1、 Pharmacopoeia standard of Fructus aurantii Immaturus
Fructus aurantii Immaturus
Zhishi
AURANTII FRUCTUS IMMATURUS
[character] this product is hemispherical, a few are spherical, with a diameter of 0.5 ~ 2.5cm. The exocarp is dark green or brown, with granular protrusions and wrinkles, and there are obvious style remnants or fruit stem marks. On the cut surface, the mesocarp is slightly uplifted, 0.3-1.2cm thick, yellowish white or yellowish brown, with 1-2 rows of oil chambers on the edge, and brown pulp capsules. It is hard. It has a light fragrance and a bitter, slightly sour taste.
[identification] (1) the powder of this product is light yellow or brownish yellow. Mesocarp cells were round or irregular in shape, and most of the walls were unevenly thickened. The epidermal cells of pericarp are polygonal, square or rectangular in appearance, with stomatal rings, 18-26 μ m in diameter, and 5-9 accessory guard cells; Lateral view of the cuticle. Calcium oxalate crystals exist in pericarp and juice sac cells, which are oblique square, polyhedral or biconical, with a diameter of 2-24 μ M. Hesperidin crystals exist in parenchyma cells, yellow or colorless, in round or amorphous masses, and some show radial texture. Fragments of the oil chamber were more common, and the secretory cells were narrow and curved. .
(2) Take 0.5g of this product powder, add 10ml of methanol, sonicate for 20 minutes, filter, evaporate the filtrate, and add 0.5ml of methanol to dissolve the residue as the test solution. . According to the test of thin-layer chromatography (general rule 0502), suck 2 μ l of each of the above two solutions, dot them on the same silica gel G thin-layer plate, use the upper solution of n-butanol glacial acetic acid water (4:1:5) as the developing agent, develop, take out, dry, spray 0.5% ninhydrin ethanol solution, heat at 105 ℃ until the spots are clear. In the chromatogram of the test sample, spots with the same color appear at the corresponding position of the chromatogram of the control sample.
[check] moisture Not more than 15.0% (the fourth method of general rule 0832).
Total ash .
[extract] According to the hot leaching method under the determination of alcohol soluble extract (general rule 2201), 70% ethanol is used as solvent, which shall not be less than 12.0%.
[content determination] determine according to HPLC (general rule 0512).
; Octadecylsilane bonded silica gel was used as filler; The mobile phase was methanol potassium dihydrogen phosphate solution (0.6g potassium dihydrogen phosphate, 1.0g sodium dodecyl sulfonate, 1ml glacial acetic acid, dissolved with water and diluted to 1000ml) (50:50); The detection wavelength is 275nm. The number of theoretical plates should not be less than 2000 according to the simflynn peak.
Preparation of reference solution Take a proper amount of synephrine reference substance and weigh it accurately. Add water to make a solution containing 30 μ g per 1ml.
Preparation of test solution Take about 1g of the powder in this product, accurately weigh it, place it in a corked conical flask, precisely add 50ml of methanol, weigh it, heat it for reflux for 1.5 hours, cool it, weigh it again, use methanol to make up the lost weight, shake it well, filter it, accurately measure 10ml of the continuous filtrate, evaporate it to dryness, add 10ml of water to dissolve the residue, pass it through a polyamide column (60-90 mesh, 2.5G, inner diameter 1.5cm, dry packed column), elute with 25ml of water, collect the eluent, transfer it to a 25ml volumetric flask, add water to the scale, shake it well, and then get it.
Assay Precisely suck 10 ～ 20 μ l of the reference solution and the test solution respectively, inject them into the liquid chromatograph, and determine.
The content of synephrine (C9H13NO2) in this product shall not be less than 0.30% according to the calculation of dry product.
Decoction pieces
[processing] Fructus aurantii Immaturus Remove impurities, wash, moisten thoroughly, slice and dry.
The product is irregular arc-shaped strip or circular flake. The cut exocarp is dark green to dark brownish green, the mesocarp part is yellowish white to yellowish brown, there are 1-2 rows of punctate oil chambers near the outer edge, and there are brownish pulp capsules in the inner side of the strip or in the center of the disc. It has a light fragrance and a bitter, slightly sour taste.
[identification], [inspection], [extract], [content determination] are the same as those of medicinal materials.
Stir fried Fructus aurantii with bran Take Zhishi tablets and stir fry them according to the bran frying method (general rule 0213) until the color turns dark.
