CN104458933B - Method for detecting quality of frangipani medicinal material or frangipani extract - Google Patents
Method for detecting quality of frangipani medicinal material or frangipani extract Download PDFInfo
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- ZUKLFFYDSALIQW-MSUKCBDUSA-N Iridoid glycoside Chemical compound [H][C@]12CC[C@H](C(O)=O)[C@@]1([H])[C@H](OC1O[C@H](CO)[C@@H](O)[C@H](O)[C@H]1O)OC=C2 ZUKLFFYDSALIQW-MSUKCBDUSA-N 0.000 abstract description 2
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Abstract
The invention provides a method for detecting the quality of a frangipani medicinal material or a frangipani extract, which adopts an HPLC method to detect the quality of dried flowers and extracts of frangipani Plumeria L, belonging to the genus frangipani of the family oleaceae, and adopts a high performance liquid chromatography to determine, wherein the chromatographic conditions are as follows: octadecyl bonded phase silica gel is used as a filling agent, acetonitrile-0.5% phosphoric acid water (8:92) is used as a mobile phase, and the detection wavelength is 210 nm. The inventor researches and discovers that the 15-demethyl frangipanin is one of iridoid glycoside components contained in the frangipani, has higher content and can be used for detecting and controlling the quality of the frangipani. The invention adopts HPLC method to determine the content of 15-demethyl frangipani glycoside in the frangipani for the first time, and provides scientific basis for the quality standard of the frangipani.
Description
Technical field
The present invention relates to a kind of method detecting frangipanis medicinal material or Flos Plumeriae Acutifoliae extract quality.
Background technology
Frangipanis, has another name called remote cape jasmine, and yolk flower, beating and beat flower, is the dry flower of Apocynaceae frangipanis platymiscium frangipanis PlumeriarubraL..It originates in tropical America, existing extensively plants in global tropical area, China then main product in Guangdong, Fujian, Guangxi, the ground such as Hainan.Its taste is sweet, light, cool in nature, has clearing heat and promoting diuresis and stops dysentery, and the effect of the removing toxic substances that moistens the lung and relieve the cough, can be used for damp-heat diarrhea clinically, tenesmus, the diseases such as cough with lung heat, determined curative effect.It is that Lingnan area commonly uses herbal medicine, is also one of primary raw material medicinal material of guangdong herbal tea, and reputable brand cold tea " WANGLAOJI LIANGCHA " " five-flowered tea " etc. as market sale is all be main constitutive material with frangipanis.Along with the development of cold tea industry, also increasing to the demand of frangipanis, its quality problems also become increasingly conspicuous simultaneously.Iridoids material in frangipanis have very strong antimycotic, suppress HIV virus and tumor promotion effect, but from the document reported, mainly its volatile oil to be studied, still loses and have the content to its iridoids material to measure.
15-demethyl plumieride has pertinent literature report in the root skin of frangipanis, and (flood is endured, Deng, chemical composition and bioactivity research progress in frangipanis, research and development of natural products, 2011,23:565-570), but in flower not report whether containing 15-demethyl plumieride.
Summary of the invention
Technical scheme of the present invention there is provided a kind of method detecting frangipanis medicinal material or Flos Plumeriae Acutifoliae extract quality.
A kind of method detecting frangipanis medicinal material or Flos Plumeriae Acutifoliae extract quality, it is characterized in that: it adopts HPLC method to detect the dry flower of Apocynaceae frangipanis platymiscium frangipanis PlumeriarubraL., the quality of its extract, high performance liquid chromatography is adopted to measure, chromatographic condition is: with Octadecylsilane bonded phase silica gel for filling agent, with acetonitrile-0.5% phosphoric acid water (8:92) for mobile phase, determined wavelength is 210nm.
