CN104897806B - Judge Flos Chrysanthemi whether through the HPLC detection method of stove drying - Google Patents
Judge Flos Chrysanthemi whether through the HPLC detection method of stove drying Download PDFInfo
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- CN104897806B CN104897806B CN201510247076.9A CN201510247076A CN104897806B CN 104897806 B CN104897806 B CN 104897806B CN 201510247076 A CN201510247076 A CN 201510247076A CN 104897806 B CN104897806 B CN 104897806B
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Abstract
The invention discloses judging Flos Chrysanthemi whether through the HPLC detection method of stove drying.The method includes：(1) utilize the extraction with aqueous solution Flos Chrysanthemi to be detected of water, alcohol or alcohol, to obtain test sample；(2) HPLC is utilized to detect described test sample, chromatographic condition is as follows：Chromatographic column：C18Chromatographic column；Detection wavelength：350±5nm；Mobile phase：A：Acetonitrile or methanol, B：Solution containing 0.05 0.2 volume % organic acid, gradient elution program：0～10min, 12～16%A；10～11min, 16～20%A；11～25min, 20～26%A；25～55min, 26%～65%A.Using method of the present invention detection Flos Chrysanthemi whether through stove drying, appearance time is early, only 20 minutes about with regard to appearance, the run time of detection is short, only need 50 minutes about, and discrepant chromatographic peak before and after more than 15 stove dryings can be symbolized simultaneously, save considerably reagent dosage and manpower, and the baseline stability of HPLC detection, object separating degree are good, thus reach using HPLC quick, accurately judge Flos Chrysanthemi whether through the purpose of stove drying.
Description
Technical field
The present invention relates to whether Flos Chrysanthemi is through the detection method of stove drying, in particular it relates to whether Flos Chrysanthemi is through stove drying
HPLC detection method.
Background technology
Flos Chrysanthemi is the dry capitulum of feverfew Flos Chrysanthemi (Chrysanthemum morifolium Ramat), and tool is dredged
Wind, heat clearing away, improving eyesight, merit of removing toxic substances effect.Tea uses, medicinal all suitable, and tea use can be reduced internal heat, nourishing the liver to improve visual acuity, medicinal can antibacterial, antiinflammatory, fall
Pressure, anti-coronary heart disease etc., using value is high.The various in recent years health tea beverage exploitations with Flos Chrysanthemi as raw material and listing, Flos Chrysanthemi is former
Material demand surges.Sulfur fumigation tool is dried, bleaching, insect protected and anti-mildew, extend the effect such as storage phase.Due to stove drying possess with
Upper " beauty treatment " effect, can make medical material appearance color vivid, cater to Popular Aesthetics demand.In recent years, by the economy of medical material grade
Interests are ordered about, and Flos Chrysanthemi also becomes one of large kind of conventional sulfur fumigation processing.But the Flos Chrysanthemi flavour of a drug after sulfur fumigation can become
Acid, causes main component loss to affect clinical efficacy, and remaining sulfur dioxide simultaneously causes toxicity to be superimposed.Research finds, sulfur
Can be combined with oxygen during stifling, produce sulfur dioxide, sulfur dioxide is harmful material, and Long Term Contact can cause to glue
Theca cell produces variation, has serious detrimental effect to the respiratory mucosa of human body, gastrointestinal mucosal, hepatic and renal function is also had directly
Connect impact.During processing of crude drugs, expired medical material is fumigated repeatedly, or even directly sprays sulfur, has had a strong impact on medical material quanlity；
" sulfur dioxide event " was once propagandizing " tripolycyanamide " into Chinese herbal medicine circle hotly, becomes the focal issue threatening public health, draws
Play social extensive concern.The consideration Ji Yu TBT (TBT (Technical Barriers to Trade)) for the Korea S, takes the lead in formulating sulfur dioxide residue standard, causes
Make sulfur in recent years smoke event to be paid high attention to.
