CN108362810A - A kind of Solid Phase Extraction measures the detection method and Solid Phase Extraction stick of traditional medicine volatile oil content - Google Patents
A kind of Solid Phase Extraction measures the detection method and Solid Phase Extraction stick of traditional medicine volatile oil content Download PDFInfo
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- CN108362810A CN108362810A CN201810127146.0A CN201810127146A CN108362810A CN 108362810 A CN108362810 A CN 108362810A CN 201810127146 A CN201810127146 A CN 201810127146A CN 108362810 A CN108362810 A CN 108362810A
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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
- G01N30/88—Integrated analysis systems specially adapted therefor, not covered by a single one of the groups G01N30/04 - G01N30/86
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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
- 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 present invention relates to detection methods and Solid Phase Extraction stick that the evaluation of Chinese medicine storage quality and control method more particularly to a kind of Solid Phase Extraction measure traditional medicine volatile oil content.It is an object of the present invention to provide a kind of Solid Phase Extraction stick of traditional medicine volatile oil, another object of the present invention is to provide a kind of detection method of Solid Phase Extraction measurement traditional medicine volatile oil content.The present invention realizes that Chinese medicine non-destructive testing and quality monitor in real time for extracting traditional medicine volatile oil, and its application in Chinese medicine storage quality is evaluated and is controlled.
Description
Technical field
The present invention relates to the evaluations of Chinese medicine storage quality and control method more particularly to a kind of Solid Phase Extraction to measure Chinese medicine volatilization
The detection method and Solid Phase Extraction stick of oil content.
Background technology
Volatile oil is a big constituents of Chinese herbal medicine, is commonly used to the quality good or not of evaluation Chinese medicine and fragrance.Volatile oil content
Generally 1% hereinafter, mainly containing terpenoid, aromatic compound, aliphatic compound etc..These ingredients are mostly small point
Sub- substance can quickly be absorbed by body, have effects that resuscitation with aromatics more, in cardio-cerebrovascular, central nervous system, exhales
Desorption system, gastrointestinal system, antibacterial, anti-inflammatory, antitumor, antiviral and promotion drug absorption etc. are many-sided all to have effect.Cause
This, volatile ingredient has very important effect to the drug action of many Chinese medicines.Quality comparison is always during Chinese medicine is stored
Research hotspot, wherein the variation of volatile ingredient is the important feature of Chinese medicine storage quality.
The extraction and separation process of volatile oil is most important to ingredient qualitative and quantitative analysis.The extraction separation side of volatile oil at present
Method includes mainly steam distillation, organic solvent extraction, super critical extraction and Head space.(1) as defined in Chinese Pharmacopoeia
Many volatile oil extractings are all steam distillations.Although the method uses extensively, the problem of can not be ignored there is also some, example
Such as sampling amount is big, complicated for operation, volatile oil is easy loss；(2) organic solvent extraction utilizes low boiling point organic solvent such as stone
Oily ether, ether, with Chinese medicine in continuous extractor heating extraction, it is high compared with the extraction efficiency of steam distillation.But the method institute
Volatile oil viscosity it is very big, liposoluble constituent such as resin, grease, wax etc. is also extracted simultaneously in raw material, and impurity is more；(3) surpass
Critical extraction method is compared with traditional steam distillation, the advantages that meeting low extraction temperature, system sealing.But the method is only applicable to
The small substance of relative molecular mass is extracted, and is invested greatly, certain difficulty and limitation are brought to industrial applications.(4) in recent years
There is scholar to combine gas chromatographic detection volatile oil component using Head space.This method be on the basis of steam distillation, it is attached
Add solid phase extraction concentration to extract volatile oil.Volatile oil component similar with steam distillation, which easily makes part unstable
Heat damage.In addition, above method all can not achieve non-destructive testing, it is not suitable for treasuring the survey of medicinal material fragrance or a small amount of sample
It is fixed, it is also not suitable for the real time monitoring of Chinese medicine storage quality variation.Therefore, the new technology of traditional extraction process drawback can be overcome by finding
A new hot spot of volatile oil extracting research is had become with device.
