CN109580849A - A kind of method of index ingredient in measurement traditional Chinese medicine oral liquid - Google Patents
A kind of method of index ingredient in measurement traditional Chinese medicine oral liquid Download PDFInfo
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Abstract
The invention discloses a kind of methods of index ingredient in measurement traditional Chinese medicine oral liquid, include the following steps: that sample solution imports adjustable current divider after liquid chromatogram separates, efflux is divided into two-way: connecting all the way with ionic migration spectrometer, electro-spray ionization occurs under spray voltage effect, the ion of formation enters in the migration tube of ionic migration spectrometer separated after, eventually arrive at Faraday cup detector and detect to obtain corresponding test map；Another way efflux enters triple quadrupole mass spectrometer, and the signal of determinand is acquired under multiple-reaction monitoring pattern, makees further confirmation to the testing result of ionic migration spectrometer.The method that the present invention measures index ingredient in traditional Chinese medicine oral liquid uses liquid chromatogram-electrospray ionisation-ion mobility spectrometry joint technology, provides scientific and effective technological means for the control of Chinese materia medica preparation quality and active component detection.
Description
Technical field
The present invention relates to a kind of detection methods of chemical substance, more particularly to a kind of using liquid chromatogram-electron spray electricity
From 7 kinds of index ingredients in-ion mobility spectrometry method for combined use measurement traditional Chinese medicine oral liquid.
Background technique
Chinese medicine is the important component of China's traditional medicine, is the important tool of disease preventing and treating.According to incompletely statistics, mesh
There is a countries and regions sale Chinese medicine more than 130 in the preceding whole world, and the population of nearly a quarter uses Chinese medicine in the world.Chinese materia medica preparation be with
Traditional Chinese medical theory is guidance, using Chinese medicine as raw material, is made into certain dosage form according to prescription and directly uses for clinical, to reach most
Play to limits the purpose of curative effect of medication.Active ingredient of Chinese herbs is the key that guarantee clinical efficacy, and quality control is especially heavy
It wants.Establish Chinese materia medica preparation index components analyzing detecting method can for Chinese materia medica preparation quality control provide safeguard, while be also in
Medicine modernization, international key.
Ion mobility spectrometry is a kind of to utilize the difference that the gaseous ion of formation migration rate in the electric field is ionized under atmospheric pressure
Come the analytical technology for being separated and being characterized to chemical substance, illicit drugs inspection, public safety, food peace have been widely used in it
Entirely, the related fieldss such as environmental monitoring.The basic principle of ion mobility spectrometry is that sample to be tested is ionized in ionization reaction area, is generated
Ion under electric field power drive, drift region is entered by the ion gate periodically opened, with reverse neutral drift gas point
Son constantly collides, so that the ion with different mobilities is separated and successively reaches detecting electrode.In Ion transfer
In spectrometry, first has to generate gaseous ion and then just can be carried out the separation and detection of product ion.Ion mobility spectrometry is existing
Ionization mode includes isotopic ion, corona discharge ionization, photo-ionization, flame ion, electro-spray ionization
Deng.Wherein, the appearance in electrospray ionisation source, analyzes ion mobility spectrometry directly to fluid sample.Electron spray electricity
From the important method for having become using ion mobility spectrometry measurement biomolecule and carrying out Analysis of environmental samples.
Although ion mobility spectrometry has many advantages, such as simple portable, low in cost, rapid sensitive, separating capacity is limited,
In the case that sample substrate is complex, it is understood that there may be unable to satisfy multicomponent while separating demand, different in ionization process
The problems such as ionization Competitive assays are generated between substance.
Summary of the invention
The technical problem to be solved in the present invention is to provide index ingredients in a kind of traditional Chinese medicine oral liquid of measurement easily to operate
Method.
Ion mobility spectrometry and liquid chromatogram are combined by electrospray interface, detection of the ion mobility spectrometry as liquid chromatogram
Device, the obtained ion transfer spectrogram of measurement chromatographic isolation effluent, thus based on chromatography hydrophobic difference before ionizing and from
After sonization while ionic mobility difference realize chromatography two dimensional separation, for complex compound precise Identification provide it is more rich
Rich chemical information, enhances the break-up value of ion mobility spectrometry.Meanwhile ion mobility spectrometry is to carry out under normal pressure to gas ion
Analysis rather than high vacuum condition needed for mass spectrum, convenient place associated with liquid chromatogram and ion mobility spectrometry are between the two
Interface arrangement is simple.
