CN107941927A - A kind of method of UPLC/Q TOF MS measure lobetyolin content - Google Patents
A kind of method of UPLC/Q TOF MS measure lobetyolin content Download PDFInfo
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Abstract
The invention belongs to Chinese medicines for dynamics field, and in particular to a kind of method of the content of lobetyolin in UPLC/Q TOF MS measure invigorating the spleen prescriptions and Radix Codonopsis extract, comprises the following steps：1) invigorating the spleen prescription or Radix Codonopsis extracting solution are prepared；2) high performance liquid chromatography mass spectrometer separation detection lobetyolin is used；3) with various concentrations lobetyolin and corresponding response peak area mapping, the standard curve of lobetyolin is obtained, sample to be tested peak area reference standard curve is calculated into its lobetyolin's content.The present invention establish using in LC-MS technology for detection Chinese medicine Radix Codonopsis, in invigorating the spleen prescription lobetyolin's content method.This method is quick, sensitive, stability is good, and new reference method is provided for the assay of lobetyolin.
Description
Technical field
The invention belongs to Chinese medicines for dynamics field, and in particular to a kind of UPLC/Q-TOF-MS measure lobetyolin contains
The method of amount.
Background technology
Chinese medicine pharmacokinetics (Pharmacokineties, PK) is applied dynamics principle, Study of Traditional Chinese Medicine active ingredient,
The body absorption (Abosorpton) of active component, simple and compound, distribution (Distribution), metabolism
(Metabolism), drain (Excretion) and the dynamic rule of toxicity (ADME/Tox) and its internal amount-effect, when-effect
Relation, and it is subject to mathematical function a new branch of science of quantitative description.It is to illustrating bioactive components, disclosing Chinese medicine
Scientific meaning, the research to innovation of new drugs of TCM, improving dosage form and prescription component rules for compatibility play highly important
Effect, as an indivisible important component on current modernization of cmm chain, so as to become China's medicine
For the hot spot of dynamics research.Blood concentration method is the classical way of pharmacokinetic, is that calculating pharmacokinetics is most normal
With most accurate assay method, so accurately measure is the vital link of Chinese medicine pharmacokinetic to blood concentration.
Applications of the LC-MS in terms of Chinese medicine pharmacokinetics research is very extensive.
Wu Xiaoxia etc. starts with from huanglian jiedu decoction alkaloids, combination (LC-MS/MS) technology establish measure jateorrhizine,
The method of palmatine, fruitlet blood plasma concentration, and the medicine for being successfully applied to this 3 components huanglian jiedu decoction normal rat body Nei moves
Research is learned, the analysis method that can be used for reference is provided for Chinese medicine compound prescription pharmacokinetic studies.Fourth, which is built, just to be waited using diazepam as internal standard, is adopted
With HPLC-MS/MS technologies, the assay method of tanshinone IIA in Dog Plasma, and the minimum quantitative concentrations of this law are established
For 1ng/ml, it has been fully able to meet requirement of experiment, and sample treatment and continuous mode are easy, are adapted to medicine generation in beasle dog body dynamic
Mechanics study.LI etc. establishes one quickly, and special and sensitive UPLC-MS/MS art analyzing rats take orally sleeve skin glycosides and sleeve skin
Pharmacokinetic parameter after plain (Rhizoma Drynariae extract), the results show, this method meet point of the biologics under FDA is instructed
The pharmacokinetic of analysis standard, sleeve skin glycosides and its active metabolite sleeve skin element can provide for the clinical practice of the rhizome of davallia
One rational reference.Chen Ning etc. establishes the method for Astragaloside content in SPE-HPLC-MS measure rat plasmas, and have studied
Pharmacokinetics and Tissue distribution of the Astragaloside IV in rat body.Yujuan Li application LC-MS/MS quantitative analysis rat serums
The content of atractylenolide Ⅰ and its pharmacokinetics is studied in slurry.Xiao-hua Liu et al. applications UPLC-MS is same
When detect after Oral Administration in Rats astragalus extraction night calycosin glucose glucosides, ononin, calycosin, rest-harrow in blood plasma
II 6 kinds of element, Astragaloside IV, astragaloside components, pharmacokinetic is carried out to every kind of component.Mei-Ling Hou etc. are applied
The content of 6 kinds of active ingredients in 7 kinds of Chinese patent medicine preparations of the UPLC-MS/MS technical research based on three yellow Xiexin Tangs.And compare