Applicant has applied for Chinese invention patent (publication number：CN104549593A) one kind having ultrafiltration and Solid Phase Extraction is double
The functionalization liquid transfer gun head of weight catharsis, and its for the preceding processing of biological sample and quantitative point during Pharmaceutical Analysis
Analysis.The pipette tips include liquid transfer gun head, Solid Phase Extraction material and hollow-fibre membrane, and the tip setting of the liquid transfer gun head is described
Hollow-fibre membrane, and it is uniformly applied to liquid transfer gun head tip and hollow-fibre membrane junction by the way that glue is arranged, described is hollow
There is tunica fibrosa upper/lower terminal mouth, upper port sealing, lower port to keep open state, the Solid Phase Extraction material
It is arranged inside the liquid transfer gun head.The device is provided with liquid transfer gun head, Solid Phase Extraction material and hollow-fibre membrane, hollow fibre
Dimension film is arranged in the inside of Solid Phase Extraction material, for liquid phase purifying extraction, but and suitable for the absorption of gas phase volatile oil.
The present invention is built in using adsorbent in hollow-fibre membrane, can be realized that sample nondestructive detects, is not necessarily to heating extraction,
It is mainly used for the situation of change of volatile oil in Study of Traditional Chinese Medicine storage process.Other are used for the experimental provision of volatile oil extracting in device
There are notable differences with the present invention on construction, operation principle, cannot be satisfied the need of sample nondestructive detection and quality real time monitoring
It wants.Through retrieval, the patent disclosure similar with the present invention is had no, and the volatile oil carried out with the similar experimental provision of the present invention
The document report of research.
Invention content
It is an object of the present invention to provide a kind of Solid Phase Extraction stick of traditional medicine volatile oil, another object of the present invention
It is to provide a kind of detection method of Solid Phase Extraction measurement traditional medicine volatile oil content.The present invention is used to extract traditional medicine volatile oil, and its
It evaluates in Chinese medicine storage quality and is monitored in real time with the application in control, realization Chinese medicine non-destructive testing and quality.
In order to realize above-mentioned first purpose, present invention employs technical solutions below：
A kind of Solid Phase Extraction stick of traditional medicine volatile oil, the Solid Phase Extraction stick are made of structure below:
1) it is used to load the hollow-fibre membrane of adsorbent
The length 1-2cm of the hollow-fibre membrane, 500-800 μm of internal diameter, 800-1200 μm of outer diameter, membranous wall aperture 0.1-
0.5 μm, shape is cylinder, and material is polypropylene；With upper/lower terminal mouth, upper and lower part is sealed using the tweezers pressing of heating
Two ports；
2) it is used to adsorb the Solid Phase Extraction material of volatile oil
It is with adsorption capacity that Solid Phase Extraction material, which uses pulverulent solids, 2-50 μm of particle diameter, Solid Phase Extraction material,
Solid powder, be filled in hollow-fibre membrane, mass range 0.005g-20g.
Preferably, the Solid Phase Extraction material is one kind in reversed material, positive phase material and ion exchange material
Or a variety of mixing.
Preferably, the Solid Phase Extraction quality of materials ranging from 0.01g-5g.Further preferably, the Solid Phase Extraction material
Material mass range is 0.1g-2g.
In order to realize above-mentioned second purpose, present invention employs technical solutions below：
A kind of Solid Phase Extraction measures the detection method of traditional medicine volatile oil content, and this approach includes the following steps：
1) in traditional Chinese medicine sample volatile oil absorption
The Solid Phase Extraction stick is put into sample, sample encapsulates sample and Solid Phase Extraction stick without crushing together；
The adsorption time minimum time is 1 hour；Sample minimum mass is 10g；
2) it elutes
Solid Phase Extraction stick is taken out from sample, is put into eluting solvent and elutes volatile materials；Elution time is ranging from
5min-60min；
3) chromatography of volatile oil
The eluent of step 2) is taken to carry out target substance assay.
