CN106290685A - The UHPLC MS detection method of WANGLAOJI LIANGCHA chemical composition - Google Patents
The UHPLC MS detection method of WANGLAOJI LIANGCHA chemical composition Download PDFInfo
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- CN106290685A CN106290685A CN201610826315.0A CN201610826315A CN106290685A CN 106290685 A CN106290685 A CN 106290685A CN 201610826315 A CN201610826315 A CN 201610826315A CN 106290685 A CN106290685 A CN 106290685A
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- G—PHYSICS
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- G01N30/00—Investigating or analysing materials by separation into components using adsorption, absorption or similar phenomena or using ion-exchange, e.g. chromatography or field flow fractionation
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- G—PHYSICS
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- G01N—INVESTIGATING OR ANALYSING MATERIALS BY DETERMINING THEIR CHEMICAL OR PHYSICAL PROPERTIES
- G01N30/00—Investigating or analysing materials by separation into components using adsorption, absorption or similar phenomena or using ion-exchange, e.g. chromatography or field flow fractionation
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Abstract
The present invention relates to the UHPLC MS detection method of a kind of WANGLAOJI LIANGCHA chemical composition, belong to herbal tea plant beverage Quality Control Technology field.This construction method comprises the following steps: the preparation of (1) inner mark solution: precision weighs Palmic acid, with acetic acid ethyl dissolution constant volume, obtains inner mark solution；(2) preparation of need testing solution: precision measures WANGLAOJI LIANGCHA, extracts with ethyl acetate, takes ethyl acetate supernatant, obtain need testing solution；(3) precision draws above-mentioned inner mark solution and need testing solution respectively, and after mixing, injection gas chromatography instrument measures, and obtains the WANGLAOJI LIANGCHA volatile ingredients fingerprint with common characteristic peak.This construction method and detection method can comprehensively characterize each composition added in WANGLAOJI LIANGCHA, and have the feature of good stability, can the quality of Efficient Characterization WANGLAOJI LIANGCHA, be conducive to again monitoring the quality of product.
Description
Technical field
The present invention relates to herbal tea plant beverage Quality Control Technology field, particularly relate to a kind of WANGLAOJI LIANGCHA chemistry and become
The UHPLC-MS detection method divided.
Background technology
South of the Five Ridges herbal tea culture has that long history is long-pending accumulates and folk custom intension.The ancient times south of the Five Ridges is hundred inducing vomiting ground, many miasma, dye
Person is the most dead without having.The south of the Five Ridges people, with the constantly fight of extreme natural environment, have accumulated the preciousness that conditioning keeps healthy, prevents and cures diseases
Experience.They, according to local weather, water and soil characteristic, have heat-clearing and toxic substances removing, promoting the production of body fluid to quench thirst, effects such as fire dehumidifying of dispelling with some
Based on Lingnan features Chinese herbal medicine, through long-term practice under tcm health preserving theoretical direction, create various " herbal tea ",
For preventing and curing diseases, define unique scenery of a Lingnan Culture.
WANGLAOJI LIANGCHA is history guangdong herbal tea the earliest, firstly appears in 1828 (clean the street light 8 years), the most more than 180
Year history, is acknowledged as herbal tea first ancestor, has the title of " medicated tea king ".Decades recently, along with modern production equipment and first inlet pipe
The introducing of reason theory, herbal tea industry there occurs great change, keeps herbal tea paving in the past and drinks the situation of herbal tea and be broken, and herbal tea is processed to
Drink more easily granule, teabag, Tetra Pak, the plurality of specifications such as canned.
WANGLAOJI LIANGCHA with water, white sugar, Herba mesonae chinensis, egg flower, Flos Chrysanthemi, Spica Prunellae, Radix Glycyrrhizae, Flos Lonicerae, Folium Microcoris paniculatae as raw material,
Extracted, concentrate, prepare, sterilizing, the main process such as packaging are made, its cool taste is tasty and refreshing, cold and hot drinks all suitable, is subject to
Consumer is liked.For comprehensively reflecting and monitor the inherent quality of this kind, promote the development of this kind, this kind should be carried out
In the research of each component detection method.
Summary of the invention
The present invention provides the UHPLC-MS detection method of a kind of WANGLAOJI LIANGCHA chemical composition, in order to WANGLAOJI LIANGCHA
Quality is monitored, it is possible to identify trace constituent therein, it is achieved the purpose of general warranty WANGLAOJI LIANGCHA quality.
