CN108717084A - The liquid chromatography-mass spectrography detection method of ursodeoxycholic acid content in bear gall powder - Google Patents
The liquid chromatography-mass spectrography detection method of ursodeoxycholic acid content in bear gall powder Download PDFInfo
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Abstract
The present invention relates to a kind of liquid chromatography-mass spectrography detection methods of ursodeoxycholic acid content in bear gall powder, it is characterised in that：This method comprises the following steps：1) preparation of standard working solution；2) preparation of sample working solution：3) Liquid Chromatography-Tandem Mass Spectrometry tests and analyzes.The design of the invention is scientific and reasonable, can carry out accurate qualitative and quantitative analysis to the ursodesoxycholic acid in bear gall powder so that composition detection is analyzed more rapidly, the time is saved, and detection sensitivity is high, detection data is accurate, sample usage amount is saved, it is cost-effective, improve detection efficiency.
Description
Technical field
The invention belongs to pharmaceutical active ingredient detection fields, are related to bear gall powder active component detection, more particularly to a kind of bear
The liquid chromatography-mass spectrography detection method of ursodeoxycholic acid content in courage powder.
Background technology
Bear gall is the gall-bladder of ursidae animal black bear or brown bear, and the fresh bile of artificial breeding bear living is taken in the method for science,
Bear gall powder is made through science processing and refining.It is confirmed through function test, bear gall powder has the work for adjusting blood fat, reducing total cholesterol
With without any auxiliary material and chemical addition agent.Bear gall powder is also rare Chinese medicine, for heat-clearing, detoxifies, clears liver and improve vision, and treatment is frightened
The diseases such as wind twitch, hot eyes, abscess of throat.Modern pharmacological research proves that bear gall powder has clearing away heat and alleviating pain, antibechic, calmness, resists and shy
Faint, spasmolysis, liver protection, cholagogic, it is antibacterial and to cardiovascular disease, antiviral, anti-inflammatory, antibacterial, prevent gall stone and dissolving gall stone etc.
Effect (《Pharmacopoea Chinensis》2015 editions one, P1701).
It capable of quickly being absorbed by human body in bear gall powder, the main component that good action is played to body is ursodesoxycholic acid,
There is good effect to the prevention of acholia and gall stone.Therefore, in bear gall powder the detection of ursodesoxycholic acid and efficiently
It is extracted into the core technology for medicine and biological field, operating personnel there must be the content of ursodesoxycholic acid in bear gall powder
Clearly understand.
Currently, common ursodesoxycholic acid Detection and Extraction method is complicated for operation in experimental implementation, due to bear gall meal component compared with
For complexity, and the more similar Cholic acids compound of property is all concentrated on, therefore can not be qualitative to the analysis of ursodesoxycholic acid
Quantitative, detection structure is inaccurate；And bear gall powder is expensive, extraction used sample amount is larger in experiment detection, causes sample unrestrained
Take, improves cost.
By the retrieval to patent document, the public affairs to ursodesoxycholic acid detection method of content in bear gall powder are not found
Patent document is opened, does not also find patent document identical with present patent application.
Invention content
It is an object of the invention to overcome the deficiencies of the prior art and provide it is a kind of detection it is easy to operate, accuracy of detection is high, inspection
Precise and high efficiency is surveyed, and liquid chromatogram-matter of ursodeoxycholic acid content in the cost-effective bear gall powder of sample usage amount can be saved
Spectrum detection method.