At present, conventional HPLC detects Flos Chrysanthemi whether through the method for stove drying, and detection time-histories is long, and nearly 100 minutes, gradient was washed
De- baseline drift, causes integration difficult, the repeatability of sample determination result, accuracy equal difference.
Therefore, this area is in the urgent need to providing the HPLC detection side that a kind of run time is short, baseline stability, separating degree are good
Method.
Content of the invention
It is contemplated that at least solving one of technical problem present in prior art.For this reason, one object of the present invention
It is to propose that a kind of run time is short, baseline stability, separating degree are good judges Flos Chrysanthemi whether through the HPLC detection side of stove drying
Method.
Thus, according to an aspect of the present invention, the invention provides whether a kind of judge Flos Chrysanthemi through the HPLC of stove drying
Detection method.According to embodiments of the invention, this includes：(1) utilize the extraction with aqueous solution Flos Chrysanthemi to be detected of water, alcohol or alcohol, with
Just obtain test sample；(2) HPLC is utilized to detect described test sample, chromatographic condition is as follows：Chromatographic column：C18Chromatographic column；Detection
Wavelength：350±5nm；Mobile phase：A：Acetonitrile or methanol, B：Solution containing 0.05-0.2 volume % organic acid, gradient elution journey
Sequence：0～10min, 12～16%A；10～11min, 16～20%A；11～25min, 20～26%A；25～55min, 26%
～65%A.
Inventor has surprisingly found that, whether using method of the present invention detection Flos Chrysanthemi through stove drying, appearance time is early, only 20
About minute with regard to appearance, the run time of detection short it is only necessary to 50 minutes about, and more than 15 stove dryings can be symbolized simultaneously
Discrepant chromatographic peak in front and back, save considerably reagent dosage and manpower, and the baseline stability of HPLC detection, object separate
Degree is good, thus reach using HPLC quick, accurately judge Flos Chrysanthemi whether through the purpose of stove drying.
In addition, according to the above embodiment of the present invention judge Flos Chrysanthemi whether through the HPLC detection method of stove drying, acceptable
There is the technical characteristic adding as follows：
According to embodiments of the invention, the flow velocity of described mobile phase is 1.0mL min-1.Thus, the more other flow velocity of peak type
There is improvement, sample appearance speed is accelerated.
According to embodiments of the invention, the aqueous solution of described alcohol or alcohol is the aqueous solution of methanol or methanol.Thus, to Flos Chrysanthemi
Composition extraction effect good.
According to embodiments of the invention, described organic acid is selected from least one of formic acid, acetic acid and phosphoric acid.Thus, to be measured
Thing and the good separating effect of impurity peaks.Preferably, described organic acid is formic acid.Thus, the separating effect of determinand and impurity peaks
More preferably.
According to embodiments of the invention, described Flos Chrysanthemi is Flos Chrysanthemi and Flos Chrysanthemi.Thereby, it is possible to fast and accurately judge Hangzhoupro
Whether Flos Chrysanthemi and Flos Chrysanthemi are through stove drying.
According to embodiments of the invention, the concentration of described organic acid is 0.1 volume %.Thus, peak type is significantly improved, peak
Separating degree and peak between improves.
According to embodiments of the invention, the column temperature of described chromatographic column is 25 ± 5 degrees Celsius.Thus, peak conditions of streaking improves,
The symmetrical degree in peak improves.According to embodiments of the invention, the size of described chromatographic column is 4.6mm × 250mm, 5 μm.Thus,
Between each peak of sample, separating degree can meet the requirement of qualitative identification
According to embodiments of the invention, the methanol concentration of described methanol aqueous solution is 40-80 volume %.Thus, to Flos Chrysanthemi
The extraction effect of contained Organic substance is good.Preferably, the methanol concentration of described methanol aqueous solution is 60 volumes %.Thus, right
The extraction effect of the Organic substance contained by Flos Chrysanthemi is more preferably.
According to embodiments of the invention, in step (1), the method for described extraction is selected from backflow, ultrasonic, dipping or percolation.
