CN105954405A - Method for determination of pectolinarin in buddleja officinalis - Google Patents
Method for determination of pectolinarin in buddleja officinalis Download PDFInfo
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- CN105954405A CN105954405A CN201610268591.XA CN201610268591A CN105954405A CN 105954405 A CN105954405 A CN 105954405A CN 201610268591 A CN201610268591 A CN 201610268591A CN 105954405 A CN105954405 A CN 105954405A
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- extraction
- pectolinarin
- flos buddlejae
- assay method
- methanol
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- G—PHYSICS
- G01—MEASURING; TESTING
- 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
- G01N30/02—Column chromatography
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- G—PHYSICS
- G01—MEASURING; TESTING
- 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
- G01N30/02—Column chromatography
- G01N30/04—Preparation or injection of sample to be analysed
- G01N30/06—Preparation
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- G—PHYSICS
- G01—MEASURING; TESTING
- 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
- G01N30/02—Column chromatography
- G01N2030/022—Column chromatography characterised by the kind of separation mechanism
- G01N2030/027—Liquid chromatography
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- G—PHYSICS
- G01—MEASURING; TESTING
- 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
- G01N30/02—Column chromatography
- G01N30/04—Preparation or injection of sample to be analysed
- G01N30/06—Preparation
- G01N2030/062—Preparation extracting sample from raw material
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Abstract
The invention discloses a method for determination of pectolinarin in buddleja officinalis, wherein the method comprises the following steps: step 1, crushing the buddleja officinalis, then sieving, weighing 0.5 part by weight of the buddleja officinalis powder, mixing evenly with 0.5 part by weight of diatomite, and in an extraction pool in which a filter film is pre-placed, adding a proper amount of diatomite until the diatomite reaches a pool port of the extraction pool; covering with a lid of the extraction pool, and extracting the mixture in the extraction pool, wherein the extraction comprises a deestering step and an extraction step; step 2, diluting the extract liquid with methanol, and then carrying out centrifugal separation to obtain a supernatant; and step 3, analyzing the supernatant by liquid chromatography. The method for determination of the pectolinarin in the buddleja officinalis is provided and has the advantages of simple operation and high detection accuracy.
Description
Technical field
The present invention relates to test in laboratory field, the assay method of Pectolinarin in a kind of Flos Buddlejae.
Background technology
Within 2015, pharmacopeia have recorded the method for linarin in Flos Buddlejae of extracting: takes this product coarse powder about 0.5g, accurately weighed, puts
In apparatus,Soxhlet's, adding petroleum ether (60～90 DEG C) 100ml, be heated to reflux 2 hours, discard petroleum ether, medicinal residues volatilize,
Adding methanol 100ml again to continue to be heated to reflux 4 hours, extracting solution is put in evaporating dish, is concentrated into appropriate, is transferred to 50ml amount
In Ping, residue and container wash with a small amount of methanol, and washing liquid is incorporated in same measuring bottle. and add methanol to scale, shake up, filter,
Take subsequent filtrate, to obtain final product.Under 15000r/min, centrifugal 3min, takes supernatant, enters LC and measures.
The parameter of its liquid chromatograph is: with octadecylsilane chemically bonded silica as filler；With methanol-0.1% glacial acetic acid (48:
52) for flowing phase；Detection wavelength is 326nm.
Describe that " HPLC method measures Flos Buddlejae in Radix Cirsii Japonici granule Hunan Journal of Traditional Chinese Medicine the 6th phase of volume 29 in June, 2013
Glycosides and the content of Pectolinarin ", it uses the linarin in ultrasonic dissolution Radix Cirsii Japonici granule and Pectolinarin, and adopts
Linarin therein and Pectolinarin is extracted by high performance liquid chromatography.
The method operation that pharmacopeia and " HPLC method measures linarin and the content of Pectolinarin in Radix Cirsii Japonici granule " are recorded
Process is complicated, and the operant skill of operator is required height.
Summary of the invention
It is an object of the invention to provide the assay method of Pectolinarin in a kind of Flos Buddlejae, the method is simple to operate, detection essence
Degree height.