The present invention solves its technical problem and is achieved through the following technical solutions：
The liquid chromatography-mass spectrography detection method of ursodeoxycholic acid content in a kind of bear gall powder, it is characterised in that：This method packet
Include following steps：
1) preparation of standard working solution：
Ursodesoxycholic acid standard items 0.5g accurately is weighed, with methanol dissolved dilution and is transferred to constant volume in 100mL volumetric flasks,
It is configured to the ursodesoxycholic acid standard working solution of a concentration of 0.5g/L, it is spare；
The preparation of sample working solution：
Precise 0.1g ursodesoxycholic acid samples are added the dissolving of ursodesoxycholic acid extracting solution, are divided into 3~5 in beaker
Secondary that sample diluting liquid is transferred in 100mL volumetric flasks, sonic oscillation extracts 30min and is cooled to room temperature after vortex mixing, uses
Bear removes courage oxygen acid extracting solution constant volume and is transferred to centrifuge to carry out after centrifugal treating Aspirate supernatant and with filtering with microporous membrane, standby
With；
3) Liquid Chromatography-Tandem Mass Spectrometry tests and analyzes：
Standard working solution and sample working solution are injected separately into liquid chromatography-tandem mass spectrometry instrument, are analyzed by mass spectrometry,
Quantitative comparison is carried out with the peak area of standard working solution and sample working solution peak area, retention time is qualitative, and external standard method is counted
It calculates, calculates the mass fraction w of ursodesoxycholic acid in sample.
Moreover, the mass fraction w of ursodesoxycholic acid is calculated using following formula in the step 3)：
W=(c*V*10-7/ m) * 100%
Wherein：C is the content of ursodesoxycholic acid in sample working solution, unit ng/mL；
V is the volume of sample working solution, unit mL；
M is the quality of sample, unit g.
Moreover, the liquid phase chromatogram condition is：
Chromatographic column：RP-C181.7μm 50×2.1mm；
Mobile phase：A phases are aqueous formic acid, and B phases are formic acid methanol solution；
Flow velocity：0.15-0.5mL/min；
Column temperature：25-40℃；
Sample size：1-10μL；
Detector uses UV ultraviolet detectors；
The Mass Spectrometry Conditions are：
Mass ion source：Electron spray cation；
Mass ions source temperature：325℃；
Detection mode：The more reaction detections of MRM；
Desolvation gas：N2；
Desolvation gas flow velocity：10~40Arb；
Secondary air speed：0-20Arb；
Ion transfer tube temperature：280~400 DEG C；
Evaporator temperature：280-400℃；
Moreover, the elution requirement of mobile phase is gradient elution, 0min aqueous formic acids in the liquid phase chromatogram condition：Formic acid
Methanol is 90：10；3min aqueous formic acids：Formic acid methanol is 90：10；5min aqueous formic acids：Formic acid methanol is 10：90；
7min aqueous formic acids：Formic acid methanol is 10：90；7.1mim aqueous formic acid：Formic acid methanol is 90：10；10min formic acid is water-soluble
Liquid：Formic acid methanol is 90：10.
Moreover, in the Mass Spectrometry Conditions, the mass spectrometry parameters of ursodesoxycholic acid are：Parent ion 391.14m/z, daughter ion
359.03m/z。
Moreover, the ursodesoxycholic acid extracting solution is the methanol solution that mass fraction is 15%.
Moreover, the rotating speed of the centrifuge is 8000r/min, 3min is centrifuged.
The advantages of the present invention are：
1, in bear gall powder of the invention ursodeoxycholic acid content liquid chromatography-mass spectrography detection method, be different from current city
The method for the liquid chromatography analysis ursodesoxycholic acid largely used on field, using the analysis side of liquid chromatograph mass spectrography
Method can more targetedly more rapidly effectively carry out accurate qualitative and quantitative analysis to the ursodesoxycholic acid in bear gall powder, make
It obtains composition detection analysis more rapidly, saves the time, improve detection efficiency.
2, in bear gall powder of the invention ursodeoxycholic acid content liquid chromatography-mass spectrography detection method, the bear deoxidation of acquisition
The peak shape and separating degree of cholic acid are all fine, and linear good, avoid the interference of other substances, shorten detection time, detection carries
It takes more accurate.
3, in bear gall powder of the invention ursodeoxycholic acid content liquid chromatography-mass spectrography detection method, accuracy of detection is high, inspection
Sensitive, reduction sample usage amount is surveyed, it is cost-effective, shorten detection time, improves detection efficiency.