Thereby, it is possible to the sufficient Organic substance extracting contained by Flos Chrysanthemi.
According to embodiments of the invention, in step (2), further include：Choose chlorogenic acid, luteoloside, isochlorogenic acid
At least one of A, linarin, luteolin, apigenin, diosmetin and acacetin standard substance are as reference substance.Thus, lead to
Cross the detection to the above-mentioned effective ingredient appearance time in Flos Chrysanthemi and relative amount, can accurately judge Flos Chrysanthemi whether through over cure
Smoked.
The additional aspect of the present invention and advantage will be set forth in part in the description, and partly will become from the following description
Obtain substantially, or recognized by the practice of the present invention.
Brief description
The above-mentioned and/or additional aspect of the present invention and advantage will become from reference to the description to embodiment for the accompanying drawings below
Substantially and easy to understand, wherein：
Fig. 1 shows stove drying according to an embodiment of the invention and does not smoke Flos Chrysanthemi sample HPLC mirror image figure, wherein, A
For Flos Chrysanthemi through stove drying sample, B is Flos Chrysanthemi without stove drying hot air drying sample；
Fig. 2 shows the HPLC chromatogram of mixed mark reference substance according to an embodiment of the invention, wherein a-h chromatographic peak pair
The compound answered is respectively：a:Chlorogenic acid, b：Luteoloside, c：3,5-Dicaffeoylquinic acid, d：Linarin, e：Luteolin, f：Herba Apii graveolentis
Element, g：Diosmetin and h：Acacetin；
Fig. 3 shows 5 batches of different sources hot air drying Flos Chrysanthemi sample HPLC chromatogram according to an embodiment of the invention
Figure；
Fig. 4 shows 5 batches of Flos Chrysanthemi stove drying sample HPLC chromatogram according to an embodiment of the invention；
Fig. 5 shows stove drying according to an embodiment of the invention and does not smoke Flos Chrysanthemi sample HPLC mirror image figure, wherein, A is
Through stove drying sample, B is Flos Chrysanthemi without stove drying hot air drying sample to Flos Chrysanthemi；
Fig. 6 shows 5 batches of different sources hot air drying Flos Chrysanthemi sample HPLC chromatogram according to an embodiment of the invention；
And
Fig. 7 shows that Flos Chrysanthemi sample HPLC chromatogram is processed in 5 batches of different sources stove dryings according to an embodiment of the invention.
Specific embodiment
Embodiments of the invention are described below in detail, the example of described embodiment is shown in the drawings, wherein from start to finish
The element that same or similar label represents same or similar element or has same or like function.Below with reference to attached
The embodiment of figure description is exemplary, is only used for explaining the present invention, and is not considered as limiting the invention.
According to an aspect of the present invention, the invention provides whether a kind of judge Flos Chrysanthemi through the HPLC detection side of stove drying
Method.According to embodiments of the invention, this includes：(1) utilize the extraction with aqueous solution Flos Chrysanthemi to be detected of water, alcohol or alcohol, to obtain
Test sample；(2) HPLC is utilized to detect described test sample, chromatographic condition is as follows：Chromatographic column：C18Chromatographic column；Detection wavelength：
350±5nm；Mobile phase：A：Acetonitrile, B：Solution containing 0.05-0.2 volume % organic acid, gradient elution program：0～
10min, 12～16%A；10～11min, 16～20%A；11～25min, 20～26%A；25～55min, 26%～65%
A.
Inventor has surprisingly found that, whether using method of the present invention detection Flos Chrysanthemi through stove drying, appearance time is early, only 20
Reagent dosage and manpower is save considerably with regard to appearance, the run time of detection are short it is only necessary to 50 minutes about about minute, and
The baseline stability of HPLC detection, object separating degree are good, thus reach quickly, accurately judging whether Flos Chrysanthemi passes through using HPLC
The purpose of stove drying.