The UHPLC-MS detection method of a kind of WANGLAOJI LIANGCHA chemical composition, comprises the following steps:
The preparation of need testing solution: take test sample, crosses microporous filter membrane, prepares need testing solution；
The preparation of reference substance solution: precision weighs product danshensu, chlorogenic acid, liquirtin, narcissin, Trifolin, different green
At least one in ortho acid A, 15-demethyl plumieride, sea Fructus Mangifera Indicae acid B, rosmarinic acid, SHY-2 reference substance, to have
Machine solvent dissolves constant volume, prepares reference substance solution；
Detection: above-mentioned need testing solution and reference substance solution are injected separately in ultrahigh pressure liquid phase tandem mass spectrometer detection.
The UHPLC-MS detection method of above-mentioned WANGLAOJI LIANGCHA chemical composition, with danshensu, chlorogenic acid, liquirtin, narcissus
In glycosides, Trifolin, 3,5-Dicaffeoylquinic acid, 15-demethyl plumieride, sea Fructus Mangifera Indicae acid B, rosmarinic acid, SHY-2 at least
A kind of as reference substance, and by the use of ultrahigh pressure liquid phase chromatograph, it is possible to by Multiple components in WANGLAOJI LIANGCHA efficiently, at a high speed
Carrying out separate, coordinate high-precision mass spectrograph to detect subsequently, Multiple components in WANGLAOJI LIANGCHA (including trace constituent) entered
Row is analyzed, is measured, and then realizes the purpose of general warranty WANGLAOJI LIANGCHA quality.
Wherein in an embodiment, in described detecting step, according to following chromatographic condition carry out ultrahigh pressure liquid phase chromatograph-
Mass spectrum Series detectors:
Fixing phase: carbon octadecylsilane base bonded silica gel is the chromatographic column of filler；
Flowing phase: concentration of volume percent be the aqueous formic acid of 0.1% be mobile phase A, acetonitrile is Mobile phase B, use
Gradient elution mode；
Flow velocity: 0.2-0.3mL/min.
Carry out separating, detecting with above-mentioned chromatographic condition, it is possible to well separated by Multiple components in WANGLAOJI LIANGCHA, make each
Composition has detection and the qualification of preferable separating degree, beneficially postorder.
Wherein in an embodiment, in described detecting step, according to following chromatographic condition carry out ultrahigh pressure liquid phase chromatograph-
Mass spectrum Series detectors:
Chromatographic condition is as follows:
Sample size: 5 μ L；
Fixing phase: packing material size is 1.8 μm, and diameter, length are respectively the ZORBAX SB-C18 color of 4.6mm and 150mm
Spectrum post；
Flowing phase: concentration of volume percent be the aqueous formic acid of 0.1% be mobile phase A, acetonitrile is Mobile phase B, eluting
Gradient is: 0-25min, and the percentage by volume of Mobile phase B is 20%；25-30min, the percentage by volume of Mobile phase B is become by 20%
Change to 24%；30-45min, the percentage by volume of Mobile phase B is changed to 48% by 24%；45-49min, the volume of Mobile phase B
Percent is 48%；
Column temperature: room temperature；
Flow velocity: 0.25mL/min.
Carry out separating, detecting with above-mentioned chromatographic condition, there is optimal separating effect.
Wherein in an embodiment, in described detecting step, described mass spectrum is ion trap orbitrap type high resolution mass spectrum.
Use ion trap orbitrap type high resolution mass spectrum to carry out detection to analyze, using the teaching of the invention it is possible to provide more about compositions various in WANGLAOJI LIANGCHA
Structure feature information, preferably wherein each composition is identified, analyze.
Wherein in an embodiment, in described detecting step, according to following Mass Spectrometry Conditions carry out ultrahigh pressure liquid phase chromatograph-
Mass spectrum Series detectors:
Ionization mode: electro-spray ionization (ESI)；
Detection pattern: anion；
Sweep limits: 100-1500m/z；
Capillary temperature: 300-350 DEG C；
Sheath gas velocity: 40-50L/min；
Secondary air speed: 6-10L/min；
Source voltage: 4200-4800V；
Focus voltage: 100-120V.