This product is shaped like citrus aurantium tablets, with dark color and some spots. It smells burnt, tastes slightly bitter and sour.
[check] moisture No more than 12.0% for the same medicinal materials.
[identification] [inspection] (total ash) [content determination] is the same as that of medicinal materials.
[nature, taste and meridian tropism] bitter, pungent, sour, slightly cold. Return to spleen and stomach meridian.
[functions and indications] it can break Qi, eliminate accumulation, and dissipate phlegm and swelling. It is used for stagnation, fullness and pain, diarrhea and diarrhea, constipation, phlegm stagnation and gas obstruction, chest obstruction, chest knot, and organ sagging.
[usage and dosage] 3 ~ 10g.
[note] pregnant women should use it with caution.
[storage] store in a cool and dry place to prevent moths.
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2、 Chemical constituents of Fructus aurantii Immaturus
1. lime fruit containsHesperidin（hesperidin），Neohesperidin（neohesperidin）， Naringin,Synephrine (synephrine), n-methyltyramine. When the fruit is immature, it containsNaringin，Vernicidin（rhoifolin），Honeysuckle glycoside（lonicerin），Neohesperidin, when the fruit is ripeNeohesperidinDisappear. It is also reported that the peel also containsNobiletin(nobiletin), namely 5,6,7,8,3 ', 4' - hexamethoxy flavone,Hesperidin，Hesperidin(4', 5,6,7,8-pentamethoxyflavone), namely tangerine, 5,7,4' - trimethoxy flavone, 5,6,7,3 ', 4' - pentamethoxyflavone, namely sinensis, 5,7,8,4 '- tetramethoxyflavone and 5,7,8,4' - pentamethoxyflavone. Seed containsLimonin,Limonin（limonin），Nomilin（nomilin），Berberine（obacunone）， Deacetylnomilinic acid, isocitric acid, nomilinic acid and their 17- β - D-glucoside, and 19-hydroxydeacetylnomilinic acid-17- β - D-glucoside.
2. naringenin-7-ruti-noside in sweet orange fruit, i.eRutinPomelo peelglycoside（narirutin）， Isosaku-ranetin-7-rutinoside,Sacroside（eriocitrin）， Naringenin-4 '- glucoside-7-rutinoside,Synephrine ， N-methyltyramine. Pericarp containsHesperidin、Naringin, citrusin a, B, C,Coniferoside（coniferin），Syringin（syringin）， Dehydroconiferyl alcohol-4 - β - D-glucoside, 2-O - β - xylosylvitexin, 3-hydroxy-5, 6, 7, 8, 3 ', 4' - hexamethoxyflavone-3 β - glucoside, namely nobiletin-3-o - β - glucoside (fig nobiletin-3-o - β -glucoside), 3,8-diglucosylapigenin (3,8-di-c-glucosylapigenin), 3,8-diglucosylgeranyl lignin (3, 8-di-C-glucosyldiosmetin）， Trans-carveol-6 β -glucopyranoside, a-terpineol-8 - β -d-glucopyranoside, 9-hydroxylinalool-9 - β -glucopyranoside, vomifoliol-9-o - β -d-glucopyranoside,NaringinIsoglycosides. It also contains kumquatNobiletin, 5,7,4 '- trimethoxyflavone, 5,7,3', 4 '- tetramethoxyflavone andHesperidin, citrusin Ⅱ, Ⅲ, Ⅳ.
3. Tongju fruit containsHesperidin，Naringin，Neohesperidin, poncirin,palmitic acid（palmitic acid）， Stearic acid, oleic acid, linoleic acid, linolenic acid,Synephrine ， . Immature fruits contain poncimarin, ISO poncimarin, 7-geranyloxycoumarin, namely aurapten, 6-methoxyglucolactone,Bergamot lactone（bergapten）、Imperatorin（imperatorin）。 Seed containsIsoanisolactone（isopimpinellin），Epoxy peucedane(prangenin), namely heraclenin, prangeninhydrate, citrus lactone,Imperatorin, glucolactone, 6-methoxyglucolactone andLimoninLimonin analogues such as norepine acetate, Yichang nerobilin, norepine acetate, isocitric acid, etc.
The peel contains volatile oil (0.469%), which consists of a-pinene, β - pinene, myrcene, limonene, camphene, γ - Terpinene, p-cymene and caryophyllene.
