CN102879394A - Rapid testing method for authentic Chinese rhubarb seeds - Google Patents
Rapid testing method for authentic Chinese rhubarb seeds Download PDFInfo
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- CN102879394A CN102879394A CN201210376207XA CN201210376207A CN102879394A CN 102879394 A CN102879394 A CN 102879394A CN 201210376207X A CN201210376207X A CN 201210376207XA CN 201210376207 A CN201210376207 A CN 201210376207A CN 102879394 A CN102879394 A CN 102879394A
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Abstract
The invention discloses a rapid testing method for authentic Chinese rhubarb seeds. The method comprises the steps of 1), obtaining seeds to be tested, grinding, extracting by using methyl alcohol, filtering to obtain filter liquid, volatilizing a solvent, conducting acid hydrolysis and extracting by using an organic solvent to obtain a water layer; and 2), using the water layer obtained in the step 1), adding strong ammonia water of 1-3 times of the volume, shaking, and until no reddish brown or brown flocculent precipitation exist, identifying that the seeds to be tested are authentic Chinese rhubarb seeds. The rapid testing method for authentic Chinese rhubarb seeds is convenient to use, high in accuracy, low in cost and good in market application prospect.
Description
Technical field
The present invention relates to the detection method of genuine rhubarb seed.
Background technology
Rheum officinale is the dry root and rhizome of the ancient especially big yellow Rheum tanguticum Maxim.ex Balf. of polygonum rheum palmatum Rheum palmatum L., Tang or Rheum officinale Rheum officinale Baill..Have the logical intestines that purge heat, the effect that the stasis of blood is stimulated the menstrual flow is pursued in removing pattogenic heat from the blood and toxic material from the body.Be used for real hot constipation, stagnant stomachache, it is not well to rush down dysentery, jaundice with damp-heat pathogen, blood-head is told nosebleed, hot eyes, pharynx is swollen, abdominalgia with intestinal abscess, the carbuncle furunculosis that swells, hemostasis is through closing, and traumatic injury is controlled scald outward; Upper gastrointestinal bleeding.Sorrel is distributed in the southeast of Gansu, Qinghai, western Sichuan, northwestern Yunnan Province and Eastern Tibet; It is northern that the ancient especially big Huang of Tang is distributed in Gansu, Qinghai, Sichuan and Eastern Tibet; Rheum officinale is distributed in the ground such as Southern Shaanxi, West Henan, West of Hubei Province, Sichuan, Yunnan.North China rheum officinale, Rheum hotaoense C. Y. Cheng et C. T. Kao are common adulterant rheum officinales, easily obscure with the genuine rhubarb such as Tang ancient especially big Huang.
In recent years, because the nothing plan of wild Plant Resources of Rheum is excavated, cause wild Plant Resources of Rheum to reduce year by year, national wild Plant Resources of Rheum has been on the verge of exhaustion.Be the satisfying the market demand growing to the high-quality rheum officinale, rheum officinale artificial growth scale constantly enlarges, and the pure seed of quality is the prerequisite of the planting of medicinal materials, is the basic guarantee that improves root yield and quality.
At present, China's rheum officinale seed does not have test stone and quality standard, mainly is to differentiate to have certain limitation by proterties such as shape, size, color, epidermis, decorations.Application number: 201110337787.7, denomination of invention: a kind of Patent Application Publication of the method for identifying authenticity of Chinese rhubarb seed a kind of method of the rheum officinale seed of discerning the false from the genuine, it comprises the steps: that (1) get seed to be checked, extracts Chrysophanol and archen in the seed to be checked; (2) content of Chrysophanol and archen in the mensuration rheum officinale seed; (3) ratio of calculating Determination of chrysophanol/emodin content; (4) ratio in judgement of calculating according to step (3): be the genuine rhubarb seed if ratio, is judged this seed greater than 1, if ratio is less than or equal to 1, judge that this seed is adulterant rheum officinale seed.The method determines by the ratio of Chrysophanol in the seed and emodin content whether the rheum officinale seed is certified products, and difficult because of the Accurate Measurement component content, error is larger, and it is inconvenient to cause the method to be used, and accuracy is not high enough.Especially for the situation of doped portion adulterant in the genuine rhubarb seed, get the wrong sow by the ear easily, be difficult to substitute traditional detection method.
Need to seek a kind of more easy, accurate, reliable method and identify certified products, adulterant, and the method for the positive pseudo-rheum officinale seed that mixes.
Summary of the invention
In order to address the above problem, the invention provides a kind of detection method of genuine rhubarb seed.
The detection method of genuine rhubarb seed of the present invention, it comprises the steps:
1) get seed to be checked, pulverize, extract with methyl alcohol, filter, get filtrate, fling to solvent, organic solvent extraction is used in acid hydrolysis, gets water layer;
2) getting step 1) gained water layer, add the strong aqua of 1 ~ 3 times of volume, jolt, to the sepia flocculent deposit, is genuine rhubarb seed with Seed Identification to be checked without rufous.
