- ida
- epi
- mobile phase
- mrm
- metabolin
- Prior art date
- Legal status (The legal status is an assumption and is not a legal conclusion. Google has not performed a legal analysis and makes no representation as to the accuracy of the status listed.)
- Pending
Links
Classifications
-
- G—PHYSICS
- G01—MEASURING; TESTING
- G01N—INVESTIGATING OR ANALYSING MATERIALS BY DETERMINING THEIR CHEMICAL OR PHYSICAL PROPERTIES
- G01N30/00—Investigating or analysing materials by separation into components using adsorption, absorption or similar phenomena or using ion-exchange, e.g. chromatography or field flow fractionation
- G01N30/02—Column chromatography
- G01N30/88—Integrated analysis systems specially adapted therefor, not covered by a single one of the groups G01N30/04 - G01N30/86
-
- G—PHYSICS
- G01—MEASURING; TESTING
- G01N—INVESTIGATING OR ANALYSING MATERIALS BY DETERMINING THEIR CHEMICAL OR PHYSICAL PROPERTIES
- G01N30/00—Investigating or analysing materials by separation into components using adsorption, absorption or similar phenomena or using ion-exchange, e.g. chromatography or field flow fractionation
- G01N30/02—Column chromatography
- G01N30/88—Integrated analysis systems specially adapted therefor, not covered by a single one of the groups G01N30/04 - G01N30/86
- G01N2030/8809—Integrated analysis systems specially adapted therefor, not covered by a single one of the groups G01N30/04 - G01N30/86 analysis specially adapted for the sample
- G01N2030/8813—Integrated analysis systems specially adapted therefor, not covered by a single one of the groups G01N30/04 - G01N30/86 analysis specially adapted for the sample biological materials
- G01N2030/8822—Integrated analysis systems specially adapted therefor, not covered by a single one of the groups G01N30/04 - G01N30/86 analysis specially adapted for the sample biological materials involving blood
Landscapes
- Physics & Mathematics (AREA)
- Health & Medical Sciences (AREA)
- Life Sciences & Earth Sciences (AREA)
- Chemical & Material Sciences (AREA)
- Analytical Chemistry (AREA)
- Biochemistry (AREA)
- General Health & Medical Sciences (AREA)
- General Physics & Mathematics (AREA)
- Immunology (AREA)
- Pathology (AREA)
- Investigating Or Analysing Biological Materials (AREA)
Abstract
Detection method is identified the invention discloses a kind of DANHONG ZHUSHEYE interior metabolism product：(1) DANHONG ZHUSHEYE body tail vein injection SD rats are taken, different time points are taken a blood sample, centrifugal separation plasma, after plasma treatment, gradient elution separation is carried out to sample using Qtrap LC-MSs instrument, combines powerful MetabolitePilot metabolins identification software to analyze metabolite with reference to a variety of scan patterns such as EMS IDA EPI, (p) MRM IDA EPI, NL/Pre IDA EPI.It was found that the higher active ingredient danshensu of content in parenteral solution, protocatechuic acid, protocatechualdehyde, the II phase metabolins of Rosmarinic acid, mainly methylate, sulphation, sulphation after methylating, a series of metabolins such as glucuronidation.Each metabolite content changes with the passage of administration time, and most of metabolin reaches C in 10 min and 30 minmax, active compound and metabolin after 6 h is administered and largely eliminates.A kind of DANHONG ZHUSHEYE interior metabolism product identification detection method that the present invention is set up is simple, reproducible, accurately and reliably, can provide foundation for DANHONG ZHUSHEYE clinical practice.
Description
Technical field
The invention belongs to drug test analysis field, and in particular to a kind of DANHONG ZHUSHEYE interior metabolism product identification detection
Method.