Further preferably, described chromatographic condition is: Agilent1200 high performance liquid chromatograph, KromasilC18 chromatographic column (250 × 4.6mm, 5 μm); Mobile phase is acetonitrile-0.5% phosphoric acid water (8:92), flow velocity: 1.0mL/min, isocratic elution 15min; Column temperature: 30 DEG C, determined wavelength: 210nm, sample size: 10 μ L.Particularly, it comprises the steps:
The preparation of a, reference substance solution:
Get 15-demethyl plumieride reference substance appropriate, accurately weighed, add 50% methyl alcohol and make the solution of every 1mL containing 0.103mg, to obtain final product;
The preparation of b, need testing solution
Get medicinal material coarse powder and be about 0.2g, accurately weighed, put in tool plug conical flask, precision adds 50% methyl alcohol 25mL, weighed weight, ultrasonic extraction (100W, 40kHz) 30 minutes, cooling, more weighed weight, add the weight that 50% methyl alcohol supplies less loss, shake up, filter, filtrate filters with 0.45 μm of miillpore filter again, get subsequent filtrate, to obtain final product;
C, to detect by above-mentioned chromatographic condition.
Inventor studies discovery, and 15-demethyl plumieride is one of iridoid glycoside constituents contained in frangipanis, and its comparision contents is high, can be used for quality testing and the control of frangipanis flower.The present invention adopts HPLC method to measure the content of 15-demethyl plumieride in frangipanis, for the quality standard of frangipanis provides scientific basis first.
Accompanying drawing explanation
Fig. 1 reference substance (A) and sample (B) chromatogram
115-demethyl plumieride
Fig. 2 sample size average figure
Embodiment
The quality determining method of embodiment 1 frangipanis medicinal material of the present invention
1 instrument and material
Agilent 1200 type high performance liquid chromatograph (quaternary pump, column oven, VWD detecting device, U.S.'s Agilent Technologies); TU-1810 type ultraviolet-visible spectrophotometer (Beijing is general analyses all purpose instrument); SartoriusBP124S type electronic balance (sensibility reciprocal: 0.1mg, Germany); SartoriusBP211D type electronic balance (sensibility reciprocal: 0.01mg, Germany); KQ250B type ultrasonic cleaner (Kunshan Ultrasonic Instruments Co., Ltd.); LSF-80 type high speed disintegrator (Chinese traditional medicine machine factory of Changde City).
Buy commercially available frangipanis medicinal material (originating in totally 11 batches, Guangdong, Guangxi, Yunnan, Hubei), be accredited as the dry flower of Apocynaceae frangipanis platymiscium frangipanis PlumeriarubraL. through Chinese medicine institute of Traditional Chinese Medicine University Of Guangzhou Zhao Bin post-doctor.15-demethyl plumieride (Yuan Mu bio tech ltd, Shanghai, CAS:132586-69-7).Acetonitrile is chromatographically pure (ProductofTedia, UnitedStatesofAmerica), and phosphoric acid is for analyzing pure (1Guanghua Chemical Plant Co., Ltd., Guangdong), and water is double distilled water, and it is pure that all the other agents useful for same are analysis.
2 chromatographic conditions and system flexibility
Agilent1200 high performance liquid chromatograph (VWD detecting device), KromasilC
18chromatographic column (250 × 4.6mm, 5 μm); Mobile phase is acetonitrile-0.5% phosphoric acid water (8:92), flow velocity: 1.0mL/min, isocratic elution 15min; Column temperature: 30 DEG C, determined wavelength: 210nm, sample size: 10 μ L.
Under this chromatographic condition, accurate absorption reference substance solution, each 10 μ L injection liquid chromatographies of need testing solution, record chromatogram.The results are shown in Figure 1:15-demethyl plumieride and go out peak at 11.1min, peak shape is symmetrical; In test sample chromatogram, corresponding position has corresponding peak occur, degree of separation is greater than 1.5, and theoretical cam curve (n) calculates should be not less than 6000 by 15-demethyl plumieride peak.