The present inventor has been respectively compared the impact on compound ions degree of cation and negative ion mode, found that
In the negative ion mode, majority of compounds can detect that [M-H]-quasi-molecular ion peak.We are by analyzing UHPLC-MS
In chromatogram, the accurate molecular weight information of the combination high resolution mass spectrum of each compound, can deduce the molecule that compound is possible
Formula, then can further determine that, according to the information of multi-stage ms fragment, the structural information that compound is possible.According to Mass Spectrometer Method
As a result, on the one hand binding compounds is relevant to reference substance at retention time, accurate molecular weight and the patch information of C18 chromatographic column
Parameter is compared, online Rapid identification known compound；Can also be according to the cracking rule of a compounds, by instrument certainly
The mass spectrometric data library searching of band and compare with document thus infer the structure of unknown chemical conversion point.
Wherein in an embodiment, in described detecting step, according to following Mass Spectrometry Conditions carry out ultrahigh pressure liquid phase chromatograph-
Mass spectrum Series detectors:
Ionization mode: electro-spray ionization；
Detection pattern: anion；
Sweep limits: 100-1500m/z；
Capillary temperature: 325 DEG C；
Sheath gas velocity: 45L/min；
Secondary air speed: 8L/min；
Source voltage: 4500V；
Focus voltage: 110V.
Detect with above-mentioned Mass Spectrometry Conditions, not only there is preferable sensitivity, additionally it is possible to obtain more architectural feature
Information, in order to preferably identify wherein each composition, analyzes.
Wherein in an embodiment, in the preparation process of described reference substance solution, it is fixed to be dissolved with methanol by each reference substance
Holding, prepared concentration is the reference substance solution of 1.5-2.5mg/L.The concentration of reference substance solution is limited within the range, with confession examination
In product solution, the concentration of each composition adapts, and has preferably with reference to property.
Wherein in an embodiment, in the preparation process of described reference substance solution, each reference substance is settled to same appearance
In device, prepare mixing reference substance solution.Measure with mixing reference substance solution simultaneously, have convenient, fast and save testing cost
Advantage.
Wherein in an embodiment, in the preparation process of described need testing solution, taking WANGLAOJI LIANGCHA, to cross 0.45 μm micro-
Hole filter membrane, to obtain final product.
Compared with prior art, the method have the advantages that
The UHPLC-MS detection method of the WANGLAOJI LIANGCHA chemical composition of the present invention, selects danshensu, chlorogenic acid, Radix Glycyrrhizae
Glycosides, narcissin, Trifolin, 3,5-Dicaffeoylquinic acid, 15-demethyl plumieride, sea Fructus Mangifera Indicae acid B, rosmarinic acid, SHY-2
In at least one as reference substance, and by the use of ultrahigh pressure liquid phase chromatograph, it is possible to by Multiple components in WANGLAOJI LIANGCHA
Carrying out efficiently, at a high speed separates, and coordinates high-precision mass spectrograph to detect subsequently, (Multiple components in WANGLAOJI LIANGCHA is included trace
Amount composition) it is analyzed, measures, and then realize the purpose of general warranty WANGLAOJI LIANGCHA quality.Meanwhile, it is also WANGLAOJI LIANGCHA
The research that spectrum effect is learned is laid a good foundation.
Further, liquid-phase condition therein and Mass Spectrometry Conditions are also optimized by this detection method, it is possible to by cool for king Lao Ji
In tea, Multiple components well separates, and makes each composition have preferable separating degree and sensitivity, and can provide more about king
The structure feature information of various compositions in Lao Ji herbal tea, preferably identifies wherein each composition, analyzes.
Accompanying drawing explanation
Fig. 1 is the total ion current figure of WANGLAOJI LIANGCHA in embodiment 1.
Detailed description of the invention
For the ease of understanding the present invention, below with reference to relevant drawings, the present invention is described more fully.Hereinafter give
Go out presently preferred embodiments of the present invention.But, the present invention can realize in many different forms, however it is not limited to is retouched herein
The embodiment stated.On the contrary, providing the purpose of these embodiments is to make the understanding to the disclosure more thorough complete
Face.
Unless otherwise defined, all of technology used herein and scientific terminology and the technical field belonging to the present invention
The implication that technical staff is generally understood that is identical.The term used the most in the description of the invention is intended merely to describe tool
The purpose of the embodiment of body, it is not intended that in limiting the present invention.