Background technology
DANHONG ZHUSHEYE（Chinese medicines quasi-word Z20026866）It is from the red sage root by modern crafts（The labiate red sage root
Salvia miltiorrhiza Bunge. drying root and rhizome）And safflower（Feverfew safflower
Drying CarthamustinctoriusL. is spent）The water soluble ingredient preparation for the standardization that two taste traditional Chinese medicines are refined.It is red
Ginseng and safflower are two taste traditional Chinese medicines, are usually shared to treat cardiovascular and cerebrovascular disease.According to traditional theory of traditional Chinese medical science, the red sage root
It is main cold, the main temperature of safflower, one rise and one drop, the effect of playing promoting blood circulation and removing blood stasis, clearing and activating the channels and collaterals altogether.The clinically red red injection of application in recent years
The obstruction of qi in the chest and apoplexy caused by liquid treatment hemostasis impatency obtain curative effect, but treat the material base of ischemic cerebral disease still to it certainly
It is indefinite.Therefore DANHONG ZHUSHEYE is assessed with science, accurate method to cerebral ischemia re-pouring injured effective substance,
The metabolite and approach for understanding it are significant for the clinical application of DANHONG ZHUSHEYE.
The content of the invention
Detection method is identified it is an object of the invention to provide a kind of DANHONG ZHUSHEYE interior metabolism product, specifically use " bar-
Trap " scans IDA mode of operations and completes DANHONG ZHUSHEYE metabolite identification detection method simultaneously in a pin sample introduction；
The technical solution adopted by the present invention is as follows：
A kind of DANHONG ZHUSHEYE interior metabolism product identifies detection method, the described method comprises the following steps：
(1) DANHONG ZHUSHEYE tail vein injection SD rats are taken, injection volume is 10~12 mg/kg, at 10min~6h each time points
Eye socket is taken a blood sample, and blood sample is put in test tube of hepari centrifuge tube, centrifugal separation plasma；
(2) blood sample treatments method：Micro sample adding appliance draws the μ L of blood plasma 200, plus methanol：Acetonitrile mixture, blood plasma and mixing liquid
Product compares 1：2.5~3, vortex mixing, centrifugation takes supernatant to be measured as sample；
(3) sample is tested and analyzed using high performance liquid chromatography-triple quadrupole bar linear ion hydrazine tandem mass spectrum, instrument
Condition is as follows：
A, liquid phase chromatogram condition：Shimadzu UFLC XR
Mobile phase A: H2O (NH containing 0.05%FA+5mM4FA)
Mobile phase B: CH3OH:CH3CN (1:1)
Flow velocity:0.1~0.5 mL/min
Sampling volume:4~10 uL
Chromatographic column: PoroShell 120 EC-C18
Column temperature：40~70 DEG C
Gradient elution；
B, Mass Spectrometry Conditions: AB SCIEX Qtrap 4500 System
Scan pattern Scan Mode：ESI, NEG/POS
Mass spectrum pattern MS mode：EMS (100~750)-IDA-EPI, MRM-IDA-EPI, Prec/NL-IDA-EPI
Enhancer ion scan scope EPI Range：m/z 80-750
Dynamic filling time Dynamic Fill Time：Open
Dynamic background deducts DBS：Open
Gas curtain gas CUR：30 psi
Collision gas CAD：Medium/High
Spray voltage IS：-4500 V
Ion source temperature TEM：550 ℃
Atomization gas Gas1：50 psi
Heat gas Gas2：50 psi
(4) (data dependency is scanned Qtrap LC-MSs instrument combination IDA, automatic data collection MS2) information related scans mode,
The active ingredient and metabolin of EMS-IDA-EPI examination high contents, the highly sensitive examination targets of (p) MRM-IDA-EPI have
Composition and prediction metabolin are imitated, there is feature neutrality to lose the metabolin with feature daughter ion for NL/Pre-IDA-EPI examinations.