3、 Pharmacological effects of Fructus aurantii Immaturus
1. effect on uterus: the decoction of Fructus aurantii Immaturus and Fructus aurantii Immaturus from three different origins (Sichuan, Jiangxi, Hunan) showed inhibitory effect on mouse uterus in vitro (pregnant and nonpregnant); . It has also been proved in rabbits that uterine fistula can make the uterus contract forcefully, increase the tension, and even produce tetanic contraction. Aurantium aurantium tincture and aurantium aurantium flow extract also have excitatory effects on rabbit uterus (in vivo and in vitro); However, it was inhibited in mouse uterus (ex vivo). An alkaloid like substance isolated from citrus aurantium and citrus aurantium also has a certain contractile effect on the isolated rabbit uterus, especially the myometrium excited by pituitrin; Except the alkaloid, it has a relaxing effect on the isolated rabbit uterus. After the excitation of pituitrin, the relaxation effect of the uterus is more obvious. Cirantin isolated from the peel of citrus aurantium can inhibit the activity of hyaluronidase around the ovary, which may be related to its contraceptive effect (preventing fertilization).
; In vivo, the intestinal tract of rabbits was mostly inhibited, and a few remained unchanged. The tincture of Fructus aurantii Immaturus and its flow extract inhibited the intestinal tract of mice (ex vivo) and rabbits (in vivo and ex vivo). High concentration (1:1000) inhibited the effects of acetylcholine and histamine on isolated rabbit and guinea pig small intestine; Low concentration (1:10000) can present excitatory effect, with increased amplitude and frequency after brief inhibition. The eutopic intestine of anesthetized dogs was also significantly inhibited by decoction; However, for dogs with gastroenterostomy, it has a certain excitatory effect and can make the contraction rhythm of gastrointestinal motility powerful.
3. effects on heart and blood vessels: it is a small amount of excitation and a large amount of inhibition on toad isolated heart. This is true of the decoction of Fructus aurantii Immaturus and Fructus aurantii Immaturus, tincture of Fructus aurantii Immaturus and flow extract. Using the decoction or alcohol extract of Fructus aurantii Immaturus to give dogs intravenous injection can cause significant pressor effect. The decoction of Fructus aurantii Immaturus and Fructus aurantii Immaturus from three different origins was proved to have mild vasoconstrictive effect by toad whole-body vascular perfusion method; It has a significant and rapid pressor effect on anesthetized dogs. It does not have respiratory depression and post depressor phenomenon caused by epinephrine pressor, nor does its heart rate increase significantly.
The mechanism of pressor is related to the following factors: 3.1. excite α receptors, causing vasoconstriction in some organs (anilinoline can turn pressor into depressor response).
3.2. myocardial contraction is strengthened and cardiac output is increased (isolated guinea pig heart perfusion and cardiopulmonary preparation). After reserpinization, the pressor effect of Fructus aurantii Immaturus was more significant. It has a very significant effect on increasing coronary flow in anesthetized dogs with Fructus aurantii Immaturus (bubble flowmeter, coronary flow can be increased by 289.4%), cerebral and renal blood flow also increased by 86.4% and 64.5% on average, which is significantly different from that of norepinephrine; Femoral artery blood flow decreased and myocardial oxygen consumption increased slightly, but not significantly, which was not parallel to the significant increase in coronary flow. . Alkaloids isolated from Fructus aurantii Immaturus and Fructus citri can also temporarily enhance the tension of vascular smooth muscle, especially after the action of pituitrin.
4. antithrombotic: 0.1g/ml of Zhishi decoction has obvious antithrombotic effect in vitro.
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6. other effects: citrus plant mucilage can reduce the content of cholesterol in serum and liver of rats (fed with cholesterol containing feed). The alcohol extract of Fructus aurantii Immaturus has inhibitory effect on Mycobacterium tuberculosis H37Rv in the test tube, and its inhibitory concentration is 1:1000. Its decoction has no effect on guinea pig bronchus. It has been reported that citrus juice can promote the fermentation rate of (bread) yeast, and the activity does not decrease after boiling, so it is not an enzymatic component. The main medical use of orange juice is that it is rich in vitamin C, and contains a considerable amount of vitamin A and B. the skin does not contain vitamin C, but is rich in vitamin A. It tastes bitter and can strengthen the stomach. .