Preferably, the encapsulating material is salable bag, salable box or warehouse.
Preferably, the eluting solvent can be n-hexane, water, ethyl acetate, ether or acetone.
Preferably, the traditional Chinese medicine sample is Rhizoma Atractylodis Macrocephalae, eluting solvent is n-hexane, elution time 10min；Chromatography point
Analysis use Shimadzu gas chromatograph-mass spectrometer GCMS-QP2010SE, DB-5 chromatographic column, column begin temperature 60 DEG C, keep 4min, with 5 DEG C/
Min, temperature programming keep 5min, then be warming up to 250 DEG C with 10 DEG C/min, keep 5min to 180 DEG C；Carrier gas is high pure nitrogen,
Hydrogen flowing quantity 1mL/min；EI ion sources；Electron energy 70eV；Scanning range m/z 50~500, acquisition mode are full scan mould
Formula.
The present invention has the characteristics that following as a result of above-mentioned Solid Phase Extraction stick and method：
1, manufacturing process is easy to be controllable
Head space extraction volatile oil based on Solid Phase Extraction principle needs to arrange by vapor and Solid Phase Extraction two walks
Suddenly, and extraction process needs to realize by extra means such as ml headspace bottles, and operation is more, process is complicated.The Solid Phase Extraction of the present invention
Stick is simple in structure, can strictly control each factor in manufacturing process, fiber material dosage can be precisely controlled, and may be implemented
Sample nondestructive detects, and amount of samples is small, can provide reliable sample pre-treatments for the storage process quality monitoring of precious Chinese medicine
Device.
2, method applied science is reasonable
Current essential oil extraction method be required for heating assisted extraction, but heat easily keep part unstable volatile oil at
Divide heat damage.Apparatus of the present invention need to be only positioned in sample, without heating, can be used for waving for most room temperature preservation samples
Volatile material detects, and is embodied in the variation of sample volatile materials in true storage condition, methodological science is reasonable, easy to use.
3, extraction conditions is adjusted flexibly
The capacity of head space solid phase extraction is limited at present, and material utilization amount and type are difficult to adjust.The experimental provision of the present invention,
Different target substance and sample can be directed to, facilitate a variety of fiber materials of selection, by adjusting different material types, dosage and
Elution requirement provides diversified experimental data, meets the analysis requirement of different samples.
4, convenient material drawing has good prospects
Making material of the present invention such as Solid Phase Extraction material is that consumptive material, hollow fibre are commonly tested in all kinds of laboratories
Dimension membrane material is widely used, and can very easily be obtained.Production method through the invention, it may be convenient to produce with solid
The volatile oil extractor of phase extraction ability, and can repeatedly use, it can be to reduce time for sample pretreatment, reduce
Experimental expenses plays positive effect.
Description of the drawings
The structural schematic diagram of Fig. 1 volatile oil Solid Phase Extraction sticks.1- hollow-fibre membranes, 2- Solid Phase Extraction materials, 3- sealings.
The photo of Fig. 2 volatile oil Solid Phase Extraction sticks.1- contains the device of adsorbent；2- hollow-fibre membranes.
Fig. 3 gives birth to the chromatography figure of atractylodes slice sample.1- steam distillation extraction results；2- hollow fiber membrane extractions
As a result；3- adsorbent extraction results；4- volatile oil Solid Phase Extraction stick extraction results.
Specific implementation mode
1) preparation of Solid Phase Extraction stick
Take 1 segment length 5cm, 600 μm of internal diameter, 1000 μm of outer diameter, 0.2 μm of membranous wall aperture, the doughnut of polypropylene material
Film；Hollow-fibre membrane lower port is pressed with the tweezers of heating, is sealed against, upper port keeps open state；Weigh 0.1g
Black carbon nanotube solid absorbent materials, are put into inside hollow-fibre membrane；Hollow-fibre membrane upper end is pressed with the tweezers of heating
Mouthful, it is sealed against.