(p) MRM-IDA-EPI is three kinds of scan mode medium sensitivity highest patterns, pMRM=Predictive MRM, predictive MRM
Detection, pMRM according to analogue or metabolin there is identical fragment to predict MRM.Data acquisition and processing：
MetabolitePilot metabolins identify software；
Further, the step（1）In, DANHONG ZHUSHEYE tail vein injection SD rats are taken, injection volume is 12 mg/kg, 10
Each time point eye socket blood sampling of min, 30 min, 60 min, 6 h, blood sample is put in test tube of hepari centrifuge tube, and 4000 r/min are centrifuged
Blood plasma；
The step（2）In, blood sample treatments method：Micro sample adding appliance draws the μ L of blood plasma 200, plus methanol：Acetonitrile（1:9）Mixing
Liquid, blood plasma compares 1 with mixeding liquid volume：3, vortex mixes 30 s, and 13000 r centrifuge 15 min, take supernatant to be measured as sample；
The step（3）In, flow velocity:0.3 mL/min, sampling volume:5 uL；
The step（3）In, column temperature：50 ℃；
The step（3）In：Chromatographic column:The mm of the mm of 120 EC-C18 dimensions of PoroShell 150 × 2.1, packing material size
2.7 μm；
The step（3）In：Gradient elution program：0~2min, the volume fraction of Mobile phase B is 2%；2~10min, Mobile phase B
Volume fraction from 2% increase be 40%；10~13min, the volume fraction of Mobile phase B increases to 95% from 40%；13~16min,
The volume fraction of Mobile phase B is 95%, 16~16.1min, the volume fraction of Mobile phase B from 95% be reduced to 2%, 16.1min~
21min, afterwards, the volume fraction of Mobile phase B keep 2%；In gradient elution, the volume fraction sum of mobile phase A and Mobile phase B
For 100%；
More specifically, preferably the inventive method is operated according to the following steps：
(1) DANHONG ZHUSHEYE tail vein injection SD rats are taken, injection volume is 12 mg/kg, in 10 min, 30 min, 60 min,
6 h, 0.3 mL of each time point eye socket blood sampling, blood sample is put in test tube of hepari centrifuge tube, 4000 r/min centrifugal separation plasmas；
(2) blood sample treatments method：Micro sample adding appliance draws the μ L of blood plasma 200, plus methanol：Acetonitrile（1:9）Mixed liquor, blood plasma is with mixing
Close liquid volume ratio 1：3, vortex mixing 30s, 13000r centrifugation 15min, take supernatant to be measured as sample；
(3) sample is tested and analyzed using high performance liquid chromatography-triple quadrupole bar linear ion hydrazine tandem mass spectrum, instrument
Condition is as follows：
A, liquid phase chromatogram condition：Shimadzu UFLC XR
Mobile phase A: H2O (NH containing 0.05%FA+5mM4FA)
Mobile phase B: CH3OH:CH3CN (1:1)
Flow velocity:0.3 mL/min
Sampling volume: 5 uL
Chromatographic column: PoroShell 120 EC-C18 (150×2.1mm, 2.7um)
Column temperature：50 ℃
Gradient elution：0~2min, the volume fraction of Mobile phase B is 2%；2~10min, the volume fraction of Mobile phase B increases from 2%
For 40%；10~13min, the volume fraction of Mobile phase B increases to 95% from 40%；13~16min, the volume fraction of Mobile phase B is
95%, 16~16.1min, the volume fraction of Mobile phase B are reduced to 2%, 16.1min~21min, afterwards, Mobile phase B from 95%
Volume fraction keeps 2%；In gradient elution, the volume fraction sum of mobile phase A and Mobile phase B is 100%；