Compared with rat oral gavage traditional Chinese medicine monomer Rhein, Chinese herb rhubarb, after the yellow Xiexin Tang of Chinese medicine compound prescription three, the drug metabolism of rheum officinale acid monomers
Dynamic process.Research shows that the absorptivity of the Rhein in Chinese medicine compound prescription and single medicinal material is higher than the absorption of rheum officinale acid monomers
Rate, so as to show that three yellow Xiexin Tang compounds are better than single medicinal material rheum officinale and the knot of monomer Rhein in terms of the absorptivity of Rhein
By.Chinese medicine impurity is more, and measured object concentration or activity are extremely low, few for the sample size of analysis, especially during METHOD FOR CONTINUOUS DETERMINATION,
It is difficult to obtain identical sample once again, workload is very big in addition, because contain a variety of chemical compositions in Chinese medicine, and also it is every kind of
Chemical composition content is low, it is necessary to which substantial amounts of data processing and analysis, these all bring certain difficulty to analysis, also seriously limit
Its development is made, LC-MS chromatographic isolation efficiency height, high sensitivity, high selectivity, eliminate the interference of these factors, promote
The development of Chinese medicine pharmacokinetics.
Gegen qinlian decoction is to be used to treat enterogastric diseases tradition compound.Zhang Y etc. are established using LC-MS technology
It is a kind of to detect Puerarin and the effective method of Daidezin at the same time.And application this method compares gegen qinlian decoction and pueraria lobata carries
Take the pharmacokinetic difference of Puerarin and Daidezin in liquid.The result shows that compared with Gegen Decoction, the Pueraria lobota in gegen qinlian decoction
The absorption efficiency higher of root element and Daidezin, and supersession rate declines.Provided to disclose the Compatibility Law of gegen qinlian decoction
Scientific basis.
Radix Codonopsis is China's tradition rare traditional Chinese medicine,《Pharmacopoeia of People's Republic of China》2010 editions Radix Codonopsis recorded derive from tangerine
3 kinds of stalk section plant, are respectively Radix Codonopsis Codonopsis pliosula (Franch) Nannf, codonopsis pilosula var. modesta
Codoncpsis pilosula Nannf.var.modesta (Nannf) L.T.Shen or radix codonpsis tangshen Codonopisis
The dry root of tangshen Oliv..Radix Codonopsis is sweet in flavor, mild-natured, and returns spleen, lung two pass through, and has tonifying middle-Jiao and Qi, promotes the production of body fluid and the effect of stomach.
Clinically it is mainly used for treating the diseases such as weakness of the spleen and the stomach, the deficiency of qi in middle-jiao, temper virtual loss, consumption of body fluid caused by febrile disease.Chemical composition bag in Radix Codonopsis
Sterols, glycoside, alkaloids and nitrogen containing component, volatile oil component, triterpenes and other constituents are included, also have a variety of human bodies
Necessary inorganic elements and amino acid.Modern pharmacological studies have shown that Radix Codonopsis, which has, adjusts blood glucose, promote hematopoietic function, be depressured, resist
Anoxic, endurance, strengthens immunity of organisms, adjusts a variety of effects such as stomach contraction and antiulcer.Polyacetylene class chemical combination in Radix Codonopsis
Thing lobetyolin is the water soluble ingredient isolated from Radix Codonopsis.There is very well the mucosal lesion caused by ethanol in lobetyolin
Protective effect, be consistent with traditional effect that Radix Codonopsis strengthens the spleen and stomach, be one of active ingredient of Radix Codonopsis protection stomach lining.Can conduct
The index component of Radix Codonopsis quality control.
For invigorating the spleen prescription using invigorating the spleen tonifying Qi as primary efficacy, Radix Codonopsis is clinically common invigorating the spleen medicine.Lobetyolin be from
A kind of polyacetylene class compound isolated in Radix Codonopsis, version in 2010《Chinese Pharmacopoeia》(one) is using lobetyolin as Radix Codonopsis matter
Measure the index component of control.More methods using HPLC-UV, RP-HPLC carry out the content of lobetyolin both at home and abroad at present
Measure.This kind of method needs to carry out cumbersome and complicated pretreatment to Radix Codonopsis, and because it contains a variety of chemical compositions, to it is specific into
The measure of point content brings difficulty.LC-MS technology separation efficiency height, high sensitivity, high selectivity, eliminate these because
The interference of element, excellent technological means is provided for lobetyolin's measure.