The method of index ingredient, includes the following steps: in a kind of measurement traditional Chinese medicine oral liquid
Sample solution imports adjustable current divider after liquid chromatogram separates, and efflux is divided into two-way: all the way with ion
Under spray voltage effect electro-spray ionization occurs for mobility spectrometer connection, and the ion of formation enters moving for ionic migration spectrometer
Faraday cup detector is eventually arrived at after being separated in shifting pipe to detect to obtain corresponding test map；Another way efflux enters three
Weight quadrupole mass spectrometer, acquires the signal of determinand under multiple-reaction monitoring pattern, makees to the testing result of ionic migration spectrometer
Further confirmation.
The method of index ingredient in measurement traditional Chinese medicine oral liquid of the present invention, wherein use liquid chromatogram-EFI
Mist-ion mobility spectrometry is combined experimental provision, and described device includes ionic migration spectrometer, adjustable current divider, ultra high efficiency liquid phase
Chromatograph and triple quadrupole mass spectrometer, wherein the inlet end of the adjustable flow distributing device and the ultra performance liquid chromatography
The liquid outlet of instrument is connected, the liquid outlet end of the adjustable flow distributing device respectively with the ionic migration spectrometer and the triple quadrupole
The mass spectrometric inlet end of bar is connected.
The method of index ingredient in measurement traditional Chinese medicine oral liquid of the present invention, wherein the index ingredient is pellet
Ginseng element, chlorogenic acid, glycyrrhizic acid, rutin, scutelloside, Gastrodin and Puerarin, totally 7 kinds.
The method of index ingredient in measurement traditional Chinese medicine oral liquid of the present invention, wherein described adjustable point of setting
The split ratio for flowing device is 50:1, the low flow velocity liquid outlet end of the adjustable flow distributing device and the inlet of the ionic migration spectrometer
End is connected, and the high flow rate liquid outlet end of the adjustable flow distributing device is connected with the inlet end of the triple quadrupole mass spectrometer.
The method of index ingredient in measurement traditional Chinese medicine oral liquid of the present invention, wherein the ionic migration spectrometer
Sample introduction flow velocity is about 1 μ L/min, and exact numerical is 0.98 μ L/min.
The method of index ingredient in measurement traditional Chinese medicine oral liquid of the present invention, wherein liquid chromatogram separation condition are as follows:
Chromatographic column: ACQUITY UPLC BEH C18, 50mm × 1mm, 1.7 μm；Flow velocity: 50 μ L/min；Mobile phase A is
0.5% aqueous formic acid, B are acetonitrile；Gradient elution program: 0~3min, 5%B~10%B；3~10min, 10%B~80%
B；10~12min, 80%B；12~12.1min, 80%B~5%B；12.1~15min, 5%B；Column temperature: 25 DEG C；Sample room temperature
Degree: 20 DEG C；Sample volume: 5 μ L.
The method of index ingredient in measurement traditional Chinese medicine oral liquid of the present invention, wherein the ionic migration spectrometer
Analysis condition are as follows:
Electron spray voltage: 2400V；Ionization mode: negative ion mode；Migrate tube voltage: 8000V；Migration tube temperature:
190℃；Gas preheater temperature: 190 DEG C；Migrate spectrum width: 26ms；Bradbury-Nielsen ion gatewidth: 110 μ
s；Bradbury-Nielsen ion gate voltage: 37V；Drift about gas velocity: 1.4L/min；Exhaust pump pumping speed: 1.0L/min.
The method of index ingredient in measurement traditional Chinese medicine oral liquid of the present invention, wherein mass spectral analysis condition is as follows:
Electric spray ion source negative ion mode；Capillary voltage: 2.8kV；Radio-frequency lens voltage: 0.3kV；Ion source temperature
Degree: 150 DEG C；Desolvation temperature: 500 DEG C；Desolventizing gas flow: 800L/h；Taper hole throughput: 50L/h；Photoelectric multiplier electricity
Pressure: 650V；Collision gas: argon gas；Collide air pressure: 0.32Pa.