The technical scheme that the present invention provides is the assay method of Pectolinarin in a kind of Flos Buddlejae, comprises the following steps:
Step 1: by Flos Buddlejae grinding and sieving, weighs 0.5 weight portion Flos Buddlejae powder, mixes with 0.5 weight portion kieselguhr
Uniformly, in the abstraction pool putting filter membrane in advance well, add appropriate kieselguhr to the Chi Kou reaching abstraction pool；Cover extraction
The lid in pond, extracts the mixture in abstraction pool, is extracted liquid, and extraction is divided into ester step and extraction step；
The condition going ester step is: extractant is ethyl acetate；Extraction temperature 70 DEG C；Static extracting time 5min；Punching
Wash volume 100%；Quiet cycle number of times 1 time；
The condition of extraction step is: extractant be mass ratio be methanol and the alcohol mixed solution of 82:18；Extraction temperature
100℃；Static extracting time 5min；Flush volume 60%；Quiet cycle number of times 3 times；
Step 2: by centrifugation after extract methanol dilution, obtain supernatant；
Step 3: use liquid chromatography to be analyzed supernatant；
Wherein, the analysis condition of liquid chromatography is:
A) instrument: high performance liquid chromatograph
B) chromatographic column specification: carbon 18 chromatographic column, 3*100mm 3um
C) column temperature: 30 DEG C
D) flow velocity: 0.5mL/min
E) flowing phase: methanol-0.1wt% acetic acid, volume ratio 80:20
F) detection wavelength: 332nm.
In above-mentioned Flos Buddlejae in the assay method of Pectolinarin, the volume of described abstraction pool is 10ml, described
The pressure removing the static extracting of ester step and extraction step is 1500psi, and the described purge time going ester step is 200s,
The purge time of extraction step is 60s.
In above-mentioned Flos Buddlejae in the assay method of Pectolinarin, step 2 is particularly as follows: by after extract methanol dilution
Under conditions of 15000r/min, centrifugal 3min, takes supernatant.
In above-mentioned Flos Buddlejae in the assay method of Pectolinarin, described instrument is Thermo U3000UHPLC
Chromatograph of liquid, described chromatographic column is Thermo Syncronis C18.
In above-mentioned Flos Buddlejae in the assay method of Pectolinarin, the instrument that described ASE extraction is used is
ASE350 Accelerate solvent extraction instrument.
The present invention is after using technique scheme, and it has the beneficial effect that
The detection method of the present invention is simple to operate, and extraction precision is high, and detection is accurately.
Detailed description of the invention
Below in conjunction with detailed description of the invention, technical scheme is described in further detail, but does not constitute this
Bright any restriction.
Embodiment 1:
Size-reduced for Flos Buddlejae machine is pulverized, excessively No. three sieves, about 0.5g, accurately weighed, mix homogeneously with 0.5g kieselguhr,
Stand-by, it is moved into and puts filter membrane in advance wellAdding proper amount of silicon diatomaceous earth in 10ml abstraction pool, shaking is allowed to gently
With Chi Kou in the same horizontal line, abstraction pool upper cover is tightened.After extraction terminates, extract is shifted in 50ml volumetric flask,
With methanol dilution to scale, under 15000r/min, centrifugal 5min, takes supernatant, enters LC and measures.
Extraction conditions (being shown in Table 1) is:
Table 1
Analysis method is LC liquid chromatography, liquid-phase chromatographic analysis condition:
A) the double ternary liquid phase (U-3000) of instrument: Thermo；
B) chromatographic column: Thermo Syncronis C18 3*100mm 3um, i.e. carbon 18 chromatographic column, diameter 3mm,
Length 100mm, particle diameter 3 microns；
C) column temperature: 30 DEG C；
D) flow velocity: 0.5mL/min；
E) flowing phase: methanol-0.1wt% acetum (20 DEG C of methanol and 0.1wt% acetum volume ratio are 80:20)；
F) detection wavelength: 332nm；
The degree of accuracy test of the extracting process of embodiment 1
The extraction and the assay method that use embodiment 1 carry out parallel testing twice to 4 batch Flos Buddlejaes, and lot number is respectively
1508090,151118,20150701,141201；
The content of Pectolinarin is as follows: 0.231%, and 0.232% (1508090), 0.215%, 0.215% (151118),
0.275%, 0.277% (20150701), 0.199%, 0.195% (141201).
The above-described presently preferred embodiments of the present invention that is only, all made in the range of the spirit and principles in the present invention any repair
Change, equivalent and improvement etc., should be included within the scope of the present invention.