The content of the invention
To solve the above problems, the present invention is provided in a kind of UPLC/Q-TOF-MS measure invigorating the spleen prescriptions and Radix Codonopsis extract
The method of the content of lobetyolin.
The method of the content of lobetyolin in the UPLC/Q-TOF-MS measure invigorating the spleen prescriptions of the present invention and Radix Codonopsis extract,
Comprise the following steps：1) invigorating the spleen prescription or Radix Codonopsis extracting solution are prepared；2) High Performance Liquid Chromatography-Mass Spectrometry instrument separation detection is used
Lobetyolin；3) with various concentrations lobetyolin and corresponding response peak area mapping, the standard curve of lobetyolin is obtained, will
Sample to be tested peak area reference standard curve calculates its lobetyolin's content.
Wherein, comprising the concrete steps that for invigorating the spleen prescription extract is prepared：According to weight ratio 1:1:1 weighs radix astragali, Radix Codonopsis, white
Art, with 1：10 solid-liquid ratio adds 50% alcohol reflux and extracts 2 times, and 2 hours, concentration every time is settled to 200ml, and precision is drawn
100 μ L of extracting solution with 50% methanol-water ultrasonic dissolution, are settled to scale, precision is drawn appropriate into 50mL volumetric flasks after cooling
Into import EP pipes, 12000r/min centrifugation 20min, take supernatant supreme sample bottle in right amount.
Wherein, comprising the concrete steps that for Radix Codonopsis extract is prepared：Radix Codonopsis is weighed, with 1：10 solid-liquid ratio adds 50% ethanol and returns
Extraction 2 times is flowed, every time 2 hours；Concentration is settled to 200ml, and precision draws 100 μ L of extracting solution into 50mL volumetric flasks, with
50% methanol-water ultrasonic dissolution, is settled to scale after cooling, precision is drawn in right amount into import EP pipes, 12000r/min centrifugations
20min, takes supernatant supreme sample bottle in right amount.
Wherein, chromatographic condition：
Chromatographic column：Waters BEH C18 columns (2.1 × 50mm, 1.7 μm)；Column temperature：40℃；Mobile phase A：Methanol, B：Contain
There is the aqueous solution of 0.1% formic acid water；Gradient elution：0-1.5min, 60%-80%A；1.5-2min, 80%-60%；Sample room
Balance 3min；Analysis time：2 minutes；Flow velocity is 0.2ml/min；Sample size is 5 μ L；
Mass Spectrometry Conditions：
Electric spray ion source (ESI)；Capillary voltage：2500V；Ion source temperature：100℃；Atomization temperature：100℃；Cone
Hole gas velocity：50L/h；It is atomized gas velocity：800L/h；Detection pattern：Cation；Detect m/z：50-1200.
The common extracting mode of lobetyolin has cold-maceration, decocting method, ethanol refluxing process and ultrasonic extraction.Existing article
The difference of Lobetyolin in Codonopsis content obtained by different extraction processes is investigated.Binding experiment room existence conditions, the present invention use
50% ethanol condensing reflux extracts 2 hours and extracts method twice altogether.
Using acetonitrile as organic phase more than lobetyolin's content detection under high-efficient liquid phase chromatogram condition, pure water is inorganic equality
Type of elution.Acetonitrile is used during prerun of the present invention：Water (78:22、75:25)；Methanol：Water (78:22、75:25)；Isocratic progress
Elution, the peak shape of the lobetyolin as a result obtained is not good enough, after test several with gradient elution mode, obtained by organic phase of methanol
The peak shape of the lobetyolin arrived is preferable, then 0.1% formic acid is added into pure water inorganic phase, it is separated more preferably.Then using methanol,
0.1% formic acid water carries out gradient elution for mobile phase.The present invention aligns, the response of lobetyolin carries out under negative ion mode
Compare, the response under positive ion mode is better than the response under negative ion mode, therefore gathered data in the positive-ion mode.