The method of index ingredient in measurement traditional Chinese medicine oral liquid of the present invention, wherein the mass spectral analysis of 7 kinds of determinands
Parameter is as follows:
The mass spectrometry parameters of 17 kinds of determinands of table
* with the ion of higher response.
The method difference from prior art that the present invention measures index ingredient in traditional Chinese medicine oral liquid is: the present invention surveys
The method of index ingredient in traditional Chinese medicine oral liquid is determined using liquid chromatogram-electrospray ionisation-ion mobility spectrometry joint technology, is established
In traditional Chinese medicine oral liquid danshensu, glycyrrhizic acid, Gastrodin, chlorogenic acid, Puerarin, scutelloside, rutin etc. 7 kinds representative indexs at
The analysis method divided, and optimize liquid chromatogram, spray voltage, migration tube and gas pre-heating temperature, drift gas velocity equal part
Parameter is analysed, while establishing the liquid chromatography-tandem mass spectrometry confirmation method of index ingredient, is controlled for Chinese materia medica preparation quality and living
Property composition detection provides scientific and effective technological means.The detection of 7 kinds of Chinese medicine index ingredients is limited to 2~10 μ g/mL, quantitative
It is limited to 5~25 μ g/mL.
The method of index ingredient in measurement traditional Chinese medicine oral liquid of the invention is described further with reference to the accompanying drawing.
Detailed description of the invention
Fig. 1 is that liquid chromatogram-electron spray-ion mobility spectrometry is combined experimental provision and flow diagram in the present invention；
Fig. 2 is the ion transfer spectrogram of 7 kinds of determinands in the present invention；
Fig. 3 is the Salbutamol Selected Ion Monitoring chromatogram of 7 kinds of determinands in the present invention；
Fig. 4 is that the signal of the lower 7 kinds of determinands of different spray voltages in the present invention responds (n=3)；
Fig. 5 responds (n=3) for the signal of 7 kinds of determinands at a temperature of migration tubes different in the present invention and gas preheater；
Fig. 6 is that the signal of the different drift lower 7 kinds of determinands of gas velocity in the present invention responds (n=3)；
Fig. 7 is the two dimensional separation analysis of 7 kinds of determinands in the present invention.
Wherein, in Fig. 2, Fig. 3 and Fig. 7, the corresponding relationship of number and substance are as follows:
Spectral peak confirmation: 1. danshensus；2. glycyrrhizic acid；3. Gastrodin；4. 5. Puerarin of chlorogenic acid；6. scutelloside；7. rutin.
The Chinese table of comparisons of the English occurred in attached drawing
Specific embodiment
1, experimental section
1.1 instruments and reagent
GA2100 type portable ionic migration spectrum instrument (Excellims company, the U.S.): it be furnished with electric spray ion source, ion grid
Door controller, air filter (sulfur acid calcium and molecular sieve), high-resolution Ion transfer analyzer, Faraday cup detection
Device, VisIon instrument controlling and data processing system use tryptophan and the citric acid school under positive and negative ion mode respectively using preceding
Positive instrument；The adjustable current divider of QuickSplit 600-PO10-04 type (U.S. Analytical Scientific
Instruments company)；ACQUITY Ultra Performance Liquid Chromatography instrument, Xevo TQ-MS triple quadrupole mass spectrometer, MassLynx
Data processing system (Waters, US)；5 type Superpure water machine of Milli-Q Integral (U.S. Merck Millipore
Company).Danshensu (CAS 22681-72-7, purity 98%) and chlorogenic acid (CAS 327-97-9, purity 98%) are purchased from Beijing
Zhong Ke quality inspection Bioisystech Co., Ltd；Glycyrrhizic acid (CAS1405-86-3, purity 98%), rutin (CAS153-18-4, purity
98%), scutelloside (CAS 21967-41-9, purity 98%) and Gastrodin (CAS 62499-27-8, purity 98%) are purchased from hundred
Ling Wei Science and Technology Ltd.；Puerarin (CAS 3681-99-0, purity 98%) is purchased from National Institute for Food and Drugs Control.7 kinds
Standard substance is configured to 1g/L standard reserving solution with methanol, and when use uses methanol dilution at hybrid standard working solution as needed；
Methanol (chromatographically pure) is purchased from U.S. Fisher company；Tryptophan and citric acid are purchased from Sigma-Aldrich, with methanol
It is made into 10mg/L correcting fluid and carries out instrumental correction.