According to embodiments of the invention, the flow velocity of described mobile phase is 1.0mL min-1.Thus, the more other flow velocity of peak type
There is improvement, sample appearance speed is accelerated.According to embodiments of the invention, the species of described organic acid is not particularly limited, only
Can be used for separating target peak and the impurity peaks of Flos Chrysanthemi.Preferably, described organic acid is selected from formic acid, acetic acid and phosphoric acid extremely
One of few.Thus, the good separating effect of determinand and impurity peaks.It is further preferred that described organic acid is formic acid.Thus, treat
The separating effect of survey thing and impurity peaks is more preferably.
According to embodiments of the invention, described Flos Chrysanthemi is Flos Chrysanthemi and Flos Chrysanthemi.Thereby, it is possible to fast and accurately judge Hangzhoupro
Whether Flos Chrysanthemi and Flos Chrysanthemi are through stove drying.
According to embodiments of the invention, the concentration of described organic acid is 0.1 volume %.Thus, peak type is obviously improved, peak with
Separating degree between peak improves.According to embodiments of the invention, the column temperature of described chromatographic column is 25 ± 5 degrees Celsius.Thus, peak drags
Tail phenomenon is improved, and the symmetrical degree in peak improves.
According to embodiments of the invention, the size of described chromatographic column is 4.6mm × 250mm, 5 μm.Thus, peak conditions of streaking
Improve, the symmetrical degree in peak improves.According to embodiments of the invention, the methanol concentration of described methanol aqueous solution is 40-80 body
Long-pending %.Thus, good to the extraction effect of the Organic substance contained by Flos Chrysanthemi.Preferably, the methanol concentration of described methanol aqueous solution is
For 60 volumes %.Thus, to the extraction effect of the Organic substance contained by Flos Chrysanthemi more preferably.
According to embodiments of the invention, in step (1), the method for described extraction is selected from backflow, ultrasonic, dipping or percolation.
Thereby, it is possible to the sufficient Organic substance extracting contained by Flos Chrysanthemi.
According to embodiments of the invention, in step (2), further include：Choose chlorogenic acid, luteoloside, isochlorogenic acid
At least one of A, linarin, luteolin, apigenin, diosmetin and acacetin standard substance are as reference substance.Thus, lead to
Cross the detection to above-mentioned content of organics, can accurately judge Flos Chrysanthemi whether through stove drying.
Below with reference to specific embodiment, the present invention will be described, it should be noted that these embodiments are only explanation
Property, and be not considered as limiting the invention.
Below in conjunction with embodiment, the solution of the present invention is explained.It will be understood to those of skill in the art that it is following
Embodiment is merely to illustrate the present invention, and should not be taken as limiting the scope of the invention.Unreceipted particular technique or bar in embodiment
Part, carry out according to the technology described by document in the art or condition or according to product description.Agents useful for same or instrument
The unreceipted production firm person of device, be can by city available from conventional products, for example can purchase from Sigma company.
Embodiment 1
Using the method for the present invention, to the multiple stove dryings directly collected from each Genuine producing area and the Flos Chrysanthemi do not smoked and and Bo
Chrysanthemum is detected, whether judges Flos Chrysanthemi through stove drying, specific as follows：
1 material
1.1 experimental apparatus
Agilent 1260 highly effective liquid phase chromatographic system, chromatographic column Diamonsil C18(4.6mm × 250mm, 5 μm).
1.2 reagent and medical material
Chlorogenic acid (CA), luteolin (L) (are all purchased from National Institute for Food and Drugs Control, lot number is respectively：
110753-200413 and 111520-200504)；Luteoloside (L-7G), 3,5-Dicaffeoylquinic acid (3,5-diCQA), linarin (Li),
Apigenin (A), diosmetin (D) and acacetin (Ac) (be all purchased from Shanghai and contain Chinese medicine Chemical Co., Ltd.)；Acetonitrile
(Fisher)；Wahaha Pure Water, it is pure that remaining reagent is analysis.
