CN106153750A - One utilizes the method for wilforine content in ion liquid abstraction/HPLC detection tripterygium hypoglaucum hutcs rhizome - Google Patents
One utilizes the method for wilforine content in ion liquid abstraction/HPLC detection tripterygium hypoglaucum hutcs rhizome Download PDFInfo
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Abstract
The present invention relates to one and utilize the method for wilforine content in ion liquid abstraction/HPLC detection tripterygium hypoglaucum hutcs rhizome, comprise the following steps: (1) sample extraction: weigh tripterygium hypoglaucum hutcs powder sample and put in the container with stirrer, the ionic liquid solution adding solid-to-liquid ratio to be 1:20～60, microwave radiation exaraction 1～9min under 200～600w microwave power；(2) detect: using HPLC to detect, HPLC chromatogram condition is: use Kromasil ODS-C18 post (4mm × 250mm, 5um)；Flowing is acetonitrile-water mutually；Flow velocity is 0.3～0.5ml/min；Detection wavelength is 275nm；Column temperature is 25 DEG C.The method is simple to operate, extraction efficiency is high, detection quick and precisely, can realize rapidly and efficiently detecting the content of wilforine in tripterygium hypoglaucum hutcs rhizome.
Description
Technical field
The present invention relates to Chinese medicine active component detection field, particularly relate to one and utilize the method for wilforine content in ion liquid abstraction/HPLC detection tripterygium hypoglaucum hutcs rhizome.
Background technology
Wilforine (wilforine) is one of medicinal active ingredient in tripterygium hypoglaucum hutcs (Tripterygium hypoglaucum (Levl.) Hutch) rhizome, belong to sequiterpene macrolide Alkaloid, be the one in thunder godvine alkaloids substance.Research shows that thunder godvine alkaloids substance is generally efficient higher in terms for the treatment of rheumatoid arthritis, the effect of also male fertility antitumor, anti-simultaneously, some of which alkaloid monomer has the feature of obvious anti-immunosupress, antitumor action and less toxicity, such as wilforine has obvious humoral immunity inhibitory action, and thunder godvine health alkali (wilfordconine) has good inhibition to leukaemia.Therefore, the angle from Chinese medicine quality control, needs to detect the wilforine content in tripterygium hypoglaucum hutcs raw material in the production of tripterygium hypoglaucum hutcs preparation.
At present, the analyzing detecting method of thunder godvine alkaloid is more, such as fluorescence method, electrochemical process, evaporative light-scattering method etc., the application of especially LC/MS GC-MS, enhance the qualitative detection ability to alkaloid, improve detection sensitivity, in recent years document report also day by day increases, such as in the Tripterygium Oral ultraviolet spectrophotometry detection of TA, wilforine in high efficiency liquid chromatography for separating and determining velamen of Tripterygium wilfordii, also document is had to use Capillary Electrophoresis chromatography to measure wilforine, the and for example Chinese invention patent detection method of wilforine " in a kind of honey " of Application No. 201410402202.9 (application publication number is CN 104407081 A).But, all there are some problems in said method, subject matter is that detecting used pre-treating method for the alkaloid in tripterygium hypoglaucum hutcs rhizome raw material is mostly refluxing extraction, the means such as extraction, therefore relatively low for content or that matrix is relative complex tripterygium hypoglaucum hutcs rhizome material sample, these methods are difficult to meet the demand of actually detected work, how to extract the alkaloid in medicinal material fast and efficiently and carry out content analysis, need to set up a kind of feasible effective analysis method.
Content of the invention
The technical problem to be solved is to provide a kind of extraction efficiency high for prior art, and detection utilizes the method for wilforine content in ion liquid abstraction/HPLC detection tripterygium hypoglaucum hutcs rhizome fast and accurately.