B, Mass Spectrometry Conditions: AB SCIEX Qtrap 4500 System
Scan pattern Scan Mode：ESI, NEG/POS
Mass spectrum pattern MS mode：EMS (100~750)-IDA-EPI, MRM-IDA-EPI, Prec/NL-IDA-EPI
Enhancer ion scan scope EPI Range：m/z 80-750
Dynamic filling time Dynamic Fill Time：Open
Dynamic background deducts DBS：Open
Gas curtain gas CUR：30 psi
Collision gas CAD：Medium/High
Spray voltage IS：-4500 V
Ion source temperature TEM：550 ℃
Atomization gas Gas1：50 psi
Heat gas Gas2：50 psi
(4) (data dependency is scanned Qtrap LC-MSs instrument combination IDA, automatic data collection MS2) information related scans mode,
The active ingredient and metabolin of EMS-IDA-EPI examination high contents, the highly sensitive examination target effectives of (p) MRM-IDA-EPI
There is feature neutrality to lose the metabolin with feature daughter ion for composition and prediction metabolin, NL/Pre-IDA-EPI examinations.(p)
MRM-IDA-EPI is three kinds of scan mode medium sensitivity highest patterns, pMRM=Predictive MRM, predictive MRM inspections
Survey, pMRM according to analogue or metabolin there is identical fragment to predict MRM.Data acquisition and processing：
MetabolitePilot metabolins identify software；
This detection method finds the higher active ingredient danshensu of content, protocatechuic acid, protocatechualdehyde, Rosmarinic acid in parenteral solution
II phase metabolins, mainly methylate, a series of sulphation, sulphation after methylating, metabolins such as glucuronidation are former
Type danshensu and Rosmarinic acid are not detected by metabolic samples, are changed with the passage of administration time, most of metabolin exists
10min and 30min reaches Cmax, active compound and metabolin after 6h is administered and largely eliminates.It is exclusive based on QTRAP systems
Information Dependent Acquisition mode of operation, the MS of determinand can be obtained simultaneously in single needle sample introduction
And MS2Information, obtains the maximum amount of information, with reference to fragmentation of the specific molecular structure of Chinese medicine in mass spectrum with minimum sample size
Rule, sets up a variety of Survey Scan-IDA-Enhanced Product Ion Scan method collection analysis data, the inspection
Survey method more rapidly, it is sensitiveer；
Embodiments of the present invention are described in further detail below in conjunction with accompanying drawing, embodiment.
Brief description of the drawings
Fig. 1：DANHONG ZHUSHEYE metabolite list figure；
Fig. 2：Danshensu (Danshensu, DSS) metabolin extracts ion flow graph and second order mses figure；
Fig. 3：Protocatechuic acid (Protocatechuic acid, DBA) metabolin extracts ion flow graph and second order mses figure；
Fig. 4：Protocatechualdehyde (Protocaterchuic aldehyde, PA) metabolin extracts ion flow graph and second order mses figure；
Fig. 5：Rosmarinic acid (Rosmarinic acid, RA) metabolin extracts ion flow graph and second order mses figure；
Fig. 6：Time changing curve figure of the danshensu major metabolite in blood plasma；
Fig. 7：Protocatechuic acid and time changing curve figure of its major metabolite in blood plasma；
Fig. 8：Protocatechualdehyde and time changing curve figure of its major metabolite in blood plasma；
Fig. 9：Time changing curve figure of the Rosmarinic acid major metabolite in blood plasma.