1.2 experimental method
Liquid chromatogram-electron spray that laboratory is voluntarily built-ion mobility spectrometry is combined experimental provision schematic diagram such as Fig. 1 institute
Show.Sample solution imports adjustable current divider (setting split ratio is 50:1) after liquid chromatogram separates, and efflux is divided into two
Road: (about 1 μ L/min, exact numerical are 0.98 μ L/min) is connect with ionic migration spectrometer all the way, is issued in spray voltage effect
Raw electro-spray ionization, the ion of formation enters in the migration tube of ion mobility spectrometry separated after, eventually arrive at Faraday cup
Detector detects to obtain corresponding test map；Another way efflux enters triple quadrupole mass spectrometer, in multiple-reaction monitoring pattern
The signal of 7 kinds of determinands of lower acquisition can make further confirmation to ionic migration spectrum detection result.
1.3 liquid chromatogram separation conditions
Chromatographic column: ACQUITY UPLC BEH C18(50mm×1mm,1.7μm)；Flow velocity: 50 μ L/min；Mobile phase A is
0.5% aqueous formic acid, B are acetonitrile.Gradient elution program: 0~3min, 5%B~10%B；3~10min, 10%B~80%
B；10~12min, 80%B；12~12.1min, 80%B~5%B；12.1~15min, 5%B；Column temperature: 25 DEG C；Sample room temperature
Degree: 20 DEG C；Sample volume: 5 μ L.
1.4 ion mobility spectrometry analysis conditions
Electron spray voltage: 2400V；Ionization mode: negative ion mode；Migrate tube voltage: 8000V；Migration tube temperature:
190℃；Gas preheater temperature: 190 DEG C；Migrate spectrum width: 26ms；Bradbury-Nielsen ion gatewidth: 110 μ
s；Bradbury-Nielsen ion gate voltage: 37V；Drift about gas velocity: 1.4L/min；Exhaust pump pumping speed: 1.0L/min.7 kinds
Molecular formula, relative molecular mass and the transit time of determinand are shown in Table 2, and ion transfer spectrogram is shown in Fig. 2.
Molecular formula, relative molecular mass, Ionization mode and the transit time of 27 kinds of determinands of table
1.5 mass spectral analysis conditions
Electric spray ion source negative ion mode；Capillary voltage: 2.8kV；Radio-frequency lens voltage: 0.3kV；Ion source temperature
Degree: 150 DEG C；Desolvation temperature: 500 DEG C；Desolventizing gas flow: 800L/h；Taper hole throughput: 50L/h；Photoelectric multiplier electricity
Pressure: 650V；Collision gas: argon gas；Collide air pressure: 0.32Pa.The mass spectral analysis parameter of 7 kinds of determinands is shown in Table 1, multiple-reaction monitoring color
Spectrogram is shown in Fig. 3.
The mass spectrometry parameters of 17 kinds of determinands of table
* with the ion of higher response.
2 results and analysis
The optimization of 2.1 liquid chromatogram separation conditions
For ion mobility spectrometry when being combined with liquid chromatogram, electrospray ionisation source is the most commonly used interface mode, passes through height
Piezoelectric field generates charged drop and determinand ion, then enters ionic migration spectrum detection.Due to this experiment intermediate ion migration spectrum
The electrospray interface of outfit not built-in auxiliary gas and heating module, therefore the flow rates being resistant to are lower.Synthesis is examined
Consider and is applicable in flow velocity, separative efficiency, chromatographic peak profile and has selected microbore column with factors, this researchs such as electrospray interface compatibility
ACQUITY UPLC BEH C18(50mm×1mm,1.7μm).Through comparing, can get using acetonitrile as the organic solvent of mobile phase
Preferable chromatographic performance and signal response.It is acid compound in view of 7 kinds of determinands, needs to be added one in mobile phase water phase
The volatile acid of certainty ratio is to obtain ideal chromatographic peak profile and retention behavior.
The optimization of 2.2 ion mobility spectrometry spray voltages
Spray voltage is the important parameter for determining target component signal response intensity and ionising effect.Sample is through liquid phase color
After spectrum separation, after current divider shunts under spray voltage effect, generation ion enters ion mobility spectrometry and obtains efflux after column
Response signal.This experiment investigates spray voltage under the conditions of 1600~2600V, the response of 7 kinds of Chinese medicine index components, they
Best spray voltage slightly has difference, comprehensively considers the respective best spray voltage value of 7 kinds of untested compounds and ionising effect, really
The spray voltage for determining this method is 2400V.Experimental result is as shown in Figure 4.
