CN104330516A - Method for simultaneously determining content of allantoin and adenosine in Chinese yams - Google Patents
Method for simultaneously determining content of allantoin and adenosine in Chinese yams Download PDFInfo
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- CN104330516A CN104330516A CN201410697800.3A CN201410697800A CN104330516A CN 104330516 A CN104330516 A CN 104330516A CN 201410697800 A CN201410697800 A CN 201410697800A CN 104330516 A CN104330516 A CN 104330516A
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Abstract
The invention discloses a method for simultaneously determining the content of allantoin and adenosine in Chinese yams. The method comprises the following steps: producing a comparison product standard curve, and pre-treating and determining Chinese yam samples to be detected, specifically, carrying out the pretreatment of the samples to be detected, namely carrying out ultrasonic extraction on the Chinese yam samples with a methanol water solution with the concentration (v/v) being 20%-60% for 20-40 minutes; uniformly shaking and putting part of an extracting solution into a centrifugal tube, and centrifuging; and sucking liquid supernatant and filtering the liquid supernatant with a filter membrane to obtain a solution of the samples to be detected; determining the Chinese yam samples to be detected by adopting a liquid chromatography-tandem mass spectrometry method. The method combines the advantages of chromatography and mass spectrometry and has the advantages of strong specificity and high sensitivity; and the aims of identifying and controlling the quality are simultaneously achieved and reference evidence is provided for quality control of the Chinese yams and decoction pieces thereof.
Description
Technical field
The present invention relates to a kind of method of Simultaneously test allantoin in dried rhizoma of Dioscorea opposita and adenosine content.
Background technology
Chinese yam, another name RHIIZOMA DIOSCOREAE from Henan of China, Chinese yam rhizome, be called for short Huai Shan, for the dry rhizome of Dioscoreaceae plant Chinese yam, be medicine-food two-purpose resource, have tonifying kidney and nourishing stomach, promote the production of body fluid beneficial lung, effect of the puckery essence of kidney tonifying, is the principal ingredient of the Chinese medicines such as Liuwei Dihuang Wan, the Pill of Anemarrhena, Phellodendrom and Rehmannia, Diaoxinxue Kang, and is widely used in all kinds of Chinese medicine preparation.2010 editions " Chinese Pharmacopoeias " record yam variety, the quality control of Chinese yam and medicine materical crude slice thereof are only limitted to the detections such as conventional moisture, ash content and extract, are unfavorable for Chinese yam application clinically and popularization.
Allantoin and adenosine are one of principal ingredients of Chinese yam, and the synthesis etc. of adenosine compounds to sugar and fatty metabolism, nucleic acid and protein plays important regulating action.Pharmacological research shows, the physiologically actives such as adenosine has vasodilator, reduces blood pressure, decreasing heart rate, Antiaggregating activity on platelet, lax vascular smooth muscle, also have triggering or mediate ischemia pre-adaptation, alleviate the Cardioprotective application such as reperfusion injury; It is closely related that allantoin has the effect of repairing the epithelial tissue promotion effect such as skin ulcer and wound healing myogenic and Chinese yam.Therefore allantoin and adenosine have great effect in the quality control of Chinese yam and medicine materical crude slice thereof.
The assay of current allantoin mainly concentrates on thin-layered chromatography, infra-red chromatography, capillary electrophoresis, high performance liquid chromatography etc., but in Chinese yam, be rich in polysaccharide, starchy material, the mensuration of easy jamming target composition, therefore in current detection method, the pre-treatment of testing sample is more complicated, specificity is poor, and sensitivity is low.
Summary of the invention
For the problems referred to above, the object of the present invention is to provide a kind of method adopting Liquid Chromatography-Tandem Mass Spectrometry to be separated also Fast Measurement allantoin in dried rhizoma of Dioscorea opposita and adenosine content, high specificity, highly sensitive, the object of qualification and quality control can be reached, for the quality control of Chinese yam and medicine materical crude slice thereof provides reference frame simultaneously.
Technical scheme provided by the invention is:
A kind of method of Simultaneously test allantoin in dried rhizoma of Dioscorea opposita and adenosine content, comprise the making of reference substance typical curve, the pre-treatment of Chinese yam testing sample and mensuration, wherein the pre-treatment of testing sample is: the methanol aqueous solution being 20%-60% by Chinese yam sample concentration (v/v) carries out ultrasonic extraction 20-40min, get extracting section liquid after shaking up centrifugal to centrifuge tube, after Aspirate supernatant, adopt membrane filtration to obtain testing sample solution; The mensuration of described Chinese yam testing sample adopts liquid chromatography tandem mass spectrometry.