Embodiment
In order that the purpose of the present invention, technical scheme, good effect are more clearly understood, by following examples to this hair
It is bright to be further elaborated.Description below for specific embodiment is only used for explaining the present invention, does not limit this hair
It is bright；
A kind of DANHONG ZHUSHEYE interior metabolism product identifies detection method：
First, instrument：Qtrap LC-MS instrument（Mass spectrum AB SCIEX Qtrap 4500 System, liquid phase Shimadzu UFLC
XR）；
2nd, preparation of samples
DANHONG ZHUSHEYE tail vein injection SD rats, injection volume is 12 mg/kg, and in 10 min, 30 min, 60 min, 6 h are each
Time point eye socket 0.3 mL of blood sampling, blood sample is put in test tube of hepari centrifuge tube, 4000 r/min centrifugal separation plasmas.Micro sample adding appliance is inhaled
Take the μ L of blood plasma 200, plus methanol：Acetonitrile（1:9）Mixed liquor, blood plasma compares 1 with mixeding liquid volume：3, vortex mixing 30s, 13000r from
Heart 15min, takes supernatant to be measured as sample；
3rd, testing conditions
A, liquid phase chromatogram condition：Shimadzu UFLC XR
Mobile phase A:H2O (NH4FA containing 0.05%FA+5mM)
Mobile phase B: CH3OH:CH3CN (1:1)
Flow velocity:0.3 mL/min
Sampling volume: 5 uL
Chromatographic column: PoroShell 120 EC-C18 (150×2.1mm, 2.7um)
Column temperature：50 ℃
Gradient elution：0~2min, the volume fraction of Mobile phase B is 2%；2~10min, the volume fraction of Mobile phase B increases from 2%
For 40%；10~13min, the volume fraction of Mobile phase B increases to 95% from 40%；13~16min, the volume fraction of Mobile phase B is
95%, 16~16.1min, the volume fraction of Mobile phase B are reduced to 2%, 16.1min~21min, afterwards, Mobile phase B from 95%
Volume fraction keeps 2%；In gradient elution, the volume fraction sum of mobile phase A and Mobile phase B is 100%；
B, Mass Spectrometry Conditions: AB SCIEX Qtrap 4500 System
Scan pattern Scan Mode：ESI, NEG/POS
Mass spectrum pattern MS mode：EMS (100~750)-IDA-EPI, MRM-IDA-EPI, Prec/NL-IDA-EPI
Enhancer ion scan scope EPI Range：m/z 80-750
Dynamic filling time Dynamic Fill Time：Open
Dynamic background deducts DBS：Open
Gas curtain gas CUR：30 psi
Collision gas CAD：Medium/High
Spray voltage IS：-4500 V
Ion source temperature TEM：550 ℃
Atomization gas Gas1：50 psi
Heat gas Gas2：50 psi
4th, analysis method
Qtrap LC-MS instrument combinations IDA (data dependency is scanned, automatic data collection MS2) information related scans mode is sensitive
Degree, stability, reappearance and triple quadrupole bar are completely the same, while having high sensitivity, high sweep speed and multilevel scanning
Qualitative function, and also there is unique scan function, i.e. bar-trap to be mutually related scanning, real-time dynamic background button（DBS）, one
Secondary sample introduction, can be with positive and negative switch data collection in real time, EMS-IDA-EPI, (p) MRM-IDA-EPI, NL/Pre-IDA-EPI etc.
A variety of scan patterns, identify software MetabolitePilot, with Rapid identification metabolin in combination with the metabolin of intelligence
Unique function；
A variety of scan patterns such as the 1st, EMS-IDA-EPI, MRM-IDA-EPI, Pre/NL-IDA-EPI are combined, and find DANHONG ZHUSHEYE
The higher active ingredient danshensu of middle content, protocatechuic acid, protocatechualdehyde, mainly the II phase metabolins of Rosmarinic acid, methyl
Change, sulphation, sulphation after methylating, a series of metabolins such as glucuronidation.DANHONG ZHUSHEYE metabolite list is shown in
Shown in Fig. 1, prototype danshensu and Rosmarinic acid are not detected by metabolic samples；
2nd, as shown in Figure 2-5, be respectively danshensu, protocatechuic acid, protocatechualdehyde, Rosmarinic acid (Rosmarinic acid,
RA) metabolin extracts ion flow graph and second order mses figure；
3rd, four important activity compositions of DANHONG ZHUSHEYE（Danshensu, Rosmarinic acid, protocatechualdehyde, protocatechuic acid）Metabolin chase after
Track：The blood sample gathered respectively in 10min, 30min, 60min, 6h different time points, carried out using LC-MS instrument to female medicine and
Each metabolite carries out quantitative analysis, determines the blood concentration of different time points, draws time changing curve figure, as a result such as Fig. 6
Shown in~9, each metabolite content detected changes with the passage of administration time, and most of metabolin is in 10min and 30min
Up to Cmax, active compound and metabolin after 6h is administered and largely eliminates；
The content not being described in detail in this specification, belongs to prior art known to those skilled in the art.