Instrument in following example is as follows with reagent:
Instrument:
Thermo Scientific Accela UHPLC-LTQ Orbitrap XLTM ultrahigh pressure liquid phase series combination type
Ion trap track trap high resolution mass spectrum combined instrument (Thermo Fisher Scientific Inc., the U.S.), is equipped with ThermoAccela
1250Pump, Thermo Accela Autosampler, Thermo Accela PDA detector, Thermo
ScientificTM LTQ Orbitrap XLTM；
KQ5200 ultrasonic washing unit (Kunshan Ultrasonic Instruments Co., Ltd.)；
SI-114 ten thousand/electronic balance, TB-25 100,000/electronic balance (Instrument Ltd. of Denver, China
Beijing).
Reagent:
Methanol and acetonitrile are chromatographically pure (U.S. Honeywell), experimental water be ultra-pure water (Mili-Q pure water instrument,
Millipore company), other reagent are domestic analytical pure.
WANGLAOJI LIANGCHA is provided by Wanglaoji Pharmaceutical Co., Ltd., Guangzhou City.
Reference substance danshensu, chlorogenic acid, liquirtin, narcissin, Trifolin, 3,5-Dicaffeoylquinic acid, 15-demethyl Flos Plumeriae Acutifoliae
Glycosides, sea Fructus Mangifera Indicae acid B, rosmarinic acid, SHY-2 are self-control and determine structure, Liquid Detection purity through spectral method, and area is returned
One changes method calculated purity is all higher than 98.0%.
Embodiment 1
The UHPLC-MS detection method of a kind of WANGLAOJI LIANGCHA chemical composition, comprises the following steps:
One, the preparation of need testing solution.
Take WANGLAOJI LIANGCHA, cross 0.45 μm microporous filter membrane, obtain need testing solution.
Two, the preparation of reference substance solution.
Take reference substance danshensu, chlorogenic acid, liquirtin, narcissin, Trifolin, 3,5-Dicaffeoylquinic acid, 15-demethyl respectively
Plumieride, sea Fructus Mangifera Indicae acid B, rosmarinic acid, SHY-2 are appropriate, accurately weighed, are placed in 10mL volumetric flask, and methanol is molten
Solving, constant volume, as single reference substance solution.
During precision draws each single reference substance solution 1.0mL to 50mL volumetric flask respectively, methanol dilution constant volume, obtain 2mg/
The mixing reference substance solution of L.
Three, detection.
Respectively above-mentioned need testing solution and reference substance solution are injected separately in ultrahigh pressure liquid phase tandem mass spectrometer detection, tool
Concrete conditions in the establishment of a specific crime is as follows:
Chromatographic condition is as follows:
Sample size: 5 μ L；
Fixing phase: ZORBAX SB-C18 (4.6 × 150mm, 1.8 μm) chromatographic column；
Flowing phase: concentration of volume percent be the aqueous formic acid of 0.1% be mobile phase A, acetonitrile is Mobile phase B, eluting
Gradient is: 0-25min, and the percentage by volume of Mobile phase B is 20%；25-30min, the percentage by volume of Mobile phase B is become by 20%
Change to 24%；30-45min, the percentage by volume of Mobile phase B is changed to 48% by 24%；45-49min, the volume of Mobile phase B
Percent is 48%；
Column temperature: room temperature；
Flow velocity: 0.25mL/min.
The Mass Spectrometry Conditions of ion trap orbitrap type high resolution mass spectrum is as follows:
Ionization mode: electro-spray ionization；
Detection pattern: anion；
Sweep limits: 100-1500m/z；
Capillary temperature: 325 DEG C；
Sheath gas velocity: 45L/min；
Secondary air speed: 8L/min；
Source voltage: 4500V；
Focus voltage: 110V.
Four, result.
Obtain the total ion current figure (TIC) of WANGLAOJI LIANGCHA, as shown in Figure 1.Carry out with the testing result of reference substance solution
Compare, and analyze the master that the retention time of main chemical compositions in this WANGLAOJI LIANGCHA finished product, molecular formula and ESI-MS produce
Want isolated 29 the main chromatographic peaks of fragment ion WANGLAOJI LIANGCHA finished product UHPLC-MS to be analyzed, identify 24 chemical combination
The possible structure of thing, as shown in the table.