Since the sensitivity of LC-MS technology is high, so stringent to the processing requirement of sample.Traditional Chinese medicine ingredients are complicated, are
The indissoluble solution material in Chinese medicine is avoided to block chromatographic column, common processing sample method has through miillpore filter impurity removal method or superelevation
Fast centrifugation impurity removal method.Because using mobile phase (methanol-water) processing before sample to be tested sample introduction, in order to avoid flowing phased soln
Material in filter membrane and interference is produced to experimental result, therefore the pretreatment before this study sample sample introduction is using the side of ultracentrifugation
Method removes the impurity in sample.
The present invention establish using in LC-MS technology for detection Chinese medicine Radix Codonopsis, in invigorating the spleen prescription lobetyolin's content side
Method.This method is quick, sensitive, stability is good, and new reference method is provided for the assay of lobetyolin.
Brief description of the drawings
Fig. 1 show lobetyolin's standard curve.
Fig. 2 show mass spectrogram in lobetyolin's standard items, Radix Codonopsis extracting solution, invigorating the spleen prescription.
Fig. 3 show the total ion current figure under invigorating the spleen prescription positive ion mode.
Fig. 4 show the total ion current figure under invigorating the spleen prescription negative ion mode.
Embodiment
Following embodiments are used to illustrate the present invention, but are not limited to the scope of the present invention.
1st, laboratory apparatus：
Medicinal herb grinder：Model 103, Rui'an City Yongli pharmaceutical machine Co., Ltd；
Ultrasonic Intelligent washer：Model DL-360B, the letter Instrument Ltd. in Shanghai；
Electric-heated thermostatic water bath：HWS24 types, the permanent Science and Technology Ltd. in Shanghai one；
/ 10th electronic balances：JJ2000 types, Shuan Jie test equipments factory of Changshu City；
A ten thousandth electronic balance:BSA124S, Sai Duolisi scientific instrument (Beijing) Co., Ltd；
The special ultrapure water machine in laboratory：611 types of Arium, German Sartorius companies
High speed freezing centrifuge：3-30K, German Sigma companies
Rotary Evaporators system:R-215, B Μ CHI companies of Switzerland
Mass spectrograph：Xevo G2-S Q-TOF, Waters, US
Ultra Performance Liquid Chromatography instrument：Waters, US.
2nd, reagent
Radix Codonopsis, radix astragali, Rhizoma Atractylodis Macrocephalae are purchased from Guangdong Tian Cheng prepared slices of Chinese crude drugs Co., Ltd.The inspection of each medicinal material is provided by the said firm
Test report.
Lobetyolin's standard items (traditional Chinese medicine Chemical Co., Ltd. is contained in lot number D-026-130528, Shanghai)
Methanol, acetonitrile are chromatographically pure (Merck, German)
Formic acid Sigma ethanol chromatography ranks.
Embodiment 1 prepares Radix Codonopsis extract
Radix Codonopsis is weighed, with 1：10 solid-liquid ratio adds 50% alcohol reflux extraction 2 times, every time 2 hours；Concentration is settled to
200ml, precision draw 100 μ L of extracting solution into 50mL volumetric flasks, with 50% methanol-water ultrasonic dissolution, quarter are settled to after cooling
Degree, precision are drawn in right amount into import EP pipes, and 12000r/min centrifugation 20min, take supernatant supreme sample bottle in right amount.
Embodiment 2 prepares invigorating the spleen prescription extract
According to weight ratio 1:1:1 weighs radix astragali, Radix Codonopsis, Rhizoma Atractylodis Macrocephalae, with 1：10 solid-liquid ratio adds 50% alcohol reflux extraction 2
Secondary, 2 hours, concentration every time is settled to 200ml, and precision draws 100 μ L of extracting solution into 50mL volumetric flasks, with 50% methanol-water
Ultrasonic dissolution, is settled to scale after cooling, precision is drawn in right amount into import EP pipes, and 12000r/min centrifugation 20min, take supernatant
Appropriate supreme sample bottle.