3 methodological studies
3.1 linear relationships are investigated
Precision takes 15-demethyl plumieride reference substance 5.0mg, is placed in the brown volumetric flask of 10.0mL, dissolves and be settled to scale with methyl alcohol, shake up for subsequent use.It is 0.0257mgmL that this storing solution of accurate absorption is configured to concentration respectively
-1, 0.0515mgmL
-1, 0.103mgmL
-1, 0.1545mgmL
-1,0.206mgmL
-1, 0.2575mgmL
-1reference substance solution.The each concentrations control product solution 10 μ L injection liquid chromatography of accurate absorption, measures by the chromatographic condition drafted, record peak area.With sample size X (μ g) for horizontal ordinate, peak area Y is ordinate mapping, and drawing standard curve, obtaining regression equation is: Y=933.01X+11.352 (r=0.9997).Result shows, 15-demethyl plumieride sample size, within the scope of 0.257 ~ 2.575 μ g, is good linear relationship with peak area.
3.2 precision test
The same reference substance liquid 10 μ L injection liquid chromatography of accurate absorption, continuous sample introduction 6 times, measure 15-demethyl plumieride peak area, RSD is 1.43%, shows that instrument precision is good.
3.3 replica test
Take same batch of medicinal material coarse powder 6 parts, every part of 0.2g, by the parallel preparation of test sample preparation method 6 parts of need testing solutions, accurate absorption 10 μ L injection liquid chromatographies respectively, record peak area, calculate 15-demethyl plumieride content, RSD is 0.62%, shows that the repeatability adopting the method to extract and detect is good.
3.4 stability test
The same need testing solution 10 μ L of accurate absorption, measures respectively at 0,2,4,6,8,12,24h sample introduction, record peak area, and calculate 15-demethyl plumieride content, RSD is 1.26%, shows that sample test liquid is stable in 24h.
3.5 recovery test
Take the medicinal material coarse powder 9 parts of known content (7.399mg/g), every part of about 0.1g, accurately weighed, be divided into 3 groups, often organizing precision respectively, to add concentration be 1.03mg/mL reference substance solution 0.35mL, 0.70mL, 1.05mL, then add 50% methyl alcohol to 25mL, weigh, ultrasonic extraction 30 minutes, cooling, more weighed weight, add the weight that 50% methyl alcohol supplies less loss, shake up, filter, filtrate filters with 0.45 μm of miillpore filter again, gets subsequent filtrate, to obtain final product.Accurate absorption 10 μ L sample introductions, measure peak area, calculate the recovery, the results are shown in Table 1.The mean sample recovery rate of high, medium and low concentration group is respectively 104.02%, 103.93%, 102.01%, RSD and is respectively 0.72%, 0.56%, 1.71% (n=9), shows that the method accuracy is high.
Table 1 average recovery is tested
▲ the recovery=100 × (measured amount-medicinal material content)/add reference substance amount
4 assays
The preparation of 4.1 reference substance solution
Get 15-demethyl plumieride reference substance appropriate, accurately weighed, add 50% methyl alcohol and make the solution of every 1mL containing 0.103mg, to obtain final product.
The preparation of 4.2 need testing solutions
Get medicinal material coarse powder and be about 0.2g, accurately weighed, put in tool plug conical flask, precision adds 50% methyl alcohol 25mL, weighed weight, ultrasonic extraction (100W, 40kHz) 30 minutes, cooling, more weighed weight, add the weight that 50% methyl alcohol supplies less loss, shake up, filter, filtrate filters with 0.45 μm of miillpore filter again, get subsequent filtrate, to obtain final product.
4.3 sample tests
Take the frangipanis medicinal material of separate sources respectively, by test sample, preparation method prepares sample solution, measure under above-mentioned chromatographic condition, one point external standard method is adopted to calculate the content of 15-demethyl plumieride, calculate according to dry product, measurement result is in table 2: in the frangipanis that is produced from Guangdong, the content of 15-demethyl plumieride is all very high, and the content that is produced from Guangxi takes second place, and the content very low (see Fig. 2) of Yunnan, Hubei product.
