六 味 地 黃 丸

1、六 味 地 黃 丸LiuweidihuangwanRadix Rehma-nniae Preparata 160gFructus Corni (processed) 80gIngredientsCortex Moutan 60 g Rhizoma Dioscoreae80gPoria 60 g Rhizoma Alismatis 60 g pulverize: 研磨研磨 sift：評審，過篩：評審，過篩 q Procedure/Procedure/制法制法Pulverize the above six ingredients to fine powder, sift and mix well.

2、 To each 100 g of the powder add 3550 g of refined honey and a quantity of water to make pills and dry; alternatively add 80110 g of refined honey to make small honeyed pills or big honeyed pills.make pills : 泛丸泛丸q DescriptionBrown-black water-honeyed pills, black-brown small honeyed pills or big ho

3、neyed pills; taste, sweet and sour.q IdentificationMicroscopicalStarch granules triangular-ovoid or oblong, 2440m in diameter, hila short cleft or V-shaped. Irregular branched masses color less, dissolved in chloral hydrate solution: hyphae colorless, 46m in diameter. Parenchyma greyish-brown to bla

4、ck-brown, cells mostly shrunken, and each containing a brown nucleus-like mass. cleft：裂縫：裂縫 hyphae：菌絲：菌絲nClusters of calcium oxalate occurring in colourless parenchymatous cells, sometimes several clusters arranged in rows. Epidermal cells of pericarp orange-yellow, polygonal in surface view, with s

5、omewhat beaded anticlinal walls. Parenchymatous cells subrounded, with elliptical pits, gathered into pit groups, epidermal: 表皮的表皮的 pericarp: 果皮果皮 beaded anticlinal walls:垂周壁念珠狀增厚垂周壁念珠狀增厚anticlinal walls of the endodermis cells sinuous, thickened, lignified, with slender pit-canals.Pulverize 6 g of

6、the water-honeyed pills, or triturate 9 g of the small honeyed pills or big honeyed pills with 4 g of kieselguhr and triturate well. Heat under reflux with 40 ml of ether at a low temperature for 1 hour, cool , filter and evaporate to remove ether. kieselguhr: 硅藻土硅藻土 triturate: 研勻研勻 Physical and Che

7、mical identification Dissolve the residue in 1 ml of acetone as the test solution. Dissolve paeonol CRS in acetone to produce a solution containing 1 mg per ml, as the reference solution. Carry out the method for thin layer chromatography (Appendix B), using silica gel G as the coating substance and

8、 cyclohexane-ethyl acetate(3:1) as the mobile phase. paeonol: 丹皮酚丹皮酚 cyclohexane: 環(huán)己烷環(huán)己烷 Apply separately to the plate 10l of each of the two solutions. After developing and removal of the plate, dry it in air, spray with 5% solution of ferric chloride in ethanol acidified with hydrochloric acid and

9、 visualize under a current of hot air. The bluish-brown spot in the chromatogram obtained with the test solution corresponds in position and colour to the spot in the chromatogram obtained with the reference solution. ferric chloride：三氯化鐵：三氯化鐵 hydrochloric acid ：鹽酸鹽酸 AssaynDistil 2 g of the big hone

10、yed pills (or 5 g of the water-honeyed pills or small honeyed pills), accurately weighed, collect 450 ml of distillate, transfer to a 500 ml volumetric flask and dilute with water to volume. Carry out the method for spectrophotometry (Appendix A), measure the absorbance at 274 nm and calculate the c

11、ontent of paeonol (C9H10O3), taking 862 as the value of E1%1cm. distil: 蒸餾蒸餾 volumetric flask: 容量瓶容量瓶 spectrophotometry: 分光光度法分光光度法nIt contains not less than 0.90 mg per gram of water-honeyed pills, 0.70 mg per gram of small honeyed pills, or 0.63 mg per gram of big honeyed pills, of paeonol (C9H10O

12、3), refered to Cortex Mountan.Fructus Cornin To 5 g of pills, accurately weighed, add 30 ml of water, allow to disintegrate thoroughly on a warm water bath, add 2 g of the kieseguhr, stir well and filter through filter paper. Wash the residue with 30 ml of water, dry at 100 and grind into fine powde

13、r. Transfer the powder together with the filter paper to a Soxhelts extractor and heat under reflux with an appropriate quantity of ether for 4 hours. disintegrate/溶解；溶解； grind/成粉末；成粉末； Soxhelts extractor/索氏提取器索氏提取器 Recover the ether and macerate the residue with two 15ml quantities of petroleum eth

14、er (3060) for about two minutes each time. Decant the petroleum ether, dissolve the residue in a mixture of absolute ethanol-chloroform (3:2) by warming. Transfer accurately the solution to a 5 ml volumetric flask, dilute to volume, mix well, use the solution as the test solution. macerate：浸軟：浸軟 dec

15、ant：倒出倒出 absolute ethanol：無水乙醇無水乙醇 Dissolve ursolic acid CRS, weighed accurately, in absolute ethanol to produce a solution containing 0.5 mg per ml as the reference solution. Carry out the method for thin layer chromatography (Appendix B), using silica gel G as the coating substance and a mixture o

16、f cyclohexane-chloroform-ethyl acetate-formic acid (20:5:8:0.1) as the mobile phase. Apply separately to the plate 5 l test solution of the water-honeyed pills or 10 l of the test solution of the big or small honeyed pills, 4l and 8 l of the reference solution alternately. ursolic acid: 熊果酸熊果酸 formi

17、c acid: 甲酸甲酸 After developing and removal of the plate, dry it in air, and spray with 10% solution of sulfuric acid in ethanol. Heat at 105 for 57 minutes to the spots clear. Cover the plate with a glass plate of the same size and fix up with adhesive plaster. Carry out the method for thin layer chr

18、omatography ( thin layer chromatographic scanning method. Appendix B), scan at wavelength: S=520 nm, R =700 nm. Measure the integration values of absorbance of the test solution and the reference solution, calculate the content of ursolic acid in the egration values: 吸光度值吸光度值 熟地黃熟地黃 二氫蜜力苷二氫蜜力苷Action