Claims (7)
1. a kind of DANHONG ZHUSHEYE interior metabolism product identifies detection method, it is characterised in that the described method comprises the following steps：
(1) DANHONG ZHUSHEYE tail vein injection SD rats are taken, injection volume is 10~12 mg/kg, at 10min~6h each time points
Eye socket is taken a blood sample, and blood sample is put in test tube of hepari centrifuge tube, centrifugal separation plasma；
(2) blood sample treatments method：Micro sample adding appliance draws the μ L of blood plasma 200, plus methanol：Acetonitrile mixture, blood plasma and mixing liquid
Product compares 1：2.5~3, vortex mixing, centrifugation takes supernatant to be measured as sample；
(3) sample is tested and analyzed using high performance liquid chromatography-triple quadrupole bar linear ion hydrazine tandem mass spectrum, instrument
Condition is as follows：
A, liquid phase chromatogram condition：Shimadzu UFLC XR；
Mobile phase A: H2O (NH containing 0.05%FA+5mM4FA) ；
Mobile phase B: CH3OH:CH3CN(1:1)；
Flow velocity:0.1~0.5 mL/min；
Sampling volume:4~10 uL；
Chromatographic column: PoroShell 120 EC-C18；
Column temperature：40~70 DEG C；
Gradient elution；
B, Mass Spectrometry Conditions: AB SCIEX Qtrap 4500 System；
Scan pattern Scan Mode：ESI, NEG/POS；
Mass spectrum pattern MS mode：EMS (100~750)-IDA-EPI, MRM-IDA-EPI, Prec/NL-IDA-EPI；
Enhancer ion scan scope EPI Range：m/z 80-750；
Dynamic filling time Dynamic Fill Time：Open；
Dynamic background deducts DBS：Open；
Gas curtain gas CUR：30 psi；
Collision gas CAD：Medium/High；
Spray voltage IS：-4500 V；
Ion source temperature TEM：550 ℃；
Atomization gas Gas1：50 psi；
Heat gas Gas2：50 psi；
(4) (data dependency is scanned Qtrap LC-MSs instrument combination IDA, automatic data collection MS2) information related scans mode,
The active ingredient and metabolin of EMS-IDA-EPI examination high contents, the highly sensitive examination targets of (p) MRM-IDA-EPI have
Composition and prediction metabolin are imitated, there is feature neutrality to lose the metabolin with feature daughter ion for NL/Pre-IDA-EPI examinations；
(p) MRM-IDA-EPI is three kinds of scan mode medium sensitivity highest patterns, and pMRM=Predictive MRM are predictive
MRM detects that pMRM according to analogue or metabolin there is identical fragment to predict MRM；Data acquisition and processing：
MetabolitePilot metabolins identify software.
2. the method as described in claim 1, it is characterised in that the step（1）In, take DANHONG ZHUSHEYE tail vein injection SD
Rat, injection volume is 12 mg/kg, and in 10 min, 30 min, 60 min, 6 h, 0.3 mL of each time point eye socket blood sampling, blood sample is put
In test tube of hepari centrifuge tube, 4000 r/min centrifugal separation plasmas.
3. the method as described in claim 1, it is characterised in that the step（2）In, blood sample treatments method：Micro sample adding appliance is inhaled
Take the μ L of blood plasma 200, plus methanol：Acetonitrile（1:9）Mixed liquor, blood plasma compares 1 with mixeding liquid volume：3, vortex mixes 30 s, 13000
R centrifuges 15 min, takes supernatant to be measured as sample.
4. the method as described in claim 1, it is characterised in that the step（3）In, flow velocity:0.3 mL/min, sampling volume：
5 uL。
5. the method as described in claim 1, it is characterised in that the step（3）In, column temperature：50 ℃.
6. the method as described in claim 1, it is characterised in that the step（3）Operate by the following method：Chromatographic column：
The mm of the mm of 120 EC-C18 dimensions of PoroShell 150 × 2.1,2.7 μm of packing material size.