Flos Chrysanthemi sample is directly collected for equal 2012 and 2014 from Genuine producing area, and wherein the collection place of production of Flos Chrysanthemi is Zhejiang paulownia
Township, Jiangsu Coastal, shining sun etc., the collection place of production of Flos Chrysanthemi is Hui nationality Shi Jiuli town, and the place of production of Flos Chrysanthemi and batch information refer to
Table 1.
The place of production of table 1 different batches Flos Chrysanthemi and acquisition time
2 methods
The preparation of 2.1 need testing solutions
Weigh various Flos Chrysanthemi stove drying samples in table 1 respectively, do not smoke sample, Flos Chrysanthemi stove drying sample, smoked sample (cross 40 mesh
Sieve) each 0.5g, accurate addition 60% methanol 20ml, supersound process 30min (power 100W, 25 DEG C of temperature), cross 0.22 μm of micropore
Filter membrane, obtains final product each test sample.
Precision weighs chlorogenic acid, luteoloside, 3,5-Dicaffeoylquinic acid, linarin, sweet-scented osmanthus respectively for the preparation of 2.2 reference substance solution
Careless element, apigenin, diosmetin, acacetin reference substance are appropriate, with methanol dissolving simultaneously constant volume, make 0.1mg mL-1Ambiguity
The reference substance solution of standardization product, put 4 DEG C standby.
2.3HPLC chromatographic condition
Chromatographic column：Diamonsil C18 (4.6mm × 250mm, 5 μm)
Mobile phase：A：Acetonitrile, B：0.1% aqueous formic acid carries out gradient elution, 0～10min, 12～16%A；10～
11min, 16～20%A；11～25min, 20～26%A；25～55min, 26%～65%A
Flow velocity：1.0mL·min-1
Sample size：10μL
Column temperature：25℃
Detection wavelength：350nm
3 results and discussion
3.1 stove dryings and the HPLC trace analysis of non-smoked Flos Chrysanthemi sample
By 2.1 lower section legal system available test sample solutions, and it is measured according to 2.3 lower chromatographic conditions.HPLC is to Hang Bai
The testing result of chrysanthemum is as follows：
(1) stove drying and no sulfur Flos Chrysanthemi composition transfer detection
Detection stove drying and no sulfur Flos Chrysanthemi sample respectively, and reference substance, stove drying and the non-stove drying Flos Chrysanthemi of 2.2 configurations
Result as shown in the mirror image HPLC chromatogram of Fig. 1, top be stove drying Flos Chrysanthemi sample, bottom is the Flos Chrysanthemi sample of non-stove drying
Product, i.e. non-stove drying Flos Chrysanthemi, (sample number into spectrum is respectively：Flos Chrysanthemi HJ- has S12, Flos Chrysanthemi HJ- no S7), can be clearly from Fig. 1
Go out, sulfur fumigation method is larger on the chemical composition impact of Flos Chrysanthemi, and the big polar component in Flos Chrysanthemi after sulfur fumigation is (during reservation
Between composition between 0-34 minute, Fig. 1 center line 1 left side composition) and content reduce, and little polar component (retention time 34-55 is divided
Composition between clock, Fig. 1 center line 1 right side composition) and content raised.By the HPLC collection of illustrative plates with the standard substance shown in Fig. 2
Compare, the composition of the chromatographic peak that above-mentioned content changes is confirmed, find through comparing, in Flos Chrysanthemi after stove drying
Luteoloside and linarin equal size substantially reduce, and the content of luteolin significantly increases, meanwhile, apigenin, diosmetin
And 3 kinds of compounds of acacetin are having detection in stove drying sample, and content is higher, and in the Flos Chrysanthemi of non-stove drying not
It is detected.
(2) non-stove drying Flos Chrysanthemi detection
Detect 5 batches of non-stove drying Flos Chrysanthemi samples of different sources respectively, that is, (sample number into spectrum is respectively table to non-stove drying Flos Chrysanthemi
HJ- in 1 no S1, HJ- no S3, HJ- no S4, HJ- no S5, HJ- no S7；), result as described in Figure 3, though sample is collected from not
The same place of production, different year, but the chromatogram repeatability of 5 batch samples is good, it is indicated above that the HPLC detection side that the present invention is set up
Method can be used for characterizing no sulfur Flos Chrysanthemi chemical component fingerprint profile.
