CN105929090A

CN105929090A - Method for extracting curculigoside in Curculigo orchioides

Info

Publication number: CN105929090A
Application number: CN201610255458.0A
Authority: CN
Inventors: 陈学松; 王丽丽; 韦涛; 梁美艳; 黄新惠
Original assignee: Wuzhou Institutes for Food and Drug Control
Current assignee: Wuzhou Institutes for Food and Drug Control
Priority date: 2016-04-22
Filing date: 2016-04-22
Publication date: 2016-09-07

Abstract

The invention discloses a method for extracting curculigoside in Curculigo orchioide. The method comprises the following steps: step 1, crushing Curculigo orchioides and then extracting the crushed Curculigo orchioides by using an ASE extraction method so as to obtain extract; step 2, subjecting the extract to dilution, centrifugation and filtering so as to obtain supernatant; and step 3, analyzing the supernatant by using liquid chromatography. The method for extracting curculigoside in Curculigo orchioides is simple to operate and high in detection precision.

Description

A kind of extracting process of Curculigoside in Crude Medicine Curculigo orchioides

Technical field

The present invention relates to test in laboratory field, the extracting process of a kind of Curculigoside in Crude Medicine Curculigo orchioides.

Background technology

Pharmacopeia in 2015 have recorded and takes this product powder (crossing No. three sieves) about 1g, accurately weighed, and the accurate methanol 50ml that adds is weighed heavy Amount, is heated to reflux 2 hours, takes out, lets cool, more weighed weight, supplies the weight of less loss with methanol, shakes up, and filters.Essence Close measuring subsequent filtrate 20ml, be evaporated, residue adds methanol and dissolves, and is transferred in 10ml measuring bottle, adds methanol to scale, shakes 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.

The method operating process of pharmacopeia 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 extracting process of a kind of Curculigoside in Crude Medicine Curculigo orchioides, the method is simple to operate, and accuracy of detection is high.

The technical scheme that the present invention provides is: the extracting process of a kind of Curculigoside in Crude Medicine Curculigo orchioides, comprises the following steps:

Step 1: after Rhizoma Curculiginis is pulverized, sieve；

Step 2: weigh 1 weight portion Rhizoma Curculiginis powder, mix homogeneously stand-by with 0.5 weight portion kieselguhr；

Step 3: the mixture in S12 is moved in the abstraction pool putting filter membrane in advance well, add appropriate kieselguhr to reaching The Chi Kou of abstraction pool；The lid covering abstraction pool carries out static extracting；Extraction is extracted liquid after terminating；

Extraction conditions is: extractant is methanol；Extraction temperature 90 DEG C；Static extracting time 5min；Flush volume 100%； Quiet cycle number of times 2 times；

Step 4: extract is diluted, centrifugal, filter after, obtain supernatant.

In the extracting process of above-mentioned Curculigoside in Crude Medicine Curculigo orchioides, the volume of described abstraction pool is 10ml, described static extracting Pressure is 1500psi, and the purge time of described static extracting is 100s.

In the extracting process of above-mentioned Curculigoside in Crude Medicine Curculigo orchioides, step 3 particularly as follows: by after extract methanol dilution at 1500r/min Under conditions of centrifugal and filter, retain filtrate.

In the extracting process of above-mentioned Curculigoside in Crude Medicine Curculigo orchioides, the instrument that described ASE extraction is used is that ASE350 is quick Solvent extraction instrument.

The present invention is after using technique scheme, and it has the beneficial effect that

The extracting process of the present invention is simple to operate, and the operating time is short, and precision is consistent with the precision of official method, reproducible.

Accompanying drawing explanation

Fig. 1 is the rectangular plots of the curculigoside linear relationship of the present invention；

Fig. 2 is the chromatogram of pharmacopeia record of the present invention, the chromatogram according to embodiment 1, the chromatogram of pharmacopeia record method.

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 the present invention 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, treat With, 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, dilute with methanol Releasing 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 chromatograph, diameter 3mm, Length 100mm, particle diameter 3 microns

C) column temperature: 40 DEG C

D) flow velocity: 0.5mL/min

E) flowing phase: the methanol of methanol-0.1% phosphoric acid that is 19 unit volume and the 0.1wt% phosphoric acid solution of 81 unit volumes mixed Compound；In the present embodiment, the volume ratio under conditions of volume ratio is 20 DEG C.

F) detection wavelength: 285nm

Chromatography validation verification:

Take curculigoside reference substance appropriate, accurately weighed, add methanol and make every 1ml solution containing 70 μ g, obtain curculigoside comparison Product solution.

Take Rhizoma Curculiginis reference substance solution (concentration: 0.0204mg/ml), respectively precision draw this solution 0.5 μ l, 1 μ l, 1.5 μ l, 2 μ l, 3 μ l enter LC and measure, and measure according to said method, the results detailed in Table 2.With absolute sample size (μ g)-average Peak area carries out linear regression, tries to achieve regression equation: y=1898.1x+2.2775, R²=0.9999.Curculigoside is 0.0102～0.0312 In good linear relationship in μ g range；Its rectangular coordinate relation is shown in Fig. 1；The label 3 in Fig. 2 is shown in by its liquid chromatograph collection of illustrative plates Collection of illustrative plates.

Table 2 curculigoside linear relationship

The repeatability checking of the extracting process of embodiment 1:

Take sample (lot number: the 20150701) 1g of identical lot number, totally 6 parts, accurately weighed, extract by ASE extracting method and supply Test sample solution, sample size is 2 μ l, with the chromatographic condition parallel test of embodiment 1, records the content of curculigoside in sample and is shown in Table 2, RSD is 1.6%, and test shows that ASE extracting method repeatability is good, the results detailed in Table 3.

Table 3

The degree of accuracy test of the extracting process of embodiment 1

Using the ASE extracting process of embodiment 1 and the extracting process of pharmacopeia to extract Rhizoma Curculiginis, Rhizoma Curculiginis is 4 batches, and lot number divides It is not 1508090,151118,20150701,141201；

The ASE extracting process of embodiment 1 uses the machine that same model specification is the most different to carry out parallel to a batch of Rhizoma Curculiginis Testing twice, respectively ASE1 and ASE2 represents.

In Fig. 2, the collection of illustrative plates of label 2 is the chromatogram that sample 1508090 obtains according to the method described in pharmacopeia；

In Fig. 2, the collection of illustrative plates of label 1 is the chromatogram that sample 1508090 obtains according to the method described in embodiment 1.

Concrete test result see table 4；

Table 4

Above-described be only presently preferred embodiments of the present invention, all made in the range of the spirit and principles in the present invention any amendment, Equivalent and improvement etc., should be included within the scope of the present invention.

Claims

1. the extracting process of a Curculigoside in Crude Medicine Curculigo orchioides, it is characterised in that comprise the following steps:

Step 1: after Rhizoma Curculiginis is pulverized, sieve；

Step 4: extract is diluted, centrifugal, filter after, obtain supernatant.

The extracting process of Curculigoside in Crude Medicine Curculigo orchioides the most according to claim 1, it is characterised in that the volume of described abstraction pool For 10ml, the pressure of described static extracting is 1500psi, and the purge time of described static extracting is 100s.

The extracting process of Curculigoside in Crude Medicine Curculigo orchioides the most according to claim 1, it is characterised in that step 3 will be particularly as follows: will extract It is centrifuged under conditions of 1500r/min after taking liquid methanol dilution and filters, retaining filtrate.

The extracting process of Curculigoside in Crude Medicine Curculigo orchioides the most according to claim 1, it is characterised in that described ASE extraction The instrument used is ASE350 Accelerate solvent extraction instrument.