7. the method as described in claim 1, it is characterised in that the step（3）Operate by the following method：Gradient elution：0~
2min, the volume fraction of Mobile phase B is 2%；2~10min, it is 40% that the volume fraction of Mobile phase B increases from 2%；10~13min,
The volume fraction of Mobile phase B increases to 95% from 40%；13~16min, the volume fraction of Mobile phase B is 95%, 16~16.1min,
The volume fraction of Mobile phase B is reduced to 2%, 16.1min~21min from 95%, afterwards, and the volume fraction of Mobile phase B keeps 2%；Ladder
In degree elution, the volume fraction sum of mobile phase A and Mobile phase B is 100%.
Priority Applications (1)
| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| CN201710190629.0A CN107045034A (en) | 2017-03-28 | 2017-03-28 | A kind of DANHONG ZHUSHEYE interior metabolism product identifies detection method |
Applications Claiming Priority (1)
| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| CN201710190629.0A CN107045034A (en) | 2017-03-28 | 2017-03-28 | A kind of DANHONG ZHUSHEYE interior metabolism product identifies detection method |
Publications (1)
| Publication Number | Publication Date |
|---|---|
| CN107045034A true CN107045034A (en) | 2017-08-15 |
Family
ID=59544258
Family Applications (1)
| Application Number | Title | Priority Date | Filing Date |
|---|---|---|---|
| CN201710190629.0A Pending CN107045034A (en) | 2017-03-28 | 2017-03-28 | A kind of DANHONG ZHUSHEYE interior metabolism product identifies detection method |
Country Status (1)
| Country | Link |
|---|---|
| CN (1) | CN107045034A (en) |
Cited By (3)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN108802230A (en) * | 2018-06-27 | 2018-11-13 | 北京鸿测科技发展有限公司 | The detection method of danshensu and its metabolite in biological sample |
| CN109725072A (en) * | 2017-10-27 | 2019-05-07 | 中国医学科学院药物研究所 | A kind of targeting qualitative, quantitative metabonomic analysis methods of the screening biomarker for cancer based on LC-MS/MS technology |
| CN113917040A (en) * | 2021-11-01 | 2022-01-11 | 天津中医药大学 | Classification and identification method of ginsenoside components in panax traditional Chinese medicine and application thereof |
-
2017
- 2017-03-28 CN CN201710190629.0A patent/CN107045034A/en active Pending
Cited By (4)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN109725072A (en) * | 2017-10-27 | 2019-05-07 | 中国医学科学院药物研究所 | A kind of targeting qualitative, quantitative metabonomic analysis methods of the screening biomarker for cancer based on LC-MS/MS technology |
| CN108802230A (en) * | 2018-06-27 | 2018-11-13 | 北京鸿测科技发展有限公司 | The detection method of danshensu and its metabolite in biological sample |
| CN108802230B (en) * | 2018-06-27 | 2021-04-16 | 北京鸿测科技发展有限公司 | Method for detecting tanshinol and metabolite thereof in biological sample |
| CN113917040A (en) * | 2021-11-01 | 2022-01-11 | 天津中医药大学 | Classification and identification method of ginsenoside components in panax traditional Chinese medicine and application thereof |
Similar Documents
| Publication | Publication Date | Title |
|---|---|---|
| Li et al. | Applications of HPLC/MS in the analysis of traditional Chinese medicines | |
| Zhang et al. | Holistic quality evaluation of commercial white and red ginseng using a UPLC-QTOF-MS/MS-based metabolomics approach | |
| CN109521114B (en) | Method for detecting main effect components in Yindan Xinnaotong soft capsules | |
| Yang et al. | Localization of constituents for determining the age and parts of ginseng through ultraperfomance liquid chromatography quadrupole/time of flight-mass spectrometry combined with desorption electrospray ionization mass spectrometry imaging | |
| Pang et al. | Comprehensive chemical profiling of Yindan Xinnaotong soft capsule and its neuroprotective activity evaluation in vitro | |
| He et al. | The discovery of Q-markers of Qiliqiangxin Capsule, a traditional Chinese medicine prescription in the treatment of chronic heart failure, based on a novel strategy of multi-dimensional “radar chart” mode evaluation | |