The technical scheme that the present invention solves that above-mentioned technical problem used is: one utilizes the method for wilforine in ion liquid abstraction/HPLC detection tripterygium hypoglaucum hutcs rhizome, it is characterised in that comprise the following steps:
(1) sample extraction: weigh tripterygium hypoglaucum hutcs powder sample and put in the container with stirrer, the ionic liquid solution adding solid-to-liquid ratio to be 1:20～60, microwave radiation exaraction 1～9min under 200～600w microwave power, extracts 1～3 time；
(2) detect: using HPLC to detect, HPLC chromatogram condition is: use Kromasil ODS-C18 post (4mm × 250mm, 5um)；Flowing is acetonitrile-water mutually；Flow velocity is 0.3～0.5ml/min；Detection wavelength is 275nm；Column temperature is 25 DEG C.
The salt that ionic liquid is made up of a kind of nitrogenous heterocyclic organic cation and a kind of inorganic anion, it is in a liquid state at a temperature of room temperature or near room temperature, it is also called greenhouse ionic liquid, room temperature molten salt, organic ion liquid etc., heretofore described ionic liquid solution is mixed by the ionic liquid that volume ratio is 1:3～9 and methyl alcohol, and described ionic liquid is [Bmim] Br (bromination 3-methyl isophthalic acid-butyl imidazole), [Bmim] BF4(1-butyl-3-methyl imidazolium tetrafluoroborate), [Bmim] PF6(1-butyl-3-methylimidazole hexafluoro borate), [Hmim] Br (bromination 1-base-3 methylimidazole), [Hmim] BF4(1-base-3-methylimidazole hexafluorophosphate) and [Hmim] PF6At least one in (1-base-3-methylimidazole hexafluorophosphate).
Compared with doing extraction solution with methyl alcohol, the addition of ionic liquid significantly affects the effect of extracting of Nuciferine in lotus leaf, but the size of impact is relevant with the species of ionic liquid.The strong extracting power that ionic liquid solution is had is relevant with the character of himself, on the one hand, ionic liquid has different kinds of molecules active force and strong solvability, especially Hyarogen-bonding, polarity active force, ionic charge active force etc., these effects contribute to wilforine and dissolve in ionic liquid solution, so that wilforine can be extracted out from thunder godvine rhizome effectively；On the other hand, the organic salt that ionic liquid is made up of organic cation and organic or inorganic anion, there is strong absorption and conversion capability group to microwave, ionic liquid solution can be effectively improved to the absorption of microwave and conversion, solvent and sample is made to be brought rapidly up, therefore, the ionic liquid in described ionic liquid solution is [Bmim] BF4, and [Bmim] BF4Volume ratio with methyl alcohol is 1:9.
As preferably, in described step (1), tripterygium hypoglaucum hutcs powder sample and the solid-to-liquid ratio of ionic liquid solution are 1:50.
As preferably, in described step (1), microwave power is 400w, and extraction time is 5min, and Extracting temperature is 60 DEG C, extracts once.
As preferably, in the flowing phase in described step (2), acetonitrile-water volume ratio is 20:80, and flow velocity is 0.3ml/min.
Compared with prior art, it is an advantage of the current invention that: the present invention utilizes ionic liquid and methyl alcohol are mixed to form ionic liquid solution as extractant, in conjunction with microwave radiation exaraction, avoid target product during wilforine extracts to decompose, the relatively low problem of recovery rate, thus obtain higher extraction efficiency, in conjunction with HPLC detection technique, result display wilforine is good linear relationship in the range of 20～100 μ g/mL, recovery of standard addition is between 88.7%～93.0%, the method is simple to operate, extraction efficiency is high, detection is quick and precisely, can realize rapidly and efficiently detecting the content of wilforine in tripterygium hypoglaucum hutcs rhizome.
Brief description
Fig. 1 be embodiment 1 1-2 in wilforine canonical plotting；
Fig. 2 be embodiment 1 1-2 in wilforine standard items HPLC collection of illustrative plates；
Fig. 3 be embodiment 2 2-1 in the impact on wilforine effect of extracting for the different ionic liquid solution；
Fig. 4 be embodiment 2 2-1 in [Bmim] BF4The HPLC collection of illustrative plates of ionic liquid solution；
Fig. 5 is the impact on wilforine extraction yield for the 2-2 intermediate ion strength of fluid of embodiment 2；
Fig. 6 be embodiment 2 2-3 in the impact on wilforine extraction yield for the different microwave；
Fig. 7 be embodiment 2 2-4 in the impact on wilforine extraction yield for the extraction time；
Fig. 8 be embodiment 2 2-5 in the impact on wilforine extraction yield for the liquid-solid ratio；
Fig. 9 be embodiment 2 2-6 in the impact on wilforine extraction yield for the extraction time.