Preferably, described Simultaneously test allantoin in dried rhizoma of Dioscorea opposita and the method for adenosine content, wherein,
The making of typical curve: by drying under reduced pressure to the allantoin of weight and adenosine reference substance, add the methanol aqueous solution identical with the concentration that testing sample pre-treatment uses and prepare that the reference substance of variable concentrations is mixed marks solution, Liquid Chromatography-Tandem Mass Spectrometry method is adopted to measure, wherein allantoin adopts positive ion mode, adenosine adopts negative ion mode, with the chromatographic peak area of allantoin or adenosine for ordinate, its corresponding concentration is that horizontal ordinate carries out linear regression production standard curve;
The mensuration of Chinese yam testing sample: by testing sample through pre-treatment, measured by Liquid Chromatography-Tandem Mass Spectrometry method, wherein allantoin adopts positive ion mode, adenosine adopts negative ion mode, draw the chromatographic peak area of allantoin or adenosine, substitute into the content that typical curve calculates allantoin and adenosine in Chinese yam testing sample.
Preferably, described Simultaneously test allantoin in dried rhizoma of Dioscorea opposita and the method for adenosine content, the chromatographic condition that described liquid chromatography tandem mass spectrometry measures comprises: chromatographic column: Pursuit C182.0*100mm, 3.0 μm; Column temperature: 30 DEG C; Mobile phase is first alcohol and water, isocratic elution, and analysis time is 8min, and wherein said mobile phase volume is than being methyl alcohol: water=10: 90, and flow velocity is 0.20ml/min; Sample size: 3 μ l.
Preferably, described Simultaneously test allantoin in dried rhizoma of Dioscorea opposita and the method for adenosine content, the Mass Spectrometry Conditions that described liquid chromatography tandem mass spectrometry measures comprises: electric spray ion source (ESI); Detecting device capillary voltage 1.3kV; Electron spray voltage 5kV; Ion source temperature 50 DEG C; Desolventizing temperature degree 300 DEG C; Dry gas pressure 20psi; Atomization gas pressure 50psi; Reaction of high order monitoring (MRM) pattern measures; Positive and negative ion switched scan pattern is adopted to test, wherein allantoin adopts positive ion mode, monitoring parent ion is m/z 156.7, daughter ion is 113.6 and 96.6, and capillary voltage is-45V, and collision energy is respectively 10.5V and 13.0V, adenosine adopts negative ion mode, monitoring parent ion is m/z 268.2, and daughter ion is 135.9 and 252.7, and capillary voltage is 55V; Collision energy is respectively 16.0V and 5.0V.
Preferably, described Simultaneously test allantoin in dried rhizoma of Dioscorea opposita and the method for adenosine content, in the pre-treatment of described testing sample, every 1 Keshan medicine sample add 20ml concentration (v/v) be 40% methanol aqueous solution carry out ultrasonic extraction.
Preferably, described Simultaneously test allantoin in dried rhizoma of Dioscorea opposita and the method for adenosine content, described ultrasonic extraction time is 1 time, and ultrasonic extraction time is 30min.
Preferably, described Simultaneously test allantoin in dried rhizoma of Dioscorea opposita and the method for adenosine content, described centrifugal rotating speed is 10000r/min, and centrifugation time is 10min.
Preferably, described Simultaneously test allantoin in dried rhizoma of Dioscorea opposita and the method for adenosine content, described membrane filtration is 0.22 μm of filtering with microporous membrane.
