CN106896180A - A kind of detection method of Bushen Tianjing oral liquid - Google Patents
A kind of detection method of Bushen Tianjing oral liquid Download PDFInfo
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- CN106896180A CN106896180A CN201510965707.0A CN201510965707A CN106896180A CN 106896180 A CN106896180 A CN 106896180A CN 201510965707 A CN201510965707 A CN 201510965707A CN 106896180 A CN106896180 A CN 106896180A
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- radix angelicae
- angelicae sinensis
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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
- G01N30/90—Plate chromatography, e.g. thin layer or paper chromatography
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Abstract
The invention provides a kind of detection method of Bushen Tianjing oral liquid, the thin-layered chromatography of wherein Radix Angelicae Sinensis is：Need testing solution, control medicinal material solution, negative sample solution equal volume amounts are drawn, 5~20 μ l are respectively taken, put respectively on lamellae, be that solvent launches with cyclohexane-ethyl acetate mixed solution, taken out, dried, put and inspect under 365nm ultraviolet lamps.In test sample chromatogram, on position corresponding with control medicinal material chromatogram, show the fluorescence spot of same color, negative sample is noiseless.This method is easy to operate, and separating effect is quick, accurate, and reappearance is good, and specificity is strong.
Description
Technical field
The invention belongs to analysising drug form of Chinese materia medica technical field, and in particular to a kind of TLC Identification of Bushen Tianjing oral liquid.
Background technology
Bushen Tianjing oral liquid by ginseng, pilose antler (shortcake), pizzle (shortcake), dog whip (shortcake), the Radix Astragali, Radix Angelicae Sinensis, saline cistanche,
The 15 taste medicinal materials such as actinolite, the fruit of Chinese wolfberry, the bark of eucommia, black suitable piece, Semen Cuscutae, prepared rhizome of rehmannia, barrenwort, semen allii tuberosi are made, and have
Effect of warming kidney and enhancing body, for kidney yang virtual loss, waist knee impotence or crymodynia, hands and feet being not warm, impotence, cold sperm is One's spirits are drooping
Or weak etc..Radix Angelicae Sinensis is one of its important flavour of a drug, from the dry of umbelliferae angelica Angelica sinensis (Oliv.) Diels
Dry, there is replenishing and activating blood, menstruction regulating and pain relieving, relax bowel.Modern pharmacological research shows that its main matter basis is
Volatile ingredient and organic acid substance.
Different Chinese medicine compound prescriptions in production process, each taste medicine chemical change through compatibility and produced by different preparation process can not be pre-
Intellectual directly results in the complexity and unstability of its material base, sets up quick, simple discrimination method, to Chinese medicine compound prescription and
Its preparation important in inhibiting.At present, had no in the national drug standards of Bushen Tianjing oral liquid carries out quality control to Radix Angelicae Sinensis medicinal material
System.But provincial standard (the standard number before liter GB：WS-10824 (ZD-0824) -2002) middle regulation, the mirror of Radix Angelicae Sinensis
Not Cai Yong thin-layered chromatography, specific method is as follows：Take this product 50ml, plus the shaking of ethyl acetate-formic acid (95: 5) mixed solution
Extract 2 times, each 40ml, merge extract solution, be evaporated, residue adds the absolute ethyl alcohol 2ml to make dissolving, used as need testing solution.
Forulic acid reference substance is separately taken, plus absolute ethyl alcohol is made solution of every 1ml containing 0.5mg, as reference substance solution.According to thin-layer chromatography
Method is tested, and draws each 5 μ l of above two solution, is put respectively on same silica gel g thin-layer plate, with benzene-chloroform-glacial acetic acid (6: 5: 1)
It is solvent, launches, take out, dry, puts and inspect under ultraviolet lamp (365nm).In test sample chromatogram, with reference substance
On the corresponding position of chromatogram, show the fluorescence spot of same color.
Above-mentioned TLC Identification is oral to judge kidney tonifying, essence replenishing by differentiating the active ingredient forulic acid of Radix Angelicae Sinensis medicinal material in prescription
, there is problems with the true and false of liquid：(1) preparation of need testing solution need to use two kinds of Extraction solvents, three kinds of developing solvents, inspection
Test relatively costly.(2) in this prescription in addition to Radix Angelicae Sinensis, the fruit of Chinese wolfberry also contains more forulic acid, causes negative serious interference.(3)
Contain benzene in solvent, very big infringement is caused to experimenter and environment.