The optimization of 2.3 ion mobility spectrometry migration tubes and gas preheating temperature
The shadow of this study tour ion mobility spectrometry migration tube and gas pre-heating temperature to target compound signal strength
Ring situation.Ion transfer time poor reproducibility, response are unstable etc. caused by avoid due to heat exchange or other factors
Problem, experiment are set to identical value when optimizing above-mentioned two parameters.When temperature is too low, Environmental Water can believe ion
It number interferes；The excessively high system that will cause of temperature is unstable, leads to losses of ions.Investigated respectively different temperatures (160,170,
180,190,200 DEG C) influence to 7 kinds of Chinese medicine index components responses, as a result as shown in Figure 5.Comprehensively consider each target chemical combination
The signal strength of object ion, the stability of signal drift time and peak shape performance, select 190 DEG C for migration tube and gas pre-add
Hot temperature.
The optimization of 2.4 Ion transfer Frequency bias gas velocities
There is certain influence to ion resolution and response intensity in the type of gas of drifting about and flow velocity.Air relies on stability
By force, the advantages such as low in cost are chosen for drift gas.The different drift gas velocities (1.2~2.2L/min) of this study tour are to 7
The influence of kind compound separating effect and response intensity, experimental result is shown in Fig. 6.When the gas velocity that drifts about is too low, 7 kinds of compounds point
Resolution is poor；And flow velocity it is too high when, response signal strength reduction, reason may be that target concentration is diluted, the work of electric field force
With being cancelled, ion, which is difficult to reach detector, to be caused.It is investigated, the optimum flow rate for the gas that drifts about is 1.4L/min.
2.5 liquid chromatograies-electron spray-ion mobility spectrometry combination analysis
Liquid chromatogram and ion mobility spectrometry are the heterogeneitys for being based respectively on determinand, are separated according to different mechanism,
Thus the two dimensional separation system formed can be complementary to one another in separating capacity.Respectively to liquid chromatogram and Ion transfer spectral condition
On the basis of optimization, liquid chromatogram is combined by electric spray ion source and ion mobility spectrometry, develops danshensu, glycyrrhizic acid, day
The two dimensional separation analysis method of 7 kinds of index components such as numb element, chlorogenic acid, Puerarin, scutelloside, rutin, obtained two dimension are contour
Line chart is shown in Fig. 7.Detection limit, quantitative limit, the range of linearity, linear equation and the related coefficient of 7 kinds of Chinese medicine index ingredients are shown in Table 3.
Since the working flow rate of conventional liquid phase chromatographic column is usually in mL/min rank, and electrospray ion mobility spectrometry can be resistant to
The flow rates received are lower, usually in μ L/min rank, therebetween and mismatch.Excessively high sample introduction flow velocity will cause electron spray
Desolventizing it is difficult, to increase the noise of ion mobility spectrometry, and reduce the response signal of ion.Present invention employs suitable streams
Speed is micro- diameter chromatographic column that the internal diameter of 50 μ L/min or so is 1mm, by shunted after column obtain low flow velocity with adapt to electron spray from
The compatibility requirements of sub- migration spectrum.But since there are relatively large extra-column volumes for conventional liquid phase chromatograph, cause liquid chromatogram point
From dimension, there are a degree of peak shapes to extend.In subsequent experimental research, will using nanoliter/nanoliter level liquid chromatograph carry out
Chromatographic isolation is to reach better separating effect.
Linear equation, the range of linearity, related coefficient, detection limit and the quantitative limit of 37 kinds of determinands of table
* y: peak area；X: mass concentration, μ g/mL.
2.6 liquid chromatograies-triple quadrupole bar mass spectral analysis confirmation
This research also developed 7 kinds of indexs such as danshensu, glycyrrhizic acid, Gastrodin, chlorogenic acid, Puerarin, scutelloside, rutin
Liquid chromatogram-triple quadrupole bar mass spectrum confirmation method of property ingredient.Every kind of target compound select respectively a precursor ion and
Corresponding two product ions are shown in Table 2 as monitoring ion pair, the mass spectral analysis parameter of 7 kinds of ingredients to be measured.If mesh in sample
The ion relative abundance for marking compound is consistent with the relative abundance of the comparable standard solution of concentration, and deviation is right no more than in table 2
The tolerance answered then contains corresponding target compound in judgement sample.