Claims (5)
1. the assay method of Pectolinarin in a Flos Buddlejae, it is characterised in that comprise the following steps:
Step 1: by Flos Buddlejae grinding and sieving, weighs 0.5 weight portion Flos Buddlejae powder, mixes with 0.5 weight portion kieselguhr
Uniformly, in the abstraction pool putting filter membrane in advance well, add appropriate kieselguhr to the Chi Kou reaching abstraction pool；Cover extraction
The lid in pond, extracts the mixture in abstraction pool, is extracted liquid, and extraction is divided into ester step and extraction step；
The condition going ester step is: extractant is ethyl acetate；Extraction temperature 70 DEG C；Static extracting time 5min；Punching
Wash volume 100%；Quiet cycle number of times 1 time；
The condition of extraction step is: extractant be mass ratio be methanol and the alcohol mixed solution of 82:18；Extraction temperature
100℃；Static extracting time 5min；Flush volume 60%；Quiet cycle number of times 3 times；
Step 2: by centrifugation after extract methanol dilution, obtain supernatant；
Step 3: use liquid chromatography to be analyzed supernatant；
Wherein, the analysis condition of liquid chromatography is:
A) instrument: high performance liquid chromatograph
B) chromatographic column specification: carbon 18 chromatographic column, 3*100mm 3um
C) column temperature: 30 DEG C
D) flow velocity: 0.5mL/min
E) flowing phase: methanol-0.1wt% acetic acid, volume ratio 80:20
F) detection wavelength: 332nm.
The assay method of Pectolinarin in Flos Buddlejae the most according to claim 1, it is characterised in that described extraction
The volume taking pond is 10ml, and the pressure of the described static extracting removing ester step and extraction step is 1500psi, described
The purge time going ester step is 200s, and the purge time of extraction step is 60s.
The assay method of Pectolinarin in Flos Buddlejae the most according to claim 1, it is characterised in that step 2 has
Body is: by being centrifuged 3min after extract methanol dilution under conditions of 15000r/min, take supernatant.
The assay method of Pectolinarin in Flos Buddlejae the most according to claim 1, it is characterised in that described instrument
Device is Thermo U3000UHPLC chromatograph of liquid, and described chromatographic column is Thermo Syncronis C18.
The assay method of Pectolinarin in Flos Buddlejae the most according to claim 1, it is characterised in that described ASE
The instrument that extraction is used is ASE350 Accelerate solvent extraction instrument.
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| Application Number | Priority Date | Filing Date | Title |
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| CN201610268591.XA CN105954405A (en) | 2016-04-27 | 2016-04-27 | Method for determination of pectolinarin in buddleja officinalis |
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| CN201610268591.XA CN105954405A (en) | 2016-04-27 | 2016-04-27 | Method for determination of pectolinarin in buddleja officinalis |
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Cited By (2)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN107014927A (en) * | 2017-04-17 | 2017-08-04 | 广西壮族自治区梧州食品药品检验所 | A kind of method that ASE HPLC methods determine Determination of hesperidin in pericarpium citri reticulatae |
| CN107064351A (en) * | 2017-04-11 | 2017-08-18 | 广西壮族自治区梧州食品药品检验所 | A kind of method that ASE HPLC methods determine Determination of Hyperoside in hawthorn |
Citations (1)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN104876988A (en) * | 2015-05-12 | 2015-09-02 | 广西壮族自治区梧州食品药品检验所 | Method for extracting linarin from wild chrysanthemum flower |
-
2016
- 2016-04-27 CN CN201610268591.XA patent/CN105954405A/en active Pending
Patent Citations (1)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN104876988A (en) * | 2015-05-12 | 2015-09-02 | 广西壮族自治区梧州食品药品检验所 | Method for extracting linarin from wild chrysanthemum flower |
Non-Patent Citations (2)
| Title |
|---|
| 兰洲 等: "柳穿鱼黄酮类成分的提取工艺优化", 《中国现代中药》 * |
| 国家药典委员会: "《中华人民共和国药典 2010年版 一部》", 31 January 2010 * |
Cited By (2)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN107064351A (en) * | 2017-04-11 | 2017-08-18 | 广西壮族自治区梧州食品药品检验所 | A kind of method that ASE HPLC methods determine Determination of Hyperoside in hawthorn |
| CN107014927A (en) * | 2017-04-17 | 2017-08-04 | 广西壮族自治区梧州食品药品检验所 | A kind of method that ASE HPLC methods determine Determination of hesperidin in pericarpium citri reticulatae |
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Application publication date: 20160921 |