| Yang et al. | A novel neutral loss/product ion scan-incorporated integral approach for the untargeted characterization and comparison of the carboxyl-free ginsenosides from Panax ginseng, Panax quinquefolius, and Panax notoginseng | |
| CN108508107B (en) | Method for simultaneously determining effective components of Xuebijing injection in blood plasma | |
| Li et al. | Rapid discovery of absorbed constituents and metabolites in rat plasma after the oral administration of Zi Shen Wan using high‐throughput UHPLC–MS with a multivariate analysis approach | |
| CN107045034A (en) | A kind of DANHONG ZHUSHEYE interior metabolism product identifies detection method | |
| Li et al. | Global analysis of chemical constituents in Shengmai injection using high performance liquid chromatography coupled with tandem mass spectrometry | |
| Li et al. | Integration of multicomponent characterization, untargeted metabolomics and mass spectrometry imaging to unveil the holistic chemical transformations and key markers associated with wine steaming of Ligustri Lucidi Fructus | |
| Zhou et al. | A two-step ultra-high-performance liquid chromatography-quadrupole/time of flight mass spectrometry with mass defect filtering method for rapid identification of analogues from known components of different chemical structure types in Fructus Gardeniae-Fructus Forsythiae herb pair extract and in rat’s blood | |
| Yao et al. | A strategy for establishment of practical identification methods for Chinese patent medicine from systematic multi-component characterization to selective ion monitoring of chemical markers: Shuxiong tablet as a case study | |
| Li et al. | Ultra-high performance liquid chromatography/ion mobility time-of-flight mass spectrometry-based untargeted metabolomics combined with quantitative assay unveiled the metabolic difference among the root, leaf, and flower bud of Panax notoginseng | |
| Zhan et al. | Chemical profiling in Moutan Cortex after sulfuring and desulfuring processes reveals further insights into the quality control of TCMs by nontargeted metabolomic analysis | |
| Tu et al. | Advances in analytical techniques and quality control of traditional Chinese medicine injections | |
| Zhang et al. | An integrated approach for structural characterization of Gui Ling Ji by traveling wave ion mobility mass spectrometry and molecular network | |
| Li et al. | Rapid characterization of the constituents in Jigucao capsule using ultra high performance liquid chromatography with quadrupole time‐of‐flight mass spectrometry | |
| Xiao-Wei et al. | Metabolite profiling of Zi-Shen pill in rat biological specimens by UPLC-Q-TOF/MS | |
| CN114184727A (en) | Identification method of three medicinal materials derived from gleditschia horrida and application thereof | |
| Luo et al. | Rapid identification and analysis of the active components of traditional Chinese medicine Xiaoxuming decoction for ischemic stroke treatment by integrating UPLC-Q-TOF/MS and RRLC-QTRAP MSn method | |
| Liu et al. | Simultaneous quantification of nine components in the plasma of depressed rats after oral administration of Chaihu-Shugan-San by ultra-performance liquid chromatography/quadrupole-time-of-flight mass spectrometry and its application to pharmacokinetic studies | |
| Peng et al. | Diagnostic fragment-ion-based for rapid identification of chlorogenic acids derivatives in Inula cappa Using UHPLC-Q-Exactive orbitrap mass spectrometry | |
| Wang et al. | Rapid discovery and identification of 68 compounds in the active fraction from Xiao–Xu–Ming decoction (XXMD) by HPLC–HRMS and MTSF technique |
Legal Events
| Date | Code | Title | Description |
|---|---|---|---|
| PB01 | Publication | ||
| PB01 | Publication | ||
| SE01 | Entry into force of request for substantive examination | ||
| SE01 | Entry into force of request for substantive examination | ||
| RJ01 | Rejection of invention patent application after publication |
Application publication date: 20170815 |
|
| RJ01 | Rejection of invention patent application after publication |