The measurement of 2.7 samples
Using this method to the peaceful oral solution of youngster's cold and abating fever, QINGKAILING KOUFUYE, infantile lung clearing phlegm transforming oral solution, children's seven-star
5 traditional Chinese medicine oral liquid actual samples such as tea oral solution, Shuanghuanglian oral liquid are tested and analyzed.After measured, above-mentioned traditional Chinese medicine mouth
The content for taking index ingredient glycyrrhizic acid in liquid sample is 730.69 and 841.82 μ g/mL, the content of scutelloside is respectively 4.22,
6.51 and 13.08mg/mL has reached the content requirement in " the People's Republic of China's pharmacopeia " 2015 editions.
3 conclusions
This research uses liquid chromatogram-electrospray ionisation-ion mobility spectrometry joint technology, establishes red in traditional Chinese medicine oral liquid
Join the method for separating and analyzing of 7 kinds of index ingredients such as element, glycyrrhizic acid, Gastrodin, chlorogenic acid, Puerarin, scutelloside, rutin, knot
The characteristics of having closed ion mobility spectrometry high-resolution, quick separating and the orthogonality separated with liquid chromatogram is, it can be achieved that target chemical combination
Object simultaneously the two dimensional separation based on hydrophobicity and ionic mobility difference, for complex sample system comprehensive analysis provide it is more rich
Rich integrated information.
Embodiment described above only describe the preferred embodiments of the invention, not to model of the invention
It encloses and is defined, without departing from the spirit of the design of the present invention, those of ordinary skill in the art are to technical side of the invention
The various changes and improvements that case is made should all be fallen into the protection scope that claims of the present invention determines.
Claims (9)
1. a kind of method of index ingredient in measurement traditional Chinese medicine oral liquid, characterized by the following steps:
Sample solution imports adjustable current divider after liquid chromatogram separates, and efflux is divided into two-way: all the way with Ion transfer
Under spray voltage effect electro-spray ionization occurs for spectrometer connection, and the ion of formation enters the migration tube of ionic migration spectrometer
Faraday cup detector is eventually arrived at after inside being separated to detect to obtain corresponding test map；Another way efflux enters triple four
Pole bar mass spectrograph acquires the signal of determinand under multiple-reaction monitoring pattern, makees the testing result of ionic migration spectrometer into one
Step confirmation.
2. the method for index ingredient in measurement traditional Chinese medicine oral liquid according to claim 1, it is characterised in that: use liquid phase
Chromatography-electron spray-ion mobility spectrometry is combined experimental provision, and described device includes ionic migration spectrometer, adjustable current divider, surpasses
High performance liquid chromatograph and triple quadrupole mass spectrometer, wherein the inlet end of the adjustable flow distributing device and the ultra high efficiency
The liquid outlet of liquid chromatograph is connected, the liquid outlet end of the adjustable flow distributing device respectively with the ionic migration spectrometer and described
The inlet end of triple quadrupole mass spectrometer is connected.
3. the method for index ingredient in measurement traditional Chinese medicine oral liquid according to claim 2, it is characterised in that: the index
Property ingredient be danshensu, chlorogenic acid, glycyrrhizic acid, rutin, scutelloside, Gastrodin and Puerarin, totally 7 kinds.
4. the method for index ingredient in measurement traditional Chinese medicine oral liquid according to claim 3, it is characterised in that: described in setting
The split ratio of adjustable current divider is 50:1, the low flow velocity liquid outlet end of the adjustable flow distributing device and the ion mobility spectrometry
The inlet end of instrument is connected, the high flow rate liquid outlet end of the adjustable flow distributing device and the feed liquor of the triple quadrupole mass spectrometer
Mouth end is connected.
5. the method for index ingredient in measurement traditional Chinese medicine oral liquid according to claim 4, it is characterised in that: the ion
The sample introduction flow velocity of mobility spectrometer is 0.98 μ L/min.