The method of Simultaneously test allantoin in dried rhizoma of Dioscorea opposita of the present invention and adenosine content, liquid chromatography is connected with mass spectrum and uses, have that separating power is strong, high specificity, highly sensitive feature, the object of qualification and quality control can be reached simultaneously, compare high performance liquid chromatography, the pre-treating method of testing sample of the present invention is simple, quick, has following beneficial effect:
(1) pre-treatment of testing sample of the present invention adopts ultrasound wave to extract, simple to operate, the time is short, adopt 20ml concentration (v/v) be 40% methanol aqueous solution as extraction agent time, use that once ultrasonic extraction 30min extraction efficiency is the highest;
(2) the present invention is by the testing sample solution centrifugal 10min under the rotating speed of 10000r/min after ultrasonic, and the large molecules such as the starch in Chinese yam are fully precipitated, and improves the anti-interference that testing sample solution carries out when Liquid Chromatography-Tandem Mass Spectrometry measures;
(3) adopt 0.22 μm of filtering with microporous membrane, filter fine particle, prevent entering pillar and result in blockage and damage mass spectrum;
(4) assay method of the present invention is highly sensitive, and the detectability detecting allantoin and adenosine is respectively 0.002,0.006 μ g/ml, and quantitative limit is respectively 0.015,0.080 μ g/ml.
Accompanying drawing explanation
Fig. 1 is the allantoin standard items chromatogram that reaction monitoring pattern (MRM) of the present invention mensuration obtains;
Fig. 2 is the adenosine standard items chromatogram that multiple-reaction monitoring pattern (MRM) of the present invention mensuration obtains;
Fig. 3 is adenosine and allantoin chromatogram in the yam extract that obtains of multiple-reaction monitoring pattern (MRM) mensuration of the present invention;
Fig. 4 is allantoin typical curve of the present invention;
Fig. 5 is adenosine typical curve of the present invention.
Embodiment
Below in conjunction with accompanying drawing, the present invention is described in further detail, can implement according to this with reference to instructions word to make those skilled in the art.
The invention provides a kind of method of Simultaneously test allantoin in dried rhizoma of Dioscorea opposita and adenosine content, comprise the following steps:
(1) making of typical curve: by drying under reduced pressure to the allantoin of weight and adenosine reference substance, add concentration (v/v) be 40% methanol aqueous solution be mixed with every 1ml and contain the mixed mark solution that 150.0 μ g allantoins and every 1ml contain 20.0 μ g adenosines, be diluted to the mixed mark solution of variable concentrations as required, it is first separated allantoin and adenosine by liquid chromatography, again through mass spectroscopy, wherein allantoin adopts positive ion mode, adenosine adopts negative ion mode, with the chromatographic peak area Y of allantoin or adenosine for ordinate, its corresponding concentration X is that horizontal ordinate carries out linear regression production standard curve, and investigate linear relationship, obtain typical curve respectively as Fig. 4 and Fig. 5, typical curve, the range of linearity, related coefficient, quantitative limit and detectability are in table 1,
The typical curve of table 1 allantoin and adenosine, the range of linearity, related coefficient, quantitative limit and detectability
(2) pre-treatment of Chinese yam testing sample and mensuration: get Chinese yam sample powder 1g in 25ml volumetric flask, adding 20ml concentration (v/v) is the methanol aqueous solution of 40%, once be settled to 25ml after ultrasonic extraction 30min, shake up, get extracting section liquid to centrifuge tube, centrifugal rotational speed is 10000r/min, centrifugation time is 10min, Aspirate supernatant obtains testing sample solution through 0.22 μm of filtering with microporous membrane, first it is separated allantoin wherein and adenosine by liquid chromatography, again through mass spectroscopy, wherein allantoin adopts positive ion mode, adenosine adopts negative ion mode, draw the chromatographic peak area of allantoin or adenosine, substitute into the content that typical curve calculates allantoin and adenosine in Chinese yam testing sample.
(3) condition determination:
Chromatographic condition: Pursuit C182.0*100mm, 3.0 μm; Column temperature: 30 DEG C; Mobile phase is first alcohol and water, isocratic elution 8min, and wherein said mobile phase volume is than being methyl alcohol: water=10: 90, and flow velocity is 0.20ml/min; Sample size: 3 μ l;
Mass Spectrometry Conditions: electric spray ion source (ESI); Detecting device capillary voltage 1.3kV; Electron spray voltage 5kV; Ion source temperature 50 DEG C; Desolventizing temperature degree 300 DEG C; Dry gas pressure 20psi; Atomization gas pressure 50psi; Reaction of high order monitoring pattern measures; Positive and negative ion switched scan pattern is adopted to test, wherein allantoin adopts positive ion mode, allantoin parent ion is m/z 156.7, daughter ion is 113.6 and 96.6, and go bunch voltage to be-45V, collision energy is respectively 10.5V and 13.0V, adenosine adopts negative ion mode, adenosine parent ion is m/z 268.2, and daughter ion is 135.9 and 252.7, goes bunch voltage to be 55V; Collision energy is respectively 16.0V and 5.0V.