The preparation of 3 standard curve of embodiment
Precision draw 25,50,100,400,500,800,1000 μ L standard mother liquors, to 10mL volumetric flasks in (write mark exactly
Note), scale is settled to 50% methanol solution respectively, 0.0625 μ g/mL, 0.125 μ g/mL, 0.25 μ g/mL, 1 μ g/ is made
ML, 1.24 μ g/mL, 2 μ g/mL, 2.5 μ g/mL standard solutions.Take and managed in right amount to import EP respectively.12000r/min is centrifuged
20min, takes the supreme sample bottle of supernatant.It is measured with above-mentioned liquid matter condition, and records peak area, using concentration as abscissa, peak
Area is ordinate, obtains standard curve.
Standard solution is progressively diluted and is measured, using the amount of standard items when signal-to-noise ratio S/N=10 and S/N=3 as
Quantitative limit and test limit.
Precision system is operated by aforementioned operation method for lobetyolin's standard items of 6 parts of same concentrations, records every part of Radix Codonopsis alkynes
The peak area of glycosides simultaneously calculates RSD values.
Known sample is prepared, adds 0.25 μ g/mL, 1.24 μ g/mL, 2.5 μ g/mL standard items, each concentration is 3 parts parallel,
Measured with above-mentioned condition, rate of recovery formula (measured amount-addition)/example weight × 100%.
Conclusion：
1. using the concentration of lobetyolin's standard items as abscissa (x-axis), the corresponding peak area of each concentration is ordinate (y
Axis).Lobetyolin's standard curve is drawn using Masslynx 4.1Software and draws regression equation (Fig. 1).Its phase relation
Number is r=0.999503, and linear relationship is good in the range of 0.0625-2.5 μ g/mL.Jian Tu1 lobetyolins standard curve.
2. the quantitative limit and test limit of lobetyolin are respectively with the amount of each standard items when signal-to-noise ratio S/N=10 and S/N=3
For quantitative limit 10ng/mL and test limit 5ng/mL.
3. the precision of lobetyolin
4. the rate of recovery of lobetyolin
| Sequence number | Sample size (μ g) | Addition (μ g) | Measured amount (μ g) | Rate of recovery % |
| 1 | 1 | 0.125 | 1.09±0.02 | 96.9 |
| 2 | 1 | 0.62 | 1.56±0.06 | 96.0 |
| 3 | 1 | 1.25 | 2.13±0.04 | 94.7 |
The screening of 4 mobile phase of embodiment
Eluted using following methods
1)A：Acetonitrile, B：Water (78:22、75:25) isocratic elution；
2)A：Methanol, B：Water (78:22、75:25) isocratic elution；
3)A：Methanol B：Aqueous solution gradient elution containing 0.1% formic acid water.
Conclusion：With A：Methanol, B：Aqueous solution containing 0.1% formic acid water；Gradient elution：0-1.5min, 60%-80%A；
1.5-2min, 80%-60%；Sample room balances 3min；Analysis time：2 minutes；Flow velocity is 0.2ml/min；Sample size is 5 μ L；
The separation of lobetyolin is good, and peak shape is preferable, retention time 0.87min.Jian Tu2 lobetyolins standard items, Radix Codonopsis extracting solution, invigorating the spleen
Mass spectrogram in prescription.
The setting of 5 chromatographic column column temperature of embodiment
Under this experiment investigation room temperature and 35 DEG C, 40 DEG C of column temperatures for the separated influence of compound in compound, compound is normal
The column pressure fluctuation degree of chromatographic column is big compared with 40 DEG C of column temperatures under temperature and 35 DEG C of column temperature, and not as good as 40 DEG C columns of the separating degree of each compound
Separating degree under temperature, therefore the column temperature of chromatographic column is arranged to 40 DEG C.
The screening of 6 prescription extraction conditions of embodiment
Respectively using pure water, 30%, 50%, 70%, 95% ethanol as solvent, condensing reflux extracts 2 hours and carries altogether
Take twice.Extract part is investigated using LC-MS technology.
Conclusion：Material in 50% ethanol extract under positive and negative pattern in total ion current figure is most abundant, therefore selects 50%
Ethanol is as Extraction solvent.See the total ion current figure under Fig. 3,4 lobetyolin's invigorating the spleen prescription positive ion modes.
