on a water-bath, filter, add 1 mL of Fehling solution TS
to 3 mL of the filtrate and warm on a water-bath: red- dish brown precipitate is produced.
2) Weigh 1 g of pulverized Asparagus Tuber, add 5 mL of a mixture of butanol, water (40 : 7), shake for 30 mi- nutes and filter. Use the filtrate as the test solution. Per- form the test with the test solution as directed under Thin-layer Chromatography. Spot 10 μL the test solu- tion on a plate of silica gel for thin-layer chromatogra- phy. Deve1op the plate with a mixture of butanol, water and acetic anhydride (10 : 