The content of the invention
It is an object of the invention to provide a kind of discrimination method of Radix Angelicae Sinensis medicinal material in improved Bushen Tianjing oral liquid, supplied in this method
Test sample solution prepares simple, reduction inspection cost, excludes negative interference, more friendly to experimenter and environment.Skill of the present invention
Art scheme is as follows：
The discrimination method of Radix Angelicae Sinensis medicinal material comprises the following steps in Bushen Tianjing oral liquid：
(1) preparation of need testing solution：Take Bushen Tianjing oral liquid 30-40ml, plus equivalent petroleum ether (30~60 DEG C),
Shaking is extracted 2 times, merges petroleum ether liquid, is volatilized, and residue adds the ethanol 1-2ml to make dissolving, used as need testing solution；
(2) preparation of control medicinal material solution：Take Radix Angelicae Sinensis control medicinal material 0.5-1g, plus step (1) moderate petroleum ether
(30~60 DEG C), ultrasonic extraction 30-60 minutes, filtration, filtrate is concentrated into 1-2ml, used as control medicinal material solution；
(3) preparation of negative sample solution：Other medicinal materials in addition to Radix Angelicae Sinensis are weighed by Bushen Tianjing oral liquid prescription, is made to lack and is worked as
The negative sample returned, the negative sample solution of scarce Radix Angelicae Sinensis is made by need testing solution preparation method；
(4) launch and inspect：Aspiration step (1), (2), the need testing solution obtained by (3), control medicinal material solution,
Negative sample solution equal volume amounts, it is each to draw 5-20 μ l, put respectively on same lamellae, with volume ratio as 1-3:1 hexamethylene
Alkane-ethyl acetate mixture is solvent, is launched, and is taken out, and is dried, and puts and inspect under 365nm ultraviolet lamps.
The discrimination method of Radix Angelicae Sinensis composition of the present invention preferably comprises following steps：
(1) preparation of need testing solution：Bushen Tianjing oral liquid 30ml, plus 30ml petroleum ethers (30~60 DEG C) are taken, is shaken
Extract 2 times, merge petroleum ether liquid, volatilize, residue adds the ethanol 1ml to make dissolving, used as need testing solution；
(2) preparation of control medicinal material solution：Radix Angelicae Sinensis control medicinal material 0.5g, plus petroleum ether (30~60 DEG C) 30ml are taken, ultrasound is carried
Take 30 minutes, filter, filtrate is concentrated into 1ml, used as control medicinal material solution；
(3) preparation of negative sample solution：Other medicinal materials in addition to Radix Angelicae Sinensis are weighed by Bushen Tianjing oral liquid prescription, is made to lack and is worked as
The negative sample returned, the negative sample solution of scarce Radix Angelicae Sinensis is made by step (1) need testing solution preparation method；
(4) launch and inspect：Aspiration step (1), (2), the need testing solution obtained by (3), control medicinal material solution,
Each 10 μ l of negative sample solution, put on same lamellae, with volume ratio as 1-3 respectively:1 cyclohexane-ethyl acetate mixing is molten
Liquid is solvent, is launched, and is taken out, and is dried, and puts and inspect under 365nm ultraviolet lamps.
Lamellae of the present invention is preferably silica gel g thin-layer plate or silica G F254Lamellae.
The volume ratio of solvent cyclohexane-ethyl acetate mixed solution cyclohexane-ethyl acetate of the present invention is preferably 2-3:1,
More preferably 2:1.
The beneficial effects of the present invention are：The present invention establishes a kind of discriminating side of Radix Angelicae Sinensis medicinal material in improved Bushen Tianjing oral liquid
Bushen Tianjing oral liquid provincial standard (standard number before method, with liter GB：WS-10824 (ZD-0824) -2002) provide
The discrimination method of Radix Angelicae Sinensis medicinal material compare, with following advantage：(1) a kind of solvent is only used in the preparation of need testing solution, is launched
Solvent is reduced to two kinds by three kinds, reduces the consumption of test sample and reagent, reduces inspection cost.(2) forulic acid is compareed
Product are changed to Radix Angelicae Sinensis control medicinal material, using expansion system of the invention and inspect means, can exclude the interference of feminine gender, greatly enhance
The specificity that Radix Angelicae Sinensis medicinal material differentiates in prescription.(3) experiment overall process uses the relatively low solvent of toxicity, it is ensured that experimenter's
Safety, protects environment.(4) this method has good repeatability and stability, it is adaptable to Radix Angelicae Sinensis in Bushen Tianjing oral liquid
The indentification by TLC of medicinal material.
In addition, this prescription preparation process is complicated, after ginseng pilose antler alcohol extracting, the dregs of a decoction and other taste medicinal materials are multiple after alcohol precipitation through water extraction
Complex chemical composition in side, Radix Angelicae Sinensis volatile ingredient such as Ligustilide without reserve, organic acid substance such as forulic acid etc., also for
The material base of another main flavour of a drug fruit of Chinese wolfberry of this prescription, along with other medicines composition, causes negative serious interference；Therefore originally
Invention is favorably improved using suitable Extraction solvent, solvent etc. with preferable repeatability and the discrimination method of stability
The quality control level of Bushen Tianjing oral liquid.