The experiment of lobetyolin content of the embodiment 7 in the system of determination Radix Codonopsis extracting solution and invigorating the spleen prescription of optimization
Accurate invigorating the spleen prescription, each 100 μ L of Radix Codonopsis extracting solution of drawing is molten with 50% methanol ultrasound into 50mL volumetric flasks respectively
Solution, scale is settled to after cooling.Precision is drawn in right amount into import EP pipes, and 12000r/min, 20min ultracentrifugations, take
Clear supreme sample bottle, parallel 6 parts of samples, are measured with above-mentioned liquid matter condition.
Lobetyolin's content (μ g/mL) in 2 Radix Codonopsis extracting solution of table and invigorating the spleen prescription
Note：I Radix Codonopsis extracting solution II invigorating the spleen prescriptions
The above is only the preferred embodiment of the present invention, it is noted that for the ordinary skill people of the art
For member, without departing from the technical principles of the invention, some improvements and modifications can also be made, these improvements and modifications
Also it should be regarded as protection scope of the present invention.
Claims (4)
1. the method for the content of lobetyolin, its feature in a kind of UPLC/Q-TOF-MS measure invigorating the spleen prescriptions and Radix Codonopsis extract
It is, comprises the following steps：1) invigorating the spleen prescription or Radix Codonopsis extracting solution are prepared；2) using High Performance Liquid Chromatography-Mass Spectrometry instrument point
From detection lobetyolin；3) with various concentrations lobetyolin and corresponding response peak area mapping, the standard of lobetyolin is obtained
Curve, its lobetyolin's content is calculated by sample to be tested peak area reference standard curve.
2. the content of lobetyolin in UPLC/Q-TOF-MS measure invigorating the spleen prescriptions as claimed in claim 1 and Radix Codonopsis extract
Method, it is characterised in that prepare comprising the concrete steps that for invigorating the spleen prescription extract：According to weight ratio 1:1:1 weigh radix astragali, Radix Codonopsis,
Rhizoma Atractylodis Macrocephalae, with 1：10 solid-liquid ratio adds 50% alcohol reflux and extracts 2 times, and 2 hours, concentration every time is settled to 200ml, and precision is inhaled
100 μ L of extracting solution are taken into 50mL volumetric flasks, with 50% methanol-water ultrasonic dissolution, scale are settled to after cooling, precision is drawn suitable
For amount into import EP pipes, 12000r/min centrifugation 20min, take supernatant supreme sample bottle in right amount.
3. the content of lobetyolin in UPLC/Q-TOF-MS measure invigorating the spleen prescriptions as claimed in claim 1 and Radix Codonopsis extract
Method, it is characterised in that prepare comprising the concrete steps that for Radix Codonopsis extract：Radix Codonopsis is weighed, with 1：10 solid-liquid ratio adds 50% second
Alcohol reflux extracts 2 times, 2 hours every time；Concentration is settled to 200ml, and precision draws 100 μ L of extracting solution into 50mL volumetric flasks,
With 50% methanol-water ultrasonic dissolution, scale is settled to after cooling, precision is drawn in right amount into import EP pipes, 12000r/min centrifugations
20min, takes supernatant supreme sample bottle in right amount.
4. the content of lobetyolin in UPLC/Q-TOF-MS measure invigorating the spleen prescriptions as claimed in claim 1 and Radix Codonopsis extract
Method, it is characterised in that：
Chromatographic condition：
Chromatographic column：Waters BEH C18 columns (2.1 × 50mm, 1.7 μm)；Column temperature：40℃；Mobile phase A：Methanol, B：Contain
The aqueous solution of 0.1% formic acid water；Gradient elution：0-1.5min, 60%-80%A；1.5-2min, 80%-60%；Sample room is put down
Weigh 3min；Analysis time：2 minutes；Flow velocity is 0.2ml/min；Sample size is 5 μ L；
Mass Spectrometry Conditions：
Electric spray ion source (ESI)；Capillary voltage：2500V；Ion source temperature：100℃；Atomization temperature：100℃；Taper hole gas
Speed：50L/h；It is atomized gas velocity：800L/h；Detection pattern：Cation；Detect m/z：50-1200.
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| CN109470792B (en) * | 2018-12-13 | 2021-06-18 | 重庆医科大学 | HPLC method for simultaneously determining eight active ingredients in codonopsis pilosula |
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