CN105954407A - Method for determination of curculigine in curculigo orchioides - Google Patents
Method for determination of curculigine in curculigo orchioides Download PDFInfo
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- CN105954407A CN105954407A CN201610268820.8A CN201610268820A CN105954407A CN 105954407 A CN105954407 A CN 105954407A CN 201610268820 A CN201610268820 A CN 201610268820A CN 105954407 A CN105954407 A CN 105954407A
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- extraction
- rhizoma curculiginis
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- 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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- Health & Medical Sciences (AREA)
- Life Sciences & Earth Sciences (AREA)
- Chemical & Material Sciences (AREA)
- Analytical Chemistry (AREA)
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- General Physics & Mathematics (AREA)
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Abstract
The invention discloses a method for determination of curculigine in curculigo orchioides, wherein the method comprises the following steps: step 1, crushing the curculigo orchioides, then sieving, mixing 1 part by weight of the curculigo orchioides powder obtained from crushing and 0.5 part by weight of diatomite, adding the mixture to an extraction pool, carrying out static extraction, and extracting by using a rapid solvent extraction method to obtain an extract liquid, wherein extraction conditions comprise that an extraction solvent is a mixed solution of isopropanol and methanol with the weight ratio of 2:8, the extraction temperature is 100 DEG C and the static extraction time is 5 min, and the flushing volume is 100%; and carrying out static circulation for 1 time; step 2, carrying out dilution, centrifugation and filtration of the extract liquid, to obtain a supernatant; and step 3, analyzing the supernatant by liquid chromatography. The invention provides the method for determination of curculigine in the curculigo orchioides; the method has the advantages of simple operation and high detection accuracy.
Description
Technical field
The present invention relates to test in laboratory field, a kind of measure the method for Rhizoma Curculiginis element in Rhizoma Curculiginis.
Background technology
Pharmacopeia in 2015 have recorded extraction and the assay method of Curculigoside in Crude Medicine Curculigo orchioides: takes this product powder (crossing No. three sieves) about 1g,
Accurately weighed, accurate addition methanol 50ml, weighed weight, it is heated to reflux 2 hours, takes out, let cool, more weighed weight,
Supply the weight of less loss with methanol, shake up, filter.Precision measures subsequent filtrate 20ml, is evaporated, and residue adds methanol and dissolves,
It is transferred in 10ml measuring bottle, adds methanol to scale, shake up, filter, take subsequent filtrate, to obtain final product.
Liquid chromatographic detection condition is: with octadecylsilane chemically bonded silica as filler；With acetonitrile-0.1% phosphoric acid solution (21:
79) for flowing phase；Detection wavelength is 285nm.Number of theoretical plate is calculated by curculigoside peak should be not less than 3000.
Pharmacopeia only describes extraction and the assay method of curculigoside, does not have carrying of the open Rhizoma Curculiginis element of pertinent literature in prior art
Take and assay method.
Summary of the invention
It is an object of the invention to provide a kind of method measuring the element of Rhizoma Curculiginis in Rhizoma Curculiginis, the method is simple to operate, and accuracy of detection is high.
The technical scheme that the present invention provides is: a kind of method measuring the element of Rhizoma Curculiginis in Rhizoma Curculiginis, comprises the following steps:
Step 1: by Rhizoma Curculiginis grinding and sieving, the Rhizoma Curculiginis powder of 1 weight portion that smashing is obtained and the kieselguhr of 0.5 weight portion
Mixing, adds mixture to and carries out static extracting in abstraction pool, uses Accelerate solvent extraction method that extract is obtained by extraction；Extraction
The condition of taking is: extractant be weight ratio be isopropanol and the mixed solution of methanol of 2:8, extraction temperature 100 DEG C；Quiet
State extraction time 5min；Flush volume 100%；Quiet cycle number of times 1 time；
Step 2: extract is diluted, centrifugal, filter after, obtain supernatant；
Step 3: use liquid chromatography to be analyzed supernatant；
Wherein, the analysis condition of liquid chromatography is:
A) instrument: chromatograph of liquid
B) chromatographic column specification: carbon 18 liquid-phase chromatographic column 3mm*100mm3.0 μm
C) column temperature: 35 DEG C
D) flow velocity: 1mL/min
E) flowing phase: methanol and the mixture of 0.1wt% phosphoric acid solution, wherein methanol and the volume of 0.1wt% phosphoric acid solution
Ratio is 15:85
F) detection wavelength: 281nm.
Measure in Rhizoma Curculiginis in the method for Rhizoma Curculiginis element above-mentioned, step 2 particularly as follows: by after extract methanol dilution
It is centrifuged under conditions of 1500r/min and filters, retaining filtrate.
Measuring in Rhizoma Curculiginis in the method for Rhizoma Curculiginis element above-mentioned, the instrument used by liquid-phase chromatographic analysis is Thermo U-3000
Double ternary liquid phase chromatograph of liquid.