Wherein, the described acid hydrolysis of step 1), hydrionic concentration is 0.52 ~ 2mol/L in the solution; Organic solvent is ether.
Preferably, in the described step 1), seed meal to be checked is broken into fine powder, add methyl alcohol, the mass volume ratio of fine powder and methyl alcohol is 1:15 ~ 25, soaks 30min ~ 90min, filter, get filtrate, evaporate to dryness, add water, add concentrated hydrochloric acid again, the hydrochloric acid volume is 1/20 ~ 1/5 of water volume, add hot reflux 20 ~ 40min, extracted with diethyl ether is used in cooling, extract 2 times, each used ether volume is 3 ~ 5 times of water volume, gets water layer.
In the detection method of genuine rhubarb seed of the present invention, only have pure genuine rhubarb rufous just can not occur to the sepia flocculent deposit, as long as contain the adulterant seed in the seed to be checked, rufous will appear to the sepia flocculent deposit, therefore for the situation of doped portion adulterant seed in the genuine rhubarb seed, also be easy to it is detected.
Genuine rhubarb detection method of the present invention accuracy is high, convenient and simple for operation, quick, can substitute traditional detection method, has a good application prospect.
Obviously, according to foregoing of the present invention, according to ordinary skill knowledge and the customary means of this area, not breaking away under the above-mentioned basic fundamental thought of the present invention prerequisite, can also make modification, replacement or the change of other various ways.
The embodiment of form is described in further detail foregoing of the present invention again by the following examples.But this should be interpreted as that the scope of the above-mentioned theme of the present invention only limits to following example.All technology that realizes based on foregoing of the present invention all belong to scope of the present invention.
Description of drawings
Fig. 1 detects Seeds Structure to be checked with detection method of the present invention;
Fig. 2 detects Seeds Structure to be checked with detection method of the present invention.
Embodiment
1, detection method
(1) gets seed to be checked;
(2) get seed fine powder 1.0g to be checked, add methyl alcohol 15ml, soak 30min, filter, get filtrate 5ml, evaporate to dryness, residue add water 10ml makes dissolving, add again that hydrionic concentration is 1.09mol/L in the concentrated hydrochloric acid 0.5ml(gained dilute hydrochloric acid solution), added hot reflux 20 minutes, cooling divides 2 extractions with ether immediately, each 15ml gets water layer;
Water intaking layer adds the strong aqua of 1 times of volume, jolts, and observes to have or not rufous to the sepia flocculent deposit;
(3) in the step (2), water layer to the sepia flocculent deposit, is genuine rhubarb seed with Seed Identification to be checked without rufous.
1, detection method
(1) gets seed to be checked;
(2) get seed fine powder 1.0g to be checked, add methyl alcohol 20ml, soaked 1 hour, filter, get filtrate 5ml, evaporate to dryness, residue add water 10ml makes dissolving, add again that hydrionic concentration is 1.09mol/L in the concentrated hydrochloric acid 1ml(gained dilute hydrochloric acid solution), added hot reflux 30 minutes, cooling divides 2 extractions with ether immediately, each 20ml gets water layer;
Water intaking layer adds the strong aqua of 2 times of volumes, jolts, and observes to have or not rufous to the sepia flocculent deposit;
(3) in the step (2), water layer to the sepia flocculent deposit, is genuine rhubarb seed with Seed Identification to be checked without rufous.
Embodiment 3 detection methods of the present invention
1, detection method
(1) gets seed to be checked;
(2) get seed fine powder 1.0g to be checked, add methyl alcohol 25ml, soak 90min, filter, get filtrate 5ml, evaporate to dryness, residue add water 10ml makes dissolving, add again that hydrionic concentration is 1.09mol/L in the concentrated hydrochloric acid 1.5ml(gained dilute hydrochloric acid solution), added hot reflux 40 minutes, cooling divides 2 extractions with ether immediately, each 25ml gets water layer;
Water intaking layer adds the strong aqua of 3 times of volumes, jolts, and observes to have or not rufous to the sepia flocculent deposit;
(3) in the step (2), water layer to the sepia flocculent deposit, is genuine rhubarb seed with Seed Identification to be checked without rufous.
Experimental example 1 usefulness detection method of the present invention detects seed to be checked
1, experiment material
13 batches in the rheum officinale seed to be checked of buying from market, called after S1 ~ 11.
2, experimental technique
(1) identifies with traditional proterties discrimination method;
(2) detect according to embodiment 2 detection methods.
3, experimental result
(1) traditional proterties discrimination method qualification result:
S1: the achene prismatic, rib is sharp, and long 2 millimeters, brown is glossy; Fruit is by wealthy avette, and tip is blunt, full edge or the unconspicuous tooth of tool, and equal 3~4 millimeters of length and width have an avette strumae.Being accredited as the polygonaceae plant seed, is adulterant rheum officinale seed.