The content (unit: mg/gn=2) of 15-demethyl plumieride in table 2 separate sources frangipanis
▲ S1-S6 originates in Guangdong; S7-S9 originates in Guangxi; S10 originates in Yunnan; S11 originates in Hubei
5 discuss
The selection of 5.1 mensuration wavelength
Get 15-demethyl plumieride and add the solution that 50% methyl alcohol is made into debita spissitudo, carry out length scanning in 190 ~ 400nm, it has absorption maximum at 210nm place, therefore selected 210nm is as the mensuration wavelength of this method.
5.2 the selection of chromatographic condition
This test compares the mensuration situation of acetonitrile-water, acetonitrile-0.5% phosphoric acid water, acetonitrile-1.0% acetic acid water three flow phase system and different column temperature, different in flow rate, result shows to adopt acetonitrile-0.5% phosphoric acid water (8:92) to be mobile phase, and column temperature is that the chromatographic peak degree of separation measured under the flow velocity of 30 DEG C and 1.0mL/min is good, peak shape is symmetrical.
The selection of 5.3 test sample preparation methods
5.3.1 the selection of Extraction solvent
Select in test methyl alcohol, 50% methyl alcohol, ethanol and 50% ethanol to test as Extraction solvent, evaluate its extraction efficiency, test method is as follows:
Methyl alcohol test liquid: get the sample meal being numbered S2 and be about 0.2g, accurately weighed, put in tool plug conical flask, precision adds methyl alcohol 25mL, and close plug, weighs, ultrasonic process (100W, 40kHz) 30 minutes, after cooling, weighed weight again, add the weight that methyl alcohol supplies less loss, shake up, filter, get subsequent filtrate, to obtain final product.
50% methyl alcohol test liquid: get the sample meal being numbered S2 and be about 0.2g, accurately weighed, put in tool plug conical flask, precision adds 50% methyl alcohol 25mL, and all the other operations are the same.
Ethanol test liquid: get the sample meal being numbered S2 and be about 0.2g, accurately weighed, put in tool plug conical flask, precision adds ethanol 25mL, and all the other operations are the same.
50% ethanol test liquid: get the sample meal being numbered S2 and be about 0.2g, accurately weighed, put in tool plug conical flask, precision adds 50% ethanol 25mL, and all the other operations are the same.
The each 10 μ L of the above-mentioned need testing solution of accurate absorption respectively, injection liquid chromatography, record peak area, calculate 15-demethyl plumieride content, measurement result is in table 3.
Table 3 Extraction solvent investigates result
Test findings shows: the extraction efficiency of 50% methyl alcohol is the highest; and from chromatogram; the chromatogram peak shape that during 50% ethanol as solvent, extraction obtains is too wide and assorted peak many, is unfavorable for the protection of chromatographic column, therefore selects 50% methyl alcohol as Extraction solvent in this method.
5.3.2 the selection of extracting method
Get the sample meal two parts being numbered S2, every part of about 0.2g, accurately weighed, precision adds 50% methyl alcohol 25mL respectively, a refluxing extraction 1 hour, and a ultrasonic extraction 30 minutes, measures the content of its 15-demethyl plumieride.Measurement result is in table 4.
Table 4 extracting method investigates result
Test findings shows: the 15-demethyl plumieride content that ultrasonic extraction obtains obtains height than refluxing extraction, and easy to operate, and required time is shorter, therefore selects ultrasonic extraction in this method.
5.3.3 the selection of extraction time
Get the sample meal three parts being numbered S2, every part of about 0.2g, accurately weighed, precision adds 50% methyl alcohol 25mL respectively, compares test to different ultrasonic time, and ultrasonic time is respectively 15,30,60 minutes, measure the content of its 15-demethyl plumieride, measurement result is in table 5.
Table 5 ultrasonic time investigates result
Test findings shows: sample ultrasonic extraction is after 30 minutes, and 15-demethyl plumieride can extract completely substantially, therefore ultrasonic time is defined as 30 minutes.
In sum, need testing solution is preparation method be defined as: get medicinal material coarse powder and be about 0.2g, accurately weighed, put in tool plug conical flask, precision adds 50% methyl alcohol 25mL, weighed weight, ultrasonic process (100W, 40kHz) 30 minutes, cooling, weighed weight again, adds the weight that 50% methyl alcohol supplies less loss, shakes up, filter, filtrate filters with 0.45 μm of miillpore filter again, gets subsequent filtrate, to obtain final product.