Brief description of the drawings
Fig. 1 is the Radix Angelicae Sinensis thin layer discriminating figure of embodiment 1, wherein 1- negative samples；The need testing solution sample of 2- embodiments 1；3- Radix Angelicae Sinensis
Control medicinal material sample.
Fig. 2 is the Radix Angelicae Sinensis thin layer discriminating figure of comparative example 1, wherein 1- negative samples；The need testing solution sample of 2- comparative examples 1；3- Radix Angelicae Sinensis
Control medicinal material sample.
Fig. 3 is the Radix Angelicae Sinensis thin layer discriminating figure of comparative example 2, wherein 1- negative samples；The need testing solution sample of 2- comparative examples 2；3- Radix Angelicae Sinensis
Control medicinal material sample.
Fig. 4 is the Radix Angelicae Sinensis thin layer discriminating figure of comparative example 3, wherein 1- negative samples；2- Radix Angelicae Sinensis control medicinal material samples；3- comparative examples 3 are supplied
Test sample solution sample.
Fig. 5 is the Radix Angelicae Sinensis thin layer discriminating figure of embodiment 2, wherein 1- negative samples, the need testing solution of 2- embodiments 2 1., 3- embodiments 2
Need testing solution 2., 4- control medicinal material samples.
Specific embodiment
Embodiment 1
The discriminating of Radix Angelicae Sinensis composition comprises the following steps in a kind of Bushen Tianjing oral liquid：
(1) preparation of need testing solution：Bushen Tianjing oral liquid 35ml, plus 35ml petroleum ethers (30~60 DEG C) are taken, is shaken
Extract 2 times, merge petroleum ether liquid, volatilize, residue adds the ethanol 2ml to make dissolving, used as need testing solution；
(2) preparation of control medicinal material solution：Radix Angelicae Sinensis control medicinal material 0.6g, plus petroleum ether (30~60 DEG C) 35ml are taken, ultrasound is carried
Take 35 minutes, filter, filtrate is concentrated into 2ml, used as control medicinal material solution；
(3) preparation of negative sample solution：Other medicinal materials in addition to Radix Angelicae Sinensis are weighed by Bushen Tianjing oral liquid prescription, is made to lack and is worked as
The negative sample returned, the negative sample solution of scarce Radix Angelicae Sinensis is made by step (1) need testing solution preparation method；
(4) launch and inspect：Aspiration step (1), (2), the need testing solution obtained by (3), control medicinal material solution,
Each 5 μ l of negative sample solution, put on same lamellae respectively, are 3 with volume ratio:1 cyclohexane-ethyl acetate mixed solution
It is solvent, launches, take out, dry, puts and inspect under 365nm ultraviolet lamps.
Identification result is：In test sample chromatogram, on position corresponding with control medicinal material chromatogram, show the fluorescence spot of same color.
Negative sample is noiseless.
Embodiment 2
The discriminating of Radix Angelicae Sinensis composition comprises the following steps in a kind of Bushen Tianjing oral liquid：
(1) preparation of need testing solution：Bushen Tianjing oral liquid 30ml, plus 30ml petroleum ethers (30~60 DEG C) are taken, is shaken
Extract 2 times, merge petroleum ether liquid, volatilize, residue adds the ethanol 1ml to make dissolving, used as need testing solution；
(2) preparation of control medicinal material solution：Radix Angelicae Sinensis control medicinal material 0.5g, plus petroleum ether (30~60 DEG C) 30ml are taken, ultrasound is carried
Take 30 minutes, filter, filtrate is concentrated into 1ml, used as control medicinal material solution；
(3) preparation of negative sample solution：Other medicinal materials in addition to Radix Angelicae Sinensis are weighed by Bushen Tianjing oral liquid prescription, is made to lack and is worked as
The negative sample returned, the negative sample solution of scarce Radix Angelicae Sinensis is made by step (1) need testing solution preparation method；
(4) launch and inspect：Aspiration step (1), (2), the need testing solution obtained by (3), control medicinal material solution,
Each 10 μ l of negative sample solution, put on same lamellae respectively, are 2 with volume ratio:1 cyclohexane-ethyl acetate mixed solution
It is solvent, launches, take out, dry, puts and inspect under 365nm ultraviolet lamps.
Identification result is：In 3 test sample chromatograms, on position corresponding with control medicinal material chromatogram, show the fluorescence of same color
Spot, and clear spot, without conditions of streaking, negative sample is noiseless.
The solvent of comparative example 1 is volume ratio 10:1 chloroform-methyl alcohol mixed solution, remaining is with embodiment 1.Identification result is：
Target blob can be preferably separated, but spot and R f value is higher.