S2 ~ 4 and S7: fruit is bright orange brown, long 7 ~ 8.5mm, wide about 6mm, the less oval that is of seed, close with fruit color, puckery is after the plantation, according to the character of medicinal material, be accredited as the seed of North China rheum officinale Rheum franzenbachii Munt., be adulterant rheum officinale seed.
S5, S6, S8: fruit is bright orange brown, long 7 ~ 8.5mm, wide about 6mm, the less oval that is of seed, close with fruit color, puckery is after the plantation, according to the character of medicinal material, be accredited as the seed of Rheum hotaoense C. Y. Cheng et C. T. Kao Rhum hotaoense C.Y.Cheng et C.T.Kao, be adulterant rheum officinale seed;
S9 and S11: the fruit yellowish-brown is to tawny, long 7 ~ 9mm(fruit top is to base portion), the ultimate range of two fruit wing wing edge on wide 5 ~ 7mm(fruit square section), the less oval that is of seed, color is slightly darker than fruit, tawny is to brown, bitter is after the plantation, according to the character of medicinal material, be accredited as the seed of sorrel Rheum palmatum L., be the genuine rhubarb seed;
S10: the fruit yellowish-brown is to tawny, long 7 ~ 9mm(fruit top is to base portion), the ultimate range of two fruit wing wing edge on wide 5 ~ 7mm(fruit square section), the less oval that is of seed, color is slightly darker than fruit, tawny is to brown, bitter is after the plantation, according to the character of medicinal material, being accredited as ancient especially big yellow Rheum tanguticum ' the Maxim.ex Balf of Tang, is the genuine rhubarb seed.
(2) detection method qualification result of the present invention:
The result is shown in Fig. 1 ~ 2:
S1 ~ 8 rufous occurs to the sepia flocculent deposit, are accredited as adulterant rheum officinale seed; S9 ~ 11 rufous do not occur to the sepia flocculent deposit, are accredited as the genuine rhubarb seed.
The experimental result explanation, whether the testing result of the inventive method is consistent with the result of traditional discrimination method, can precise Identification seed to be checked be the genuine rhubarb seed.No matter use detection method of the present invention, as long as contain adulterant in the seed to be checked, be full adulterant rheum officinale, or the melange of adulterant and certified products rufous all can occur to the sepia flocculent deposit, only has pure genuine rhubarb seed, precipitation just can not occur, thereby accuracy is high.
To sum up, the testing result of genuine rhubarb seed detection method of the present invention is consistent with the result of traditional discrimination method, and accuracy is high, and is easy and simple to handle, with low cost, has a good application prospect and economic benefit.
Claims (3)
1. the detection method of a genuine rhubarb seed, it is characterized in that: it comprises the steps:
1) get seed to be checked, pulverize, extract with methyl alcohol, filter, get filtrate, fling to solvent, organic solvent extraction is used in acid hydrolysis, gets water layer;
2) getting step 1) gained water layer, add the strong aqua of 1 ~ 3 times of volume, jolt, to the sepia flocculent deposit, is genuine rhubarb seed with Seed Identification to be checked without rufous.
2. method according to claim 1 is characterized in that: the described acid hydrolysis of step 1), and hydrionic concentration is 0.52 ~ 2mol/L in the solution; Organic solvent is ether.
3. method according to claim 2 is characterized in that: in the described step 1), seed meal to be checked is broken into fine powder, add methyl alcohol, the mass volume ratio of fine powder and methyl alcohol is 1:15 ~ 25, soaks 30min ~ 90min, filter, get filtrate, evaporate to dryness, add water, add concentrated hydrochloric acid again, the hydrochloric acid volume is 1/20 ~ 1/5 of water volume, add hot reflux 20 ~ 40min, extracted with diethyl ether is used in cooling, extract 2 times, each used ether volume is 3 ~ 5 times of water volume, gets water layer.
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Cited By (1)
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CN103999643A (en) * | 2014-06-04 | 2014-08-27 | 湄潭县高岩玄参中药材专业合作社 | Preservation method of medicinal rhubarb seeds |
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CN102042978A (en) * | 2009-10-22 | 2011-05-04 | 中国人民解放军第三〇二医院 | Colorimetric card for quickly judging grades of Chinese medicinal materials and preparation method thereof |
CN102106907A (en) * | 2011-03-21 | 2011-06-29 | 江西汇仁药业有限公司 | Quality control method for rhubarb (traditional Chinese medicine) ethanol-extraction process |
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CN103999643A (en) * | 2014-06-04 | 2014-08-27 | 湄潭县高岩玄参中药材专业合作社 | Preservation method of medicinal rhubarb seeds |
CN103999643B (en) * | 2014-06-04 | 2016-06-08 | 湄潭县高岩玄参中药材专业合作社 | The store method of Rheum officinale seed |
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