Measuring in Rhizoma Curculiginis in the method for Rhizoma Curculiginis element above-mentioned, 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 present invention uses isopropanol and methanol mixed solution as extractant, and extraction efficiency is high, at methanol and 0.1wt% phosphoric acid
In the case of the mixture of solution is as flowing mutually, in the case of detection wavelength 281 nanometer, the absworption peak area of Rhizoma Curculiginis element is maximum,
It is the most accurate to measure.
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 Rhizoma Curculiginis sample machine is pulverized, excessively No. three sieves, about 1g, accurately weighed, mix homogeneously with 0.5g kieselguhr,
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 and Chi Kou gently
In the same horizontal line, abstraction pool upper cover is tightened.After extraction terminates, extract is shifted in 50ml volumetric flask, uses first
Alcohol is diluted to scale, and 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 chromatograph, diameter 3mm,
Length 100mm, particle diameter 3 microns
C) column temperature: 35 DEG C
D) flow velocity: 1mL/min
E) flowing phase:: the methanol of 15 unit volumes and 85 unit volumes under the conditions of methanol-0.1% phosphoric acid that is 20 DEG C
The mixture of 0.1wt% phosphoric acid solution
F) detection wavelength: 281nm
The extraction of embodiment 1 and the degree of accuracy test of detection method
The ASE extracting process using embodiment 1 extracts and tests, and Rhizoma Curculiginis is 4 batches, and lot number is respectively 1508090,
151118,20150701,141201；Every batch sample parallel testing twice, Rhizoma Curculiginis cellulose content is 0.112%, 0.115%
(1508090)；0.125%, 0.127% (151118)；0.088%, 0.087% (20150701)；0.127%, 0.128%
(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 (4)
1. one kind measures the method for Rhizoma Curculiginis element in Rhizoma Curculiginis, it is characterised in that comprise the following steps:
Step 1: by Rhizoma Curculiginis grinding and sieving, the Rhizoma Curculiginis powder of 1 weight portion that smashing is obtained and the kieselguhr of 0.5 weight portion
Mixing, adds mixture to and carries out static extracting in abstraction pool, uses Accelerate solvent extraction method that extract is obtained by extraction；Extraction
The condition of taking is: extractant be weight ratio be isopropanol and the mixed solution of methanol of 2:8, extraction temperature 100 DEG C；Quiet
State extraction time 5min；Flush volume 100%；Quiet cycle number of times 1 time；
Step 2: extract is diluted, centrifugal, filter after, obtain supernatant；
Step 3: use liquid chromatography to be analyzed supernatant；
Wherein, the analysis condition of liquid chromatography is:
A) instrument: chromatograph of liquid
B) chromatographic column specification: carbon 18 liquid-phase chromatographic column 3mm*100mm3.0 μm
C) column temperature: 35 DEG C
D) flow velocity: 1mL/min
E) flowing phase: methanol and the mixture of 0.1wt% phosphoric acid solution, wherein methanol and the volume of 0.1wt% phosphoric acid solution
Ratio is 15:85
F) detection wavelength: 281nm.
The most according to claim 1 measure the method for Rhizoma Curculiginis element in Rhizoma Curculiginis, it is characterised in that step 2 particularly as follows:
By being centrifuged under conditions of 1500r/min after extract methanol dilution and filtering, retain filtrate.
The method of Rhizoma Curculiginis element in mensuration Rhizoma Curculiginis the most according to claim 1, it is characterised in that liquid-phase chromatographic analysis institute
Instrument be the double ternary liquid phase chromatograph of liquid of Thermo U-3000.
The method of Rhizoma Curculiginis element in mensuration Rhizoma Curculiginis the most according to claim 1, it is characterised in that described ASE extraction
The instrument that method is used is ASE350 Accelerate solvent extraction instrument.
Priority Applications (1)
| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| CN201610268820.8A CN105954407A (en) | 2016-04-27 | 2016-04-27 | Method for determination of curculigine in curculigo orchioides |
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| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| CN201610268820.8A CN105954407A (en) | 2016-04-27 | 2016-04-27 | Method for determination of curculigine in curculigo orchioides |
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| CN105954407A true CN105954407A (en) | 2016-09-21 |
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| CN201610268820.8A Pending CN105954407A (en) | 2016-04-27 | 2016-04-27 | Method for determination of curculigine in curculigo orchioides |
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Cited By (2)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN106918666A (en) * | 2017-04-11 | 2017-07-04 | 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 the curculigoside content in thizoma curculiginis |
| CN111420010A (en) * | 2020-04-21 | 2020-07-17 | 山东中医药大学 | Medicine-separating moxibustion medicine for tonifying internal organs and preparation method thereof |
-
2016
- 2016-04-27 CN CN201610268820.8A patent/CN105954407A/en active Pending
Cited By (2)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN106918666A (en) * | 2017-04-11 | 2017-07-04 | 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 the curculigoside content in thizoma curculiginis |
| CN111420010A (en) * | 2020-04-21 | 2020-07-17 | 山东中医药大学 | Medicine-separating moxibustion medicine for tonifying internal organs and preparation method thereof |
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