Detailed description of the invention
Below in conjunction with accompanying drawing embodiment, invention is described in further detail.
Embodiment 1: testing conditions
1-1, HPLC chromatogram condition
HPLC chromatogram condition is: use Kromasil ODS-C18Post (4mm × 250mm, 5um), flowing is acetonitrile-water (20:80) mutually, and every 100ml adds 0.2ml phosphoric acid；Flow velocity: 0.3mL/min；Detection wavelength: 275nm；Column temperature: 25 DEG C.
1-2, the preparation of calibration curve
Precision measures wilforine standard items (medicine inspecting institute of China) 10mg, constant volume is standby in the volumetric flask of 10ml, it is 0.02mg/ml, 0.04mg/ml, 0.06mg/ml, 0.08mg/ml, 0.1mg/ml wilforine standard solution being each configured to concentration, use HPLC method to measure tripterygium hypoglaucum hutcs alkali content in tripterygium hypoglaucum hutcs.With peak area as ordinate, wilforine concentration is that abscissa makes calibration curve.As it is shown in figure 1, wilforine is good linear relationship in the range of 20-100 μ g/mL, regression equation is: y=39111x-21.09, R2=0.9996, wilforine standard items HPLC collection of illustrative plates is as shown in Figure 2.
Embodiment 2: sample extraction
Accurately weigh 1.0g tripterygium hypoglaucum hutcs powder sample (being purchased from shop of Chinese medicines) to be placed in round-bottomed flask, it is subsequently added into ionic liquid solution, put into stirrer, at 70 DEG C (extract equalized temperatures about 70 DEG C during microwave power 400w～600w) in microwave radiation exaraction at present.
2-1, the selection of ionic liquid species
Use VIonic liquid/VMethyl alcohol(1/9) [Bmin] Br, [Bmim] BF4、[Bmim]PF6、[Hmim]Br、[Hmim]BF4、[Hmim]PF66 kinds of ionic liquid solutions are extraction solution, tripterygium hypoglaucum hutcs powder sample is 1:30 with the solid-to-liquid ratio of above-mentioned extraction solution, microwave radiation exaraction 10min under microwave power is 400w, the solution constant volume that extracts of each experimental group gained detects in the volumetric flask of 100ml, and result is as shown in Figure 3.
As can be seen from Figure 3, [Bmim] BF4Other five kinds of ionic liquids are better than to the effect of extracting of wilforine, specifically: to [Bmim] Br, [Bmim] BF with identical cationic structural4、[Bmim]PF6[Hmim] Br, [Hmim] BF4、[Hmim]PF6Two for ionic liquid, and their extraction yield is different, [Bmim] BF4Increase 4.2% than [Bmim] Br, than [Bmim] PF6Increase 19.9%；To [Bmim] Br, [Hmim] Br and [Bmim] BF with identical anion structure4、[Hmim]BF4[Bmim] PF6、[Hmim]PF6Three for ionic liquid, and their extraction yield is different equally, and [Bmim] Br ratio [Hmim] Br increases 9.9%, [Bmim] BF4Than [Hmim] BF4Increase 6.1%, [Bmim] PF6Than [Hmim] PF6Increase 38.3%.It can thus be seen that the extraction yield of wilforine is relevant with the species of the zwitterion of ionic liquid, the magnitude relationship of anion effects is BF4 ->Br-->PF6 -, the magnitude relationship of cation impact is [Bmim]+>[Hmim]+.To sum up, the present embodiment selects [Bmim] BF4For extracting the ionic liquid of wilforine, [Bmim] BF4The HPLC collection of illustrative plates of ion liquid abstraction liquid is as shown in Figure 4.