(3) stove drying Flos Chrysanthemi detection
(HJ- that sample number into spectrum is respectively in table 1 has S12, HJ- to 5 batches of stove drying Flos Chrysanthemi samples of detection different sources respectively
S13, HJ- is had to have S13, HJ- to have S14, HJ- to have S19), though the result of HPLC detection is as shown in figure 4, sample is collected from different products
Ground, different year, but 5 batch sample chromatogram repeatability are good, it is indicated above that it is one that stove drying leads to the conversion of Flos Chrysanthemi chemical composition
Plant irreversible chemical reaction, and between different batches, repeatability is good, the HPLC chromatogram authentication method set up herein, Neng Gouyong
Flos Chrysanthemi chemical component fingerprint after characterizing stove drying.
3.2 stove dryings and the HPLC trace analysis of non-smoked Flos Chrysanthemi sample
By 2.1 lower section legal system available test sample solutions, and it is measured according to 2.3 lower chromatographic conditions.HPLC is to Flos Chrysanthemi
Testing result as follows：
(1) detection of stove drying and no sulfur Flos Chrysanthemi sample
Respectively detection stove drying and no sulfur Flos Chrysanthemi sample (BJ- no S3, BJ- no S4, the BJ- no S5 in sample such as table 1, BJ- is no
S8, BJ- no S9, BJ- have S1, BJ- to have S2, BJ- to have S3, BJ- to have S6, BJ- to have S9), and the reference substance of 2.2 configurations, its
In, as shown in figure 5, top is stove drying Flos Chrysanthemi sample, bottom is no sulfur Flos Chrysanthemi sample for stove drying and no sulfur Flos Chrysanthemi sample result.From figure
5 can clearly find out, sulfur fumigation method affects larger on the chemical composition of Flos Chrysanthemi.Big polarity in Flos Chrysanthemi after sulfur fumigation
Composition (composition between retention time 0-34 minute, Fig. 5 center line 1 left side composition) and content reduce, and little polar component (retains
Composition between time 34-55 minute, Fig. 5 center line 2 right side composition) and content raised.By with the standard substance shown in Fig. 2
HPLC collection of illustrative plates compare, the composition of the chromatographic peak that above-mentioned content changes is confirmed, through compare find, after stove drying
Luteoloside in Flos Chrysanthemi and linarin equal size substantially reduce, and luteolin, apigenin, diosmetin and acacetin 4
The content planting flavone aglycone all significantly increases.
(2) non-stove drying Flos Chrysanthemi detection
(sample number into spectrum is respectively the BJ- no S3 in table 1 to 5 batches of detection different sources no sulfur Flos Chrysanthemi sample, and BJ- is no respectively
S4, BJ- no S5, BJ- no S8, BJ- no S9), i.e. no sulfur Flos Chrysanthemi, though HPLC testing result is as shown in fig. 6, sample is collected from not
The same place of production, different year, but each batch sample chromatogram repeatability is good, it is indicated above that the method set up herein can be used for
Characterize Flos Chrysanthemi chemical component fingerprint profile.
(3) stove drying Flos Chrysanthemi detection
(BJ- that sample number into spectrum is respectively in table 1 has S1, BJ- to have to 5 batches of stove drying Flos Chrysanthemi samples of detection different sources respectively
S2, BJ- have S3, BJ- to have S6, BJ- to have S9), though HPLC testing result is as shown in fig. 7, sample is collected from different sources, not the same year
Part, but 5 batch sample chromatogram repeatability are good, it is indicated above that it is a kind of irreversible that stove drying leads to the conversion of Flos Chrysanthemi chemical composition
Between chemical reaction, and different batches, repeatability is good, the HPLC chromatogram authentication method set up herein, can be used in characterizing stove drying
Flos Chrysanthemi chemical component fingerprint afterwards.