(4) data analysis:
The chromatogram of the standard items allantoin (RT=1.41) that multiple-reaction monitoring pattern (MRM) measures and adenosine (RT=5.22), as depicted in figs. 1 and 2; The chromatogram of allantoin (RT=1.41) and adenosine (RT=5.22) in the yam extract that multiple-reaction monitoring pattern (MRM) measures, as shown in Figure 3.Allantoin in yam extract and adenosine can be differentiated by contrasting with the allantoin and adenosine of standard.
According to table 1, Fig. 1, Fig. 2 and Fig. 3, the chromatographic peak degree of separation that the Liquid Chromatography-Tandem Mass Spectrometry adopted detects allantoin and adenosine is good, high specificity, and has good linear correlation between its corresponding concentration of chromatographic peak area.Allantoin, the adenosine content of the present embodiment Chinese yam sample are respectively 3.97mg/g, 0.105mg/g.
(4) recovery test
Test adopts standard addition method to carry out recovery experiment, take the Chinese yam sample 1.0g of 9 parts of known content, add allantoin, the adenosine standard items of high, medium and low difference amount respectively, testing sample solution is prepared according to pre-treating method, measure and calculate the recovery by above-mentioned chromatographic condition sample introduction, in table 2.The average recovery of allantoin is 97.4% ~ 103.3%, and the average recovery of adenosine is 98.1 ~ 103.1.Test findings shows that set up method has higher accuracy for the content of Simultaneously test allantoin in dried rhizoma of Dioscorea opposita and adenosine.
The average recovery of table 2 allantoin and adenosine
Although embodiment of the present invention are open as above, but it is not restricted to listed in instructions and embodiment utilization, it can be applied to various applicable the field of the invention completely, for those skilled in the art, can easily realize other amendment, therefore do not deviating under the universal that claim and equivalency range limit, the present invention is not limited to specific details and illustrates here and the legend described.
Claims (8)
1. the method for a Simultaneously test allantoin in dried rhizoma of Dioscorea opposita and adenosine content, it is characterized in that, comprise the making of reference substance typical curve, the pre-treatment of Chinese yam testing sample and mensuration, wherein the pre-treatment of testing sample is: the methanol aqueous solution being 20%-60% by Chinese yam sample concentration (v/v) carries out ultrasonic extraction 20-40min, get extracting section liquid after shaking up centrifugal to centrifuge tube, after Aspirate supernatant, adopt membrane filtration to obtain testing sample solution; The mensuration of described Chinese yam testing sample adopts liquid chromatography tandem mass spectrometry.
2. the method for Simultaneously test allantoin in dried rhizoma of Dioscorea opposita as claimed in claim 1 and adenosine content, is characterized in that, wherein,
The making of typical curve: by drying under reduced pressure to the allantoin of weight and adenosine reference substance, add the methanol aqueous solution identical with the concentration that testing sample pre-treatment uses and prepare that the reference substance of variable concentrations is mixed marks solution, Liquid Chromatography-Tandem Mass Spectrometry method is adopted to measure, wherein allantoin adopts positive ion mode, adenosine adopts negative ion mode, with the chromatographic peak area of allantoin or adenosine for ordinate, its corresponding concentration is that horizontal ordinate carries out linear regression production standard curve;
The mensuration of Chinese yam testing sample: by testing sample through pre-treatment, measured by Liquid Chromatography-Tandem Mass Spectrometry method, wherein allantoin adopts positive ion mode, adenosine adopts negative ion mode, draw the chromatographic peak area of allantoin or adenosine, substitute into the content that typical curve calculates allantoin and adenosine in Chinese yam testing sample.
3. the method for Simultaneously test allantoin in dried rhizoma of Dioscorea opposita as claimed in claim 2 and adenosine content, is characterized in that, the chromatographic condition that described liquid chromatography tandem mass spectrometry measures comprises: chromatographic column: Pursuit C182.0*100mm, 3.0 μm; Column temperature: 30 DEG C; Mobile phase is first alcohol and water, isocratic elution, and analysis time is 8min, and wherein said mobile phase volume is than being methyl alcohol: water=10: 90, and flow velocity is 0.20ml/min; Sample size: 3 μ l.