2) in traditional Chinese medicine sample volatile oil absorption
5 volatile oil Solid Phase Extraction sticks of the invention are put into 500g atractylodes slices (health product or bran fry product).Medicine materical crude slice
Sample is without crushing.Sample and volatile oil Solid Phase Extraction stick are encapsulated in together in sealing polybag, extraction time is 1 hour.
Sample storage time is 1 month, 6 months, 12 months.
3) it elutes
5 volatile oil Solid Phase Extraction sticks of the invention are taken out from sample.It is put into 2mL n-hexanes and stands elution, wash
The de- time is 10min.
3) chromatography of volatile oil
By eluent direct injected, carry out chromatography.Using Shimadzu gas chromatograph-mass spectrometer (GCMS-QP2010SE),
DB-5 chromatographic columns, column begin temperature 60 DEG C, keep 4min, with 5 DEG C/min, temperature programming to 180 DEG C, keep 5min, then with 10 DEG C/
Min is warming up to 250 DEG C, keeps 5min.Carrier gas is high pure nitrogen, hydrogen flowing quantity 1mL/min.EI ion sources；Electron energy 70eV；
Scanning range m/z 50~500, acquisition mode are full scan pattern.Standard spectrum library NIST11.L is retrieved, peak area normalization meter
Calculate each component percentage contents.
The volatile materials after different time is placed to atractylodes slice respectively with gas chromatography-mass spectrum to be quantified and determined
Property analyze and be compared, table 1 be Rhizoma Atractylodis Macrocephalae volatile ingredient table.As a result as shown in table 2 and table 3.Raw atractylodes slice and bran are fried white
The changing rule of art medicine materical crude slice volatile ingredient is similar.With the extension of storage time, in volatile oil, most of ingredients are opposite contains
Amount reduces, but carypohyllene, γ-elemene, 10- tables gurjunene, 3,7 (11)-celery diene this four alkenes component ratios increase.
1 Rhizoma Atractylodis Macrocephalae volatile ingredient table of table.
The variation of raw atractylodes slice volatile component content in 2 storage of table
The variation of stir-baked RHIZOMA ATRACTYLDIS MACROCEPHALAE in bran medicine materical crude slice volatile component content during table 3 stores
Claims (7)
1. a kind of Solid Phase Extraction stick of traditional medicine volatile oil, which is characterized in that the Solid Phase Extraction stick is made of structure below:
1) it is used to load the hollow-fibre membrane of adsorbent
The length 1-2cm of the hollow-fibre membrane, 500-800 μm of internal diameter, 800-1200 μm of outer diameter, membranous wall aperture 0.1-0.5 μ
M, shape are cylinder, and material is polypropylene；With upper/lower terminal mouth, upper and lower part two is sealed using the tweezers pressing of heating
Port；
2) it is used to adsorb the Solid Phase Extraction material of volatile oil
It is consolidating with adsorption capacity that Solid Phase Extraction material, which uses pulverulent solids, 2-50 μm of particle diameter, Solid Phase Extraction material,
Body powder, is filled in hollow-fibre membrane, mass range 0.005g-20g.
2. according to claim 1 a kind of for traditional medicine volatile oil Solid Phase Extraction stick, which is characterized in that Solid Phase Extraction material
For one or more mixing in reversed material, positive phase material and ion exchange material.
3. according to claim 1 a kind of for traditional medicine volatile oil Solid Phase Extraction stick, which is characterized in that Solid Phase Extraction material
Mass range is 0.01g-5g.
4. a kind of Solid Phase Extraction measures the detection method of traditional medicine volatile oil content, which is characterized in that this approach includes the following steps：
1) in traditional Chinese medicine sample volatile oil absorption
Solid Phase Extraction stick as claimed in claim 1 or 2 is put into sample, sample is without crushing, by sample and Solid Phase Extraction stick
It encapsulates together；The adsorption time minimum time is 1 hour；Sample minimum mass is 10g；
2) it elutes
Solid Phase Extraction stick is taken out from sample, is put into eluting solvent and elutes volatile materials；Elution time ranging from 5min-
60min；
3) chromatography of volatile oil
The eluent of step 2) is taken to carry out target substance assay.