In sum, using the method for the present invention, Flos Chrysanthemi can fast and accurately be judged whether through stove drying, and chrysanthemum
The HPLC chromatogram repeatability of flower is good, can be used for characterizing Flos Chrysanthemi chemical component fingerprint profile.
In the description of this specification, reference term " embodiment ", " some embodiments ", " example ", " specifically show
The description of example " or " some examples " etc. means specific features, structure, material or the spy describing with reference to this embodiment or example
Point is contained at least one embodiment or the example of the present invention.In this manual, to the schematic representation of above-mentioned term not
Necessarily refer to identical embodiment or example.And, the specific features of description, structure, material or feature can be any
One or more embodiments or example in combine in an appropriate manner.
Although an embodiment of the present invention has been shown and described, it will be understood by those skilled in the art that：Not
Multiple changes, modification, replacement and modification can be carried out to these embodiments in the case of the principle of the disengaging present invention and objective, this
The scope of invention is limited by claim and its equivalent.
Claims (1)
1. a kind of judge Flos Chrysanthemi whether through stove drying HPLC detection method it is characterised in that described Flos Chrysanthemi is Flos Chrysanthemi and Bo
Chrysanthemum, methods described includes：
(1) 60 volume % methanol solutions are utilized to extract Flos Chrysanthemi to be detected, to obtain test sample, wherein, the side of described extraction
Method is selected from backflow, ultrasonic, dipping or percolation；
(2) HPLC is utilized to detect described test sample, chromatographic condition is as follows：
Chromatographic column：C18Chromatographic column；Column temperature is 25 ± 5 degrees Celsius；A size of 4.6mm × 250mm, 5 μm
Detection wavelength：350±5nm
Mobile phase：A：Acetonitrile or methanol, B：Solution containing 0.1 volume % formic acid, gradient elution program：0～10min, 12～
16%A；10～11min, 16～20%A；11～25min, 20～26%A；25～55min, 26%～65%A,
The flow velocity of described mobile phase is 1.0mL min-1,
Choose chlorogenic acid, luteoloside, 3,5-Dicaffeoylquinic acid, linarin, luteolin, apigenin, diosmetin and acacetin mark
At least one of quasi- product are as reference substance.
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| CN105486766A (en) * | 2015-10-13 | 2016-04-13 | 华南理工大学 | Method for determining content of three antioxidation active compositions in honeysuckle flower and plant thereof by employing HPLC |
| CN106769987A (en) * | 2017-01-22 | 2017-05-31 | 北京中医药大学 | It is a kind of distinguish the tuber of dwarf lilyturf medicinal material whether by stove drying method |
| CN108896673B (en) * | 2018-06-25 | 2021-08-24 | 贵州中医药大学 | Method for determining content of chlorogenic acid, luteolin and apigenin in spider fruits |
| CN113311085B (en) * | 2021-05-25 | 2022-05-13 | 广州白云山星群(药业)股份有限公司 | Method for measuring content of chlorogenic acid and linarin in wild chrysanthemum granules |
| CN114047264B (en) * | 2021-11-02 | 2023-06-02 | 中国中医科学院中药研究所 | Method for rapidly identifying sulfur-fumigated radix angelicae |
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| KR20070094158A (en) * | 2006-03-16 | 2007-09-20 | 재단법인서울대학교산학협력재단 | Determination of imidacloprid and maximum residue level in crown daisy by using direct competitive elisa |
| JP5275898B2 (en) * | 2009-05-21 | 2013-08-28 | ポーラ化成工業株式会社 | Evaluation method of skin condition |
| CN102928523B (en) * | 2011-08-11 | 2014-07-30 | 上海雷允上药业有限公司 | Wild chrysanthemum flower fingerprint determination method, its application, and wild chrysanthemum flower quality detection method |
| CN102706978B (en) * | 2012-06-01 | 2013-10-02 | 北京市药品检验所 | Wild chrysanthemum flower extractive and fingerprint spectrum detection method thereof |
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