Description of the drawings
Fig. 1 is the mass spectrogram of standard working solution of the present invention and sample working solution.
Specific implementation mode
Below by specific embodiment, the invention will be further described, and following embodiment is descriptive, is not limit
Qualitatively, protection scope of the present invention cannot be limited with this.
The liquid chromatography-mass spectrography detection method of ursodeoxycholic acid content, innovation are in a kind of bear gall powder：The party
Method includes the following steps：
1) preparation of standard working solution：
Ursodesoxycholic acid standard items 0.5g accurately is weighed, with methanol dissolved dilution and is transferred to constant volume in 100mL volumetric flasks,
It is configured to the ursodesoxycholic acid standard working solution of a concentration of 0.5g/L, it is spare；
The preparation of sample working solution：
Precise 0.1g ursodesoxycholic acid samples are added the methanol solution that mass fraction is 15% and dissolve in beaker,
It is divided into 3~5 times sample diluting liquid is transferred in 100mL volumetric flasks, sonic oscillation extracts 30min and is cooled to after vortex mixing
Methanol solution constant volume that room temperature is 15% with mass fraction is simultaneously transferred to centrifuge and carries out centrifugal treating, rotating speed 8000r/
Min, centrifuges 3min, Aspirate supernatant and with filtering with microporous membrane, spare；
3) Liquid Chromatography-Tandem Mass Spectrometry tests and analyzes：
Standard working solution and sample working solution are injected separately into liquid chromatography-tandem mass spectrometry instrument, are analyzed by mass spectrometry,
Quantitative comparison is carried out with the peak area of standard working solution and sample working solution peak area, retention time is qualitative, and external standard method is counted
It calculates, calculates the mass fraction w of ursodesoxycholic acid in sample.
The mass fraction w of ursodesoxycholic acid is calculated using following formula in step 3)：
W=(c*V*10-7/ m) * 100%
Wherein：C is the content of ursodesoxycholic acid in sample working solution, unit ng/mL；
V is the volume of sample working solution, unit mL；
M is the quality of sample, unit g.
Liquid phase chromatogram condition is：
Chromatographic column：RP-C181.7μm 50×2.1mm；
Mobile phase：A phases are aqueous formic acid, and B phases are formic acid methanol solution；
Flow velocity：0.15-0.5mL/min；
Column temperature：25-40℃；
Sample size：1-10μL；
Detector uses UV ultraviolet detectors；
Elution requirement is gradient elution, and parameter is shown in Table 1.
1 Parameters of gradient elution of table
Mass Spectrometry Conditions are：
Mass ion source：Electron spray cation；
Mass ions source temperature：325℃；
Detection mode：The more reaction detections of MRM；
Desolvation gas：N2；
Desolvation gas flow velocity：10~40Arb；
Secondary air speed：0-20Arb；
Ion transfer tube temperature：280~400 DEG C；
Evaporator temperature：280-400℃；
The mass spectrometry parameters of ursodesoxycholic acid are shown in Table 2.
The mass spectrometry parameters of 2 ursodesoxycholic acid of table
| Chinese | Parent ion (m/z) | Daughter ion 1 (m/z) |
| Ursodesoxycholic acid | 391.139 | 359.034 |
Although disclosing the embodiment of the present invention and attached drawing for the purpose of illustration, those skilled in the art can manage
Solution：Do not departing from the present invention and spirit and scope of the appended claims in, various substitutions, changes and modifications be all it is possible,
Therefore, the scope of the present invention is not limited to embodiment and attached drawing disclosure of that.