6. the method for index ingredient in measurement traditional Chinese medicine oral liquid according to claim 5, it is characterised in that:
Liquid chromatogram separation condition are as follows:
Chromatographic column: ACQUITY UPLC BEH C18, 50mm × 1mm, 1.7 μm；Flow velocity: 50 μ L/min；Mobile phase A is 0.5% first
Aqueous acid, B are acetonitrile；Gradient elution program: 0~3min, 5%B~10%B；3~10min, 10%B~80%B；10~
12min, 80%B；12~12.1min, 80%B~5%B；12.1~15min, 5%B；Column temperature: 25 DEG C；Sample room temperature: 20
℃；Sample volume: 5 μ L.
7. the method for index ingredient in measurement traditional Chinese medicine oral liquid according to claim 6, it is characterised in that:
The analysis condition of the ionic migration spectrometer are as follows:
Electron spray voltage: 2400V；Ionization mode: negative ion mode；Migrate tube voltage: 8000V；Migration tube temperature: 190 DEG C；
Gas preheater temperature: 190 DEG C；Migrate spectrum width: 26ms；Bradbury-Nielsen ion gatewidth: 110 μ s；
Bradbury-Nielsen ion gate voltage: 37V；Drift about gas velocity: 1.4L/min；Exhaust pump pumping speed: 1.0L/min.
8. the method for index ingredient in measurement traditional Chinese medicine oral liquid according to claim 7, it is characterised in that:
Mass spectral analysis condition is as follows:
Electric spray ion source negative ion mode；Capillary voltage: 2.8kV；Radio-frequency lens voltage: 0.3kV；Ion source temperature: 150
℃；Desolvation temperature: 500 DEG C；Desolventizing gas flow: 800L/h；Taper hole throughput: 50L/h；Photoelectric multiplier voltage:
650V；Collision gas: argon gas；Collide air pressure: 0.32Pa.
9. the method for index ingredient in measurement traditional Chinese medicine oral liquid according to claim 8, it is characterised in that:
The mass spectral analysis parameter of 7 kinds of determinands is as follows:
The mass spectrometry parameters of 17 kinds of determinands of table
* with the ion of higher response.
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Citations (3)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN105241980A (en) * | 2015-11-12 | 2016-01-13 | 陕西步长制药有限公司 | Rapid separation liquid chromatography detection method for naoxintong capsules |
| CN107271575A (en) * | 2016-04-08 | 2017-10-20 | 株式会社岛津制作所 | The method and device of ion mobility spectrometry and mass spectrum parallel parsing |
| CN108072690A (en) * | 2016-11-17 | 2018-05-25 | 中国科学院大连化学物理研究所 | A kind of ion mobility spectrometry and ion trap mass spectrometry combination device and analysis method |
-
2019
- 2019-01-25 CN CN201910073143.8A patent/CN109580849B/en active Active
Patent Citations (3)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN105241980A (en) * | 2015-11-12 | 2016-01-13 | 陕西步长制药有限公司 | Rapid separation liquid chromatography detection method for naoxintong capsules |
| CN107271575A (en) * | 2016-04-08 | 2017-10-20 | 株式会社岛津制作所 | The method and device of ion mobility spectrometry and mass spectrum parallel parsing |
| CN108072690A (en) * | 2016-11-17 | 2018-05-25 | 中国科学院大连化学物理研究所 | A kind of ion mobility spectrometry and ion trap mass spectrometry combination device and analysis method |
Non-Patent Citations (4)
| Title |
|---|
| LU WANG ET AL.: "A strategy for identification and structural characterization of compounds from Gardenia jasminoides by integrating macroporousresin column chromatography and liquid chromatography-tandem mass spectrometry combined with ion-mobility spectrometry", 《JOURNAL OF CHROMATOGRAPHY A》 * |
| 史培颖 等: "高效液相色谱法同时测定玉泉丸中的葛根素及甘草酸", 《中国医院药学杂志》 * |
| 孔景临 等: "电喷雾离子迁移谱快速检测次乌头碱的研究", 《现代仪器与医疗》 * |
| 章运典 等: "ＲP-HPLC法同时测定天智颗粒中天麻素、栀子苷、芦丁和黄芩苷", 《中成药》 * |
Cited By (1)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN110749681A (en) * | 2019-11-19 | 2020-02-04 | 山东省中医药研究院 | Quality evaluation method of traditional Chinese medicine liquorice and application thereof |
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