5. a kind of Solid Phase Extraction according to claim 3 measures the detection method of traditional medicine volatile oil content, which is characterized in that
Encapsulating material is salable bag, salable box or warehouse.
6. a kind of Solid Phase Extraction according to claim 3 measures the detection method of traditional medicine volatile oil content, which is characterized in that
Eluting solvent can be n-hexane, water, ethyl acetate, ether or acetone.
7. a kind of Solid Phase Extraction according to claim 3 measures the detection method of traditional medicine volatile oil content, which is characterized in that
The traditional Chinese medicine sample is Rhizoma Atractylodis Macrocephalae, and eluting solvent is n-hexane, elution time 10min；Chromatography uses Shimadzu gas phase color
Spectrum-mass spectrograph GCMS-QP2010SE, DB-5 chromatographic column, 60 DEG C of column beginning temperature, keeps 4min, with 5 DEG C/min, temperature programming to 180
DEG C, 5min is kept, then 250 DEG C are warming up to 10 DEG C/min, keeps 5min；Carrier gas is high pure nitrogen, hydrogen flowing quantity 1mL/min；
EI ion sources；Electron energy 70eV；Scanning range m/z 50~500, acquisition mode are full scan pattern.
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Citations (5)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| WO1995017247A1 (en) * | 1993-12-22 | 1995-06-29 | Minnesota Mining And Manufacturing Company | Sheet materials for solid phase extractions and solid phase reactions |
| CN1618503A (en) * | 2003-11-18 | 2005-05-25 | 中国科学院大连化学物理研究所 | Adsorption rod/agitating adsorption rod, and method for preparing its coating |
| CN104257818A (en) * | 2014-09-17 | 2015-01-07 | 中国中医科学院中医基础理论研究所 | Composition containing immature bitter orange extract and bighead atractylodes rhizome extract and application of composition |
| US8933007B1 (en) * | 2013-08-21 | 2015-01-13 | Arthur William Perry | Synthetic solid cleanser |
| CN105738505A (en) * | 2016-02-03 | 2016-07-06 | 长沙理工大学 | Detection method for volatile spice ingredients in coriander |
-
2018
- 2018-02-08 CN CN201810127146.0A patent/CN108362810A/en active Pending
Patent Citations (5)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| WO1995017247A1 (en) * | 1993-12-22 | 1995-06-29 | Minnesota Mining And Manufacturing Company | Sheet materials for solid phase extractions and solid phase reactions |
| CN1618503A (en) * | 2003-11-18 | 2005-05-25 | 中国科学院大连化学物理研究所 | Adsorption rod/agitating adsorption rod, and method for preparing its coating |
| US8933007B1 (en) * | 2013-08-21 | 2015-01-13 | Arthur William Perry | Synthetic solid cleanser |
| CN104257818A (en) * | 2014-09-17 | 2015-01-07 | 中国中医科学院中医基础理论研究所 | Composition containing immature bitter orange extract and bighead atractylodes rhizome extract and application of composition |
| CN105738505A (en) * | 2016-02-03 | 2016-07-06 | 长沙理工大学 | Detection method for volatile spice ingredients in coriander |
Non-Patent Citations (3)
| Title |
|---|
| NABIL AL-HADITHI 等: "A solid bar microextraction method for the liquid chromatographic determination of trace diclofenac,ibuprofen and carbamazepine in river water", 《MICROCHIM ACTA》 * |
| 朱荩雯 等: "白术饮片与其免煎饮片有效成分对比分析", 《亚太传统医药》 * |
| 梁光义主编: "《中药化学》", 31 August 2005, 北京：中医古籍出版社 * |
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Application publication date: 20180803 |