2-2, the selection of ionic liquid concentration
It is known that different ionic liquid concentration, the extracting power of ionic liquid is also different, therefore by [Bmim] BF of variable concentrations4Wilforine in tripterygium hypoglaucum hutcs is extracted respectively, specifically, respectively with VIonic liquid/V Methyl alcohol[Bmim] BF of 1:3,1:5,1:7,1:9,1:294Ionic liquid solution is extraction solution, and other extraction conditions are: solid-to-liquid ratio 1:30 (g/mL), power 400w, microwave radiation exaraction 5min, result is as shown in Figure 5.
As shown in Figure 5, as ionic liquid concentration (VIonic liquid/VMethyl alcohol) when 1:29 increases to 1:9, with ionic liquid [Bmim] BF4The increase of concentration, the extraction yield of wilforine also substantially increases, and extraction yield increases to 0.37% from 0.286%, adds 29.4%.As ionic liquid concentration (VIonic liquid/VMethyl alcohol) when 1:9 increases to 1:3, with ionic liquid [Bmim] BF4The increase of concentration, the extraction yield of wilforine is significantly reduced, and extraction yield is reduced to 0.275% from 0.37%, decreases 25.7%.Therefore ionic liquid concentration (V is selectedIonic liquid/VMethyl alcohol) 1:9 is optimal extractant.
2-3, the selection of microwave power
In view of the difference of microwave irradiation power, wilforine extraction yield may be different, therefore select wilforine in different microwave power extraction tripterygium hypoglaucum hutcses, study the impact on wilforine extraction yield for the microwave power.Respectively with microwave power 200w, 300w, 400w, 500w, 600w for microwave auxiliary extraction power in the present embodiment, other extraction conditions are: [Bmim] BF4VIonic liquid/VMethyl alcohol(1:9) for extraction solution, with solid-to-liquid ratio as 1:30, extracting 5min, as shown in Figure 6, each extraction power corresponding extract temperature is as shown in table 1 for result.
Table 1 extracts the extract temperature corresponding to power
It will be appreciated from fig. 6 that as microwave power 500w, be increased above other power to the extraction yield of wilforine, extraction yield increases with microwave power and increases；After microwave power increases to a certain degree, wilforine extraction yield reduces with the increase of microwave power, therefore selects 400w for optimal extraction power.
2-4, the selection of extraction time
Owing to microwave technology heats rapidly and efficiently, can extract considerable object in the short time, therefore extraction time is the principal element affecting extraction yield, therefore selects different extraction times to investigate the impact on extraction yield for the extraction time.Selecting 1min, 3min, 5min, 7min, 9min to be extraction time in the present embodiment respectively, other extraction conditions are: microwave power 500w irradiates, with [Bmim] BF4VIonic liquid/VMethyl alcohol(1:9) for extraction solution, with solid-to-liquid ratio as 1:30 (i.e. liquid-solid ratio 30), result is as shown in Figure 7.
As shown in Figure 7, when extraction time increases to 5min from 1min, extraction yield increases over time and increases；When extraction time increases to 9min from 5min, extraction yield increases over time and reduces, and therefore slective extraction time 5min is optimum extraction time.
2-5, the selection of liquid-solid ratio
Respectively with liquid-solid ratio the 20th, the 30th, the 40th, the 50th, 60 [Bmim] BF4For extraction solution, other extraction conditions are: microwave power 500w, extraction time 5min, [Bmim] BF4VIonic liquid/VMethyl alcohol(1:9), result is as shown in Figure 8.
As shown in Figure 8, extraction yield when liquid-solid ratio is 60 is higher than other liquid-solid ratioes, but during liquid-solid ratio 50 slightly below 60, selects liquid-solid ratio 50 to be optimal liquid-solid ratio from extracting cost consideration.
2-6, the selection of extraction time
By above-mentioned 2-1,2-2,2-3,2-4,2-5 can more excellent extraction conditions in the case of not considering extraction time be: [Bmim] BF4VIonic liquid/VMethyl alcohol(1:9) for extraction solution, microwave power 400w, solid-to-liquid ratio are 1:60, extraction 5min, carry out extraction time experiment under this more excellent extraction conditions, extract under identical extraction conditions 1 time respectively, extract 2 times, extract 3 times, result is as shown in Figure 9, as shown in Figure 9, when extracting 1 time, when i.e. extracting one time, extraction yield is higher.