The UHPLC-MS analysis result of table 1 sample chemical composition
Note: it is corresponding with the retention time of reference substance and Information in Mass Spectra that " * " is labeled as this compound.
It can be seen that after inventor is analyzed, identify the possible structure of 24 compounds in from the above.Wherein
15-demethyl plumieride (4), danshensu (5), chlorogenic acid (7), sea Fructus Mangifera Indicae acid B (10), liquirtin (13), SHY-2
(14), 10 compounds warps such as narcissin (16), Trifolin (17), 3,5-Dicaffeoylquinic acid (18), rosmarinic acid (21) and reference substance
Retention time, Information in Mass Spectra comparison confirmed.
14 compounds may be that gluconic acid (1), disaccharidase (2), disaccharidase (3), Fructus Gardeniae are new through consulting literatures data speculation
Glycosides (6), Isomeric di-O-CQA (9), glycyrrhizin-4 '-celery glucosides (11), alkannic acid (12), 4,5-Dicaffeoylquinic acid (15), red phenol
Acid B (19), 3,4-Dicaffeoylquinic acid (20), salvianolic acid A (22), salvianolic acid E (23), glycyrrhizin A3 (26), Saponin G 2 (28).
Separately having 5 compounds 8,24,25,27,29 owing to lacking relevant document report and reference substance, structure needs into one
Step Analysis and Identification.
Above-described embodiment has carried out UHPLC-MS analysis to the chemical composition of WANGLAOJI LIANGCHA, and majority of compounds can obtain
To efficiently separating and identifying.It is divided into from 29 compositions, identifies 24 therein, wherein 10 compound warps and reference substance
Retention time, Information in Mass Spectra comparison confirmed.Chemically from the point of view of composition analysis result, the primary chemical of WANGLAOJI LIANGCHA becomes
It is divided into phenolic acids, flavonoid and saponins.
Each technical characteristic of embodiment described above can combine arbitrarily, for making description succinct, not to above-mentioned reality
The all possible combination of each technical characteristic executed in example is all described, but, as long as the combination of these technical characteristics is not deposited
In contradiction, all it is considered to be the scope that this specification is recorded.
Embodiment described above only have expressed the several embodiments of the present invention, and it describes more concrete and detailed, but also
Can not therefore be construed as limiting the scope of the patent.It should be pointed out that, come for those of ordinary skill in the art
Saying, without departing from the inventive concept of the premise, it is also possible to make some deformation and improvement, these broadly fall into the protection of the present invention
Scope.Therefore, the protection domain of patent of the present invention should be as the criterion with claims.
Claims (9)
1. the UHPLC-MS detection method of WANGLAOJI LIANGCHA chemical composition, it is characterised in that comprise the following steps:
The preparation of need testing solution: take test sample, crosses microporous filter membrane, prepares need testing solution；
The preparation of reference substance solution: precision weigh danshensu, chlorogenic acid, liquirtin, narcissin, Trifolin, 3,5-Dicaffeoylquinic acid,
At least one in 15-demethyl plumieride, sea Fructus Mangifera Indicae acid B, rosmarinic acid, SHY-2 reference substance, with organic solvent
Dissolve constant volume, prepare reference substance solution；
Detection: above-mentioned need testing solution and reference substance solution are injected separately in ultrahigh pressure liquid phase tandem mass spectrometer detection.
The UHPLC-MS detection method of WANGLAOJI LIANGCHA chemical composition the most according to claim 1, it is characterised in that described
In detecting step, carry out ultrahigh pressure liquid phase chromatography-mass spectroscopy Series detectors according to following chromatographic condition:
Fixing phase: carbon octadecylsilane base bonded silica gel is the chromatographic column of filler；
Flowing phase: concentration of volume percent be the aqueous formic acid of 0.1% be mobile phase A, acetonitrile is Mobile phase B, use gradient
Type of elution；
Flow velocity: 0.2-0.3mL/min.