Claims (7)
1. the liquid chromatography-mass spectrography detection method of ursodeoxycholic acid content in a kind of bear gall powder, it is characterised in that：This method includes
Following steps：
1) preparation of standard working solution：
Ursodesoxycholic acid standard items 0.5g accurately is weighed, with methanol dissolved dilution and is transferred to constant volume in 100mL volumetric flasks, is prepared
It is spare at the ursodesoxycholic acid standard working solution of a concentration of 0.5g/L；
2) preparation of sample working solution：
The dissolving of ursodesoxycholic acid extracting solution is added in beaker in precise 0.1g ursodesoxycholic acid samples, and being divided into 3~5 times will
Sample diluting liquid is transferred in 100mL volumetric flasks, and sonic oscillation extracts 30min and is cooled to room temperature after vortex mixing, is gone with bear
Courage oxygen acid extracting solution constant volume is simultaneously transferred to centrifuge and carries out after centrifugal treating Aspirate supernatant and with filtering with microporous membrane, spare；
3) Liquid Chromatography-Tandem Mass Spectrometry tests and analyzes：
Standard working solution and sample working solution are injected separately into liquid chromatography-tandem mass spectrometry instrument, liquid chromatography-mass spectrography is carried out
Analysis carries out quantitative comparison with the peak area of standard working solution and sample working solution peak area, and retention time is qualitative, external standard method into
Row calculates, and calculates the mass fraction w of ursodesoxycholic acid in sample.
2. the liquid chromatography-mass spectrography detection method of ursodeoxycholic acid content, feature in bear gall powder according to claim 1
It is：The mass fraction w of ursodesoxycholic acid is calculated using following formula in the step 3)：
W=(c*V*10-7/ m) * 100%
Wherein：C is the content of ursodesoxycholic acid in sample working solution, unit ng/mL；
V is the volume of sample working solution, unit mL；
M is the quality of sample, unit g.
3. the liquid chromatography-mass spectrography detection method of ursodeoxycholic acid content, feature in bear gall powder according to claim 1
It is：The liquid phase chromatogram condition is：
Chromatographic column：RP-C181.7μm 50×2.1mm；
Mobile phase：A phases are aqueous formic acid, and B phases are formic acid methanol solution；
Flow velocity：0.15-0.5mL/min；
Column temperature：25-40℃；
Sample size：1-10μL；
Detector uses UV ultraviolet detectors；
The Mass Spectrometry Conditions are：
Mass ion source：Electron spray cation；
Mass ions source temperature：325℃；
Detection mode：The more reaction detections of MRM；
Desolvation gas：N2；
Desolvation gas flow velocity：10~40Arb；
Secondary air speed：0-20Arb；
Ion transfer tube temperature：280~400 DEG C；
Evaporator temperature：280-400℃.
4. the liquid chromatography-mass spectrography detection method of ursodeoxycholic acid content, feature in bear gall powder according to claim 3
It is：The elution requirement of mobile phase is gradient elution, 0min aqueous formic acids in the liquid phase chromatogram condition：Formic acid methanol is
90：10；3min aqueous formic acids：Formic acid methanol is 90：10；5min aqueous formic acids：Formic acid methanol is 10：90；7min formic acid
Aqueous solution：Formic acid methanol is 10：90；7.1mim aqueous formic acid：Formic acid methanol is 90：10；10min aqueous formic acids：Formic acid
Methanol is 90：10.
5. the liquid chromatography-mass spectrography detection method of ursodeoxycholic acid content, feature in bear gall powder according to claim 3
It is：In the Mass Spectrometry Conditions, the mass spectrometry parameters of ursodesoxycholic acid are：Parent ion 391.14m/z, daughter ion 359.03m/z.
6. the liquid chromatography-mass spectrography detection method of ursodeoxycholic acid content, feature in bear gall powder according to claim 1
It is：The ursodesoxycholic acid extracting solution is the methanol solution that mass fraction is 15%.
7. the liquid chromatography-mass spectrography detection method of ursodeoxycholic acid content, feature in bear gall powder according to claim 1
It is：The rotating speed of the centrifuge is 8000r/min, centrifuges 3min.
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Cited By (2)
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| CN111812264A (en) * | 2020-07-09 | 2020-10-23 | 苏州旭辉检测有限公司 | Biological sample analysis method of deoxycholic acid compound |
| CN114414720A (en) * | 2021-12-24 | 2022-04-29 | 重庆极泽生物科技有限公司 | Method for detecting golden gall powder |
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