Identification of raw herbs
[property identification]
Stem fleshy, long cylindrical, sometimes slightly flattened, slightly curved, 3-15cm long, 5-15cm in diameter, tapering upward, 2-5cm in diameter, some cut into segments, similar in diameter above and below. Gray-brown or tan sepals with longitudinal grooves and densely imbricate veins, scale-leaved rhombuses or triangles, 0.5-1.5 cm wide, 2 mm thick, meniscus leaves left after scale leaves fall off trace. Solid quality, not easy to break. The section is brown, with light brown vascular dots, and the ring is in deep wavy or jagged. Wood accounts for about 4/5, sometimes hollow. Surface and cross-section in the light can sometimes see the small bright spots of crystal. Gas slightly, sweet, slightly bitter. It is better to use stout, dense scales, and soft skin.
[Microscopic identification]
Stem cross-section: The epidermis is a column of flat cells outside the stratum corneum. The cortex is composed of dozens of parenchyma cells, closely arranged, and the cells near the vascular bundle are pitted with scattered leaves and vascular bundles. Vascular ligaments, usually 16-22 arranged in deep wavy or zigzag rings; phloem parenchyma cells closely arranged, sometimes divided into decadent; formation layer is not obvious; visible xylem fibers in the xylem. The ray is obvious. The pith is more fractal. Cortical and medullary parenchyma cells contain starch grains. Cross-section of scale leaf: 1 row of epidermis cells, flat and rectangular, with thin cuticle. One column of the epithelium is slightly larger. The mesophyll tissues are all spongy tissues. The cells are round, thin, and contain chloroplasts with small cell gaps. Vascular 5-7, externally tough, tangentially arranged.
[Chemical Identification of Traditional Chinese Medicine]
1. Take the product powder 0.5g, add 70% ethanol 5ml, the water bath warm 10min, filtered. The filtrate was evaporated to dryness, and 1 ml of glacial acetic acid was poured into a test tube. 1 ml of sulfuric acid was added along the wall of the tube, and a brown-red ring was formed at the interface between the two liquids. (Check crickets)
2. Take the product powder 0.5g, plus 1% hydrochloric acid solution 5ml, the water bath warm 20min, filtered. The filtrate was spiked with potassium iodide reagent to produce a brown-red precipitate. (check alkaloids)
3. Thin-layer chromatography to take the product powder 1g, add ethanol 10ml 2h, filtered. The filtrate was evaporated to dryness and dissolved in 1 ml of ethanol for test solution. Another mannitol, ethanol dissolved into a solution containing 1mg per ml as a reference solution. Take the above two solutions each 10μm, respectively, spotted on the same silica gel H sheet, with n-butanol - glacial acetic acid ethanol - water (4:1:1:2) spread, spread out 12cm, remove and air dry, spray 10% The ceric ammonium nitrate solution was developed. The test liquid chromatogram has the same brown-yellow spots on the corresponding positions of the reference chromatogram. The medicinal material is based on the fleshy stem of Cistanche deserticola. Usage and dosage Oral: decoction, 10-15g; or into the pill, scattered; or dip. Source "Chinese Materia Medica"
Physical and chemical identification
1. Take 1g of the product powder, add 8ml of ethanol solution containing 0.5% hydrochloric acid, and heat to reflux for 10 minutes. While hot filtration, add the ammonia solution to the filtrate and adjust to neutrality. Evaporate and dry. Add 3ml of 1% hydrochloric acid solution to dissolve the residue. Over. Take filtrate 1ml, add cesium-potassium iodide test solution 1 to 2 drops, generate orange red or red-brown precipitate.
2. Take the product powder 1g, add methanol 10ml, ultrasonic treatment for 10 minutes, filtered, the filtrate as a test solution. Another water chestnut past control; add methanol to make a solution containing 2.5mg per 1ml as a reference solution. 5 μl of each of the above two solutions was pipetted onto the same silica gel G plate, and an ethyl acetate-methanol 9% acetic acid solution (20:3:2) was used as a developing agent to expand, remove, dry, and spray. % ferric chloride ethanol solution. In the chromatogram of the test product, the same coloured spots are present in the corresponding positions of the chromatograms of the reference substance.
3. Take the product powder 1g, add 80% ethanol 10ml, heated to reflux for 10 minutes, filtered, the filtrate as a test solution. Another Cistanche control medicine 1g, with the legal system as the reference drug solution. Then take the betaine reference substance, add 80% ethanol to make a solution containing 5mg per 1ml as the reference solution. 5 μl of each of the above three solutions was pipetted onto a thin layer of silica gel G with the same sodium carboxymethyl cellulose as the binder. Methanol-water-acetic acid (9:2:0.5) was used as a developing agent to develop and remove the solution. , Dry, spray with modified potassium iodide test solution. In the chromatogram of the test sample, the spot with the same color was found in the position corresponding to the chromatogram of the reference drug; the same orange-red spot was observed in the position corresponding to the chromatogram of the reference substance.
[Content determination]
Chromatographic conditions and system suitability test: using octadecylsilane bonded silica as a filler; acetonitrile-methanol 1% acetic acid solution (10:15:75) as the mobile phase; detection wavelength of 334nm. The number of theoretical plates calculated according to the ergot glycoside peak should not be less than 3,000. Preparation of reference solution: Accurately weighed 4 mg ergot bitter bitter reference substance in a volumetric flask of 25 ml brown, add the mobile phase to the mark, and shake well, that is to say (every 1 ml contains ergot glycoside 160 μg). Preparation of the test solution: take the product powder (passing No. 4 sieve) about 1g (at the same time, take the product powder to determine moisture), accurately weighed, set in a 100ml brown volumetric flask, precision add methanol 50ml, stuffed, shake Evenly, weigh the weight, immerse for 0.5 hours, sonicate (power 250W, frequency 40kHz) for 40 minutes (below 50°C), take out, let cool, weigh it again, make up for lost weight with methanol, shake, centrifuge, The supernatant was filtered through a microporous membrane (0.45 μm) and the filtrate was placed in a brown volumetric flask. Assay: Precisely draw 5 μl of the reference solution and 5 to 10 μl of the test solution. Inject to the liquid chromatograph to determine, ie, to obtain. The product is based on dry products, containing ergot glycosides (C29H36O15) not less than 0.080%.
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