The UHPLC-MS detection method of WANGLAOJI LIANGCHA chemical composition the most according to claim 2, it is characterised in that described
In detecting step, carry out ultrahigh pressure liquid phase chromatography-mass spectroscopy Series detectors according to following chromatographic condition:
Sample size: 5 μ L；
Fixing phase: packing material size is 1.8 μm, and diameter, length are respectively the ZORBAXSB-C18 chromatographic column of 4.6mm and 150mm；
Flowing phase: concentration of volume percent be the aqueous formic acid of 0.1% be mobile phase A, acetonitrile is Mobile phase B, gradient
For: 0-25min, the percentage by volume of Mobile phase B is 20%；25-30min, the percentage by volume of Mobile phase B is changed to by 20%
24%；30-45min, the percentage by volume of Mobile phase B is changed to 48% by 24%；45-49min, the volume basis of Mobile phase B
Number is 48%；
Column temperature: room temperature；
Flow velocity: 0.25mL/min.
4. according to the UHPLC-MS detection method of the WANGLAOJI LIANGCHA chemical composition described in any one of claim 1-3, its feature
Being, in described detecting step, described mass spectrum is ion trap orbitrap type high resolution mass spectrum.
The UHPLC-MS detection method of WANGLAOJI LIANGCHA chemical composition the most according to claim 4, it is characterised in that described
In detecting step, carry out ultrahigh pressure liquid phase chromatography-mass spectroscopy Series detectors according to following Mass Spectrometry Conditions:
Ionization mode: electro-spray ionization；
Detection pattern: anion；
Sweep limits: 100-1500m/z；
Capillary temperature: 300-350 DEG C；
Sheath gas velocity: 40-50L/min；
Secondary air speed: 6-10L/min；
Source voltage: 4200-4800V；
Focus voltage: 100-120V.
The UHPLC-MS detection method of WANGLAOJI LIANGCHA chemical composition the most according to claim 5, it is characterised in that described
In detecting step, carry out ultrahigh pressure liquid phase chromatography-mass spectroscopy Series detectors according to following Mass Spectrometry Conditions:
Ionization mode: electro-spray ionization；
Detection pattern: anion；
Sweep limits: 100-1500m/z；
Capillary temperature: 325 DEG C；
Sheath gas velocity: 45L/min；
Secondary air speed: 8L/min；
Source voltage: 4500V；
Focus voltage: 110V.
The UHPLC-MS detection method of WANGLAOJI LIANGCHA chemical composition the most according to claim 1, it is characterised in that described
In the preparation process of reference substance solution, with methanol, each reference substance being dissolved constant volume, prepared concentration is the reference substance of 1.5-2.5mg/L
Solution.
The UHPLC-MS detection method of WANGLAOJI LIANGCHA chemical composition the most according to claim 7, it is characterised in that described
In the preparation process of reference substance solution, each reference substance is settled in same container, prepares mixing reference substance solution.
The UHPLC-MS detection method of WANGLAOJI LIANGCHA chemical composition the most according to claim 1, it is characterised in that described
In the preparation process of need testing solution, take WANGLAOJI LIANGCHA and cross 0.45 μm microporous filter membrane, to obtain final product.
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Citations (3)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN101181539A (en) * | 2007-11-20 | 2008-05-21 | 广州王老吉药业股份有限公司 | New use of chinese medicine composition |
| CN103808829A (en) * | 2014-03-10 | 2014-05-21 | 湖南师范大学 | Quantitative quality control method of herbal tea product |
| WO2014134254A1 (en) * | 2013-02-28 | 2014-09-04 | Schweitzer-Mauduit International, Inc. | Composition for making a tea beverage or herbal and vegetable broths |
-
2016
- 2016-09-14 CN CN201610826315.0A patent/CN106290685B/en active Active
Patent Citations (3)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN101181539A (en) * | 2007-11-20 | 2008-05-21 | 广州王老吉药业股份有限公司 | New use of chinese medicine composition |
| WO2014134254A1 (en) * | 2013-02-28 | 2014-09-04 | Schweitzer-Mauduit International, Inc. | Composition for making a tea beverage or herbal and vegetable broths |
| CN103808829A (en) * | 2014-03-10 | 2014-05-21 | 湖南师范大学 | Quantitative quality control method of herbal tea product |
Non-Patent Citations (3)
| Title |
|---|
| JIEWEI DENG 等: "Quality assessment and origin tracing of Guangdong Liangcha granules using direct mass spectrometry fingerprinting", 《ANAL. METHODS》 * |
| 朱平川 等: "液质联用法***老吉凉茶中的3种有效成分", 《湖北大学学报（自然科学版）》 * |
| 杨运云 等: "王老吉广东凉茶颗粒的超高效液相色谱指纹图谱研究", 《分析测试学报》 * |
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