The content of 15-demethyl plumieride in 5.4 measurings, 11 batches of frangipanis medicinal materials, result shows, the identical place of production but have certain difference from the content of 15-demethyl plumieride in the frangipanis medicinal material of different manufacturers, this may with the collecting time of medicinal material, Preparation process method and to store keeping relevant.Between the frangipanis medicinal material that Different sources produces there is larger difference in the content of 15-demethyl plumieride.From content average figure, in Different sources frangipanis medicinal material, the order of content height is: Guangdong, Guangxi, Yunnan, Hubei.This may be relevant with factors such as the edaphic condition in the medicinal material place of production, fertilizer, weather, temperature.In view of the feature of this result of study, in order to formulate more rational content measuring standard to frangipanis medicinal material, still needing and will increase the analysis of sample size further experiment and wish to optimize the processing procedure of frangipanis, for ensureing that quality of medicinal material provides safeguard.
Claims (3)
1. one kind is detected the method for frangipanis medicinal material or Flos Plumeriae Acutifoliae extract quality, it is characterized in that: it adopts HPLC method to detect the dry flower of Apocynaceae frangipanis platymiscium frangipanis PlumeriarubraL., the quality of its extract, high performance liquid chromatography is adopted to measure, chromatographic condition is: with Octadecylsilane bonded phase silica gel for filling agent, with acetonitrile-0.5% phosphoric acid water, volume ratio 8:92 is mobile phase, and determined wavelength is 210nm.
2. the method for detection frangipanis medicinal material according to claim 1 or Flos Plumeriae Acutifoliae extract quality, is characterized in that: described chromatographic condition is: Agilent1200 high performance liquid chromatograph, KromasilC18 chromatographic column 250 × 4.6mm, 5 μm; Mobile phase is acetonitrile-0.5% phosphoric acid water, volume ratio 8:92, flow velocity: 1.0mL/min, isocratic elution 15min; Column temperature: 30 DEG C, determined wavelength: 210nm, sample size: 10 μ L.
3. the method for detection frangipanis medicinal material according to claim 1 and 2 or Flos Plumeriae Acutifoliae extract quality, is characterized in that: it comprises the steps:
The preparation of a, reference substance solution:
Get 15-demethyl plumieride reference substance appropriate, accurately weighed, add 50% methyl alcohol and make the solution of every 1mL containing 0.103mg, to obtain final product;
The preparation of b, need testing solution
Get medicinal material coarse powder 0.2g, accurately weighed, put in tool plug conical flask, precision adds 50% methyl alcohol 25mL, weighed weight, ultrasonic extraction, ultrasound condition 100W, 40kHz, ultrasonic 30 minutes, cooling, more weighed weight, add the weight that 50% methyl alcohol supplies less loss, shake up, filter, filtrate filters with 0.45 μm of miillpore filter again, get subsequent filtrate, to obtain final product;
C, by described in claim 1 or 2 chromatographic condition detect.
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| CN104458933A (en) | 2015-03-25 |
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Inventor after: Xu Wenliu Inventor after: Weng Shaoquan Inventor after: Zheng Rongbo Inventor after: Li Cizhou Inventor after: Zhang Fengyuan Inventor before: Zhao Bin Inventor before: Deng Xianmei Inventor before: Li Rong Inventor before: Liu Jing Inventor before: Wang Qiong Inventor before: Liu Ruina |
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Effective date of registration: 20161014 Address after: 511458, room 93, 498 Jinling North Road, Guangdong, Guangzhou, Nansha District Patentee after: GUANGZHOU WANGLAOJI MAJOR HEALTH INDUSTRY CO., LTD. Address before: 528436, Guangdong Torch Development Zone, Zhongshan Port Road, Zhongshan Province Patentee before: Zhongshan Torch Polytechnic College Patentee before: Zhao Bin |