To sum up can obtain, optimum extraction condition is: [Bmim] BF4VIonic liquid/VMethyl alcohol(1:9) for extraction solution, microwave power 400w, solid-to-liquid ratio is 1:60, extracts 5min, extracts once.
Embodiment 3: the rate of recovery and precision test
Under the conditions of above-mentioned optimal microwave abstracting, wilforine in extraction tripterygium hypoglaucum hutcs, retain 7d at room temperature, carry out accurate in the daytime and withinday precision degree experiment.Test once every 2d in 6d, replication 3 times；Measure once every 4h in 12h, replication 3 times.
Each sample repeats sample introduction 5 times respectively in a few days and in the daytime as can be seen from Table 2, record in a few days and day to day precision relative standard deviation, its rate of recovery is between 88.7%-93.0%, and in a few days RSD is respectively the 4.7%th, 4.3% and 3.8%, and RSD is respectively the 4.2%th, 5.1% and 5.9% in the daytime.
Table 2 standard TIANZHU XINGNAO Capsul and precision
Comparative example: microwave abstracting compares with conventional extraction techniques
Microwave-assisted extraction technique, ultrasonic extraction technology and reflux extraction technology extraction wilforine contrast, and comparing result is as shown in table 3.
The data of table 3 microwave abstracting and other abstraction techniques compare
As shown in Table 3, compared with reflux extraction and ultrasonic extraction, microwave abstracting is utilized can to reach higher extraction yield in the short period of time.The extraction yield of reflux extraction 120min is similar to the extraction yield of microwave abstracting 5min, is higher than ultrasonic extraction 9.9%, is higher than reflux extraction 5.01%, has fully demonstrated microwave characteristic fast and efficiently.
Claims (6)
1. the method utilizing wilforine content in ion liquid abstraction/HPLC detection tripterygium hypoglaucum hutcs rhizome, it is characterised in that comprise the following steps:
(1) sample extraction: weigh tripterygium hypoglaucum hutcs powder sample and put in the container with stirrer, the ionic liquid solution adding solid-to-liquid ratio to be 1:20～60, microwave radiation exaraction 1～9min under 200～600w microwave power, extracts 1～3 time；
(2) detect: using HPLC to detect, HPLC chromatogram condition is: use Kromasil ODS-C18 post (4mm × 250mm, 5um)；Flowing is acetonitrile-water mutually, and flow velocity is 0.3～0.5ml/min；Detection wavelength is 275nm；Column temperature is 25 DEG C.
2. utilize the method for wilforine content in ion liquid abstraction/HPLC detection tripterygium hypoglaucum hutcs rhizome as claimed in claim 1, it is characterized in that, described ionic liquid solution is mixed by the ionic liquid that volume ratio is 1:3～9 and methyl alcohol, and described ionic liquid is [Bmim] Br, [Bmim] BF4、[Bmim]PF6[Hmim] Br, [Hmim] BF4、[Hmim]PF6In at least one.
3. utilize the method for wilforine content in ion liquid abstraction/HPLC detection tripterygium hypoglaucum hutcs rhizome as claimed in claim 2, it is characterised in that the ionic liquid in described ionic liquid solution is [Bmim] BF4, and [Bmim] BF4Volume ratio with methyl alcohol is 1:9.
4. the method utilizing wilforine content in ion liquid abstraction/HPLC detection tripterygium hypoglaucum hutcs rhizome as described in claim 1 or 2 or 3, it is characterized in that, in described step (1), tripterygium hypoglaucum hutcs powder sample and the solid-to-liquid ratio of ionic liquid solution are 1:50.
5. the method utilizing wilforine content in ion liquid abstraction/HPLC detection tripterygium hypoglaucum hutcs rhizome as described in claim 1 or 2 or 3, it is characterized in that, in described step (1), microwave power is 400w, and extraction time is 5min, Extracting temperature is 60 DEG C, extracts once.
6. the method utilizing wilforine content in ion liquid abstraction/HPLC detection tripterygium hypoglaucum hutcs rhizome as described in claim 1 or 2 or 3, it is characterized in that, in flowing phase in described step (2), acetonitrile-water volume ratio is 20:80, and flow velocity is 0.3ml/min.
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