The solvent of comparative example 2 is volume ratio 3:2:1 ethyl acetate-chloroform-formic acid mixed solution, remaining is with embodiment 1.
Identification result is：Target blob can be preferably separated, but spot is not mellow and full and Rf values are higher.
The solvent of comparative example 3 is that volume ratio is 9:1 cyclohexane-ethyl acetate mixed solution, remaining is with embodiment 1.Differentiate knot
It is really：In test sample chromatogram, on position corresponding with control medicinal material chromatogram, the fluorescence spot without same color, it is impossible to differentiate
Radix Angelicae Sinensis medicinal material in Bushen Tianjing oral liquid.
Claims (5)
1. a kind of detection method of Bushen Tianjing oral liquid, it is characterised in that the discriminating of Radix Angelicae Sinensis composition comprises the following steps：
(1) preparation of need testing solution：Take Bushen Tianjing oral liquid 30-40ml, plus equivalent petroleum ether (30~60 DEG C), shaking
Extract 2 times, merge petroleum ether liquid, volatilize, residue adds the ethanol 1-2ml to make dissolving, used as need testing solution；
(2) preparation of control medicinal material solution：Take Radix Angelicae Sinensis control medicinal material 0.5-1g, plus step (1) moderate petroleum ether (30~60 DEG C),
Ultrasonic extraction 30-60 minutes, filtration, filtrate is concentrated into 1-2ml, used as control medicinal material solution；
(3) preparation of negative sample solution：Other medicinal materials in addition to Radix Angelicae Sinensis are weighed by Bushen Tianjing oral liquid prescription, scarce Radix Angelicae Sinensis is made
Negative sample, the negative sample solution of scarce Radix Angelicae Sinensis is made by need testing solution preparation method；
(4) launch and inspect：Aspiration step (1), (2), need testing solution, control medicinal material solution, the moon obtained by (3)
Property sample solution equal volume amounts, it is each to draw 5-20 μ l, put respectively on same lamellae, with volume ratio as 1-3:1 hexamethylene-
Ethyl acetate mixture is solvent, is launched, and is taken out, and is dried, and puts and inspect under 365nm ultraviolet lamps.
2. method according to claim 1, it is characterised in that the discriminating of Radix Angelicae Sinensis composition comprises the following steps：
(1) preparation of need testing solution：Bushen Tianjing oral liquid 30ml, plus 30ml petroleum ethers (30~60 DEG C) are taken, shaking is extracted
2 times, merge petroleum ether liquid, volatilize, residue adds the ethanol 1ml to make dissolving, used as need testing solution；
(2) preparation of control medicinal material solution：Take Radix Angelicae Sinensis control medicinal material 0.5g, plus petroleum ether (30~60 DEG C) 30ml, ultrasonic extraction
30 minutes, filtration, filtrate is concentrated into 1ml, used as control medicinal material solution；
(3) preparation of negative sample solution：Other medicinal materials in addition to Radix Angelicae Sinensis are weighed by Bushen Tianjing oral liquid prescription, scarce Radix Angelicae Sinensis is made
Negative sample, the negative sample solution of scarce Radix Angelicae Sinensis is made by step (1) need testing solution preparation method；
(4) launch and inspect：Aspiration step (1), (2), need testing solution, control medicinal material solution, the moon obtained by (3)
Property each 10 μ l of sample solution, put on same lamellae, with volume ratio as 1-3 respectively:1 cyclohexane-ethyl acetate mixed solution
It is solvent, launches, take out, dry, puts and inspect under 365nm ultraviolet lamps.
3. method according to claim 1 and 2, it is characterised in that the lamellae is silica gel g thin-layer plate or silica G F254
Lamellae.
4. method according to claim 1 and 2, it is characterised in that the solvent cyclohexane-ethyl acetate mixed solution middle ring
The volume ratio of hexane-ethylacetate is 2-3:1.
5. method according to claim 4, it is characterised in that the solvent cyclohexane-ethyl acetate mixed solution cyclohexane
The volume ratio of-ethyl acetate is 2:1.
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| CN107478762B (en) * | 2017-08-16 | 2018-05-22 | 河南太龙药业股份有限公司 | The discriminating of children's compound the membrane of a chicken's gizzard chewable tablets and content assaying method |
| CN109975469A (en) * | 2017-12-27 | 2019-07-05 | 苏州唐锟辰新能源科技有限公司 | The quality determining method of dog kidney in a kind of NANBAO JIAONANG |
| CN110988194A (en) * | 2019-12-26 | 2020-04-10 | 广州白云山敬修堂药业股份有限公司 | Detection method of traditional Chinese medicine compound preparation for tonifying kidney and replenishing essence |
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Application publication date: 20170627 |