4. the method for Simultaneously test allantoin in dried rhizoma of Dioscorea opposita as claimed in claim 3 and adenosine content, is characterized in that, the Mass Spectrometry Conditions that described liquid chromatography tandem mass spectrometry measures comprises: electric spray ion source (ESI); Detecting device capillary voltage 1.3kV; Electron spray voltage 5kV; Ion source temperature 50 DEG C; Desolventizing temperature degree 300 DEG C; Dry gas pressure 20psi; Atomization gas pressure 50psi; Reaction of high order monitoring (MRM) pattern measures; Positive and negative ion switched scan pattern is adopted to test, wherein allantoin adopts positive ion mode, monitoring parent ion is m/z 156.7, daughter ion is 113.6 and 96.6, and capillary voltage is-45V, and collision energy is respectively 10.5V and 13.0V, adenosine adopts negative ion mode, monitoring parent ion is m/z268.2, and daughter ion is 135.9 and 252.7, and capillary voltage is 55V; Collision energy is respectively 16.0V and 5.0V.
5. the method for Simultaneously test allantoin in dried rhizoma of Dioscorea opposita as claimed in claim 4 and adenosine content, it is characterized in that, in the pre-treatment of described testing sample, every 1 Keshan medicine sample add 20ml concentration (v/v) be 40% methanol aqueous solution carry out ultrasonic extraction.
6. the method for Simultaneously test allantoin in dried rhizoma of Dioscorea opposita as claimed in claim 4 and adenosine content, it is characterized in that, described ultrasonic extraction time is 1 time, and ultrasonic extraction time is 30min.
7. the method for Simultaneously test allantoin in dried rhizoma of Dioscorea opposita as claimed in claim 4 and adenosine content, it is characterized in that, described centrifugal rotating speed is 10000r/min, and centrifugation time is 10min.
8. the method for Simultaneously test allantoin in dried rhizoma of Dioscorea opposita as claimed in claim 4 and adenosine content, it is characterized in that, described membrane filtration is 0.22 μm of filtering with microporous membrane.
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Cited By (5)
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| CN107349216A (en) * | 2017-07-29 | 2017-11-17 | 河南中医药大学 | Application of the adenosine in estrogen drugs are prepared |
| CN108414638A (en) * | 2018-03-24 | 2018-08-17 | 厦门市诚安毅科技有限公司 | The detection method of active constituent in a kind of quick detection common yam rhizome powder |
| CN109839470A (en) * | 2019-02-25 | 2019-06-04 | 亚宝药业贵阳制药有限公司 | A kind of thin-layer identification method of invigorating the spleen gel products |
| CN111559979A (en) * | 2020-06-12 | 2020-08-21 | 劲牌有限公司 | Method for preparing allantoin by Prep-HPLC method |
| CN115015452A (en) * | 2022-06-07 | 2022-09-06 | 山东宏济堂制药集团股份有限公司 | Method for determining content of allantoin and adenosine in Chinese yam by adopting one-test-multiple-evaluation method |
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Cited By (6)
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|---|---|---|---|---|
| CN107349216A (en) * | 2017-07-29 | 2017-11-17 | 河南中医药大学 | Application of the adenosine in estrogen drugs are prepared |
| CN108414638A (en) * | 2018-03-24 | 2018-08-17 | 厦门市诚安毅科技有限公司 | The detection method of active constituent in a kind of quick detection common yam rhizome powder |
| CN109839470A (en) * | 2019-02-25 | 2019-06-04 | 亚宝药业贵阳制药有限公司 | A kind of thin-layer identification method of invigorating the spleen gel products |
| CN111559979A (en) * | 2020-06-12 | 2020-08-21 | 劲牌有限公司 | Method for preparing allantoin by Prep-HPLC method |
| CN115015452A (en) * | 2022-06-07 | 2022-09-06 | 山东宏济堂制药集团股份有限公司 | Method for determining content of allantoin and adenosine in Chinese yam by adopting one-test-multiple-evaluation method |
| CN115015452B (en) * | 2022-06-07 | 2023-11-17 | 山东宏济堂制药集团股份有限公司 | Method for measuring content of allantoin and adenosine in Chinese yam by adopting one-measurement-multiple-evaluation method |
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Granted publication date: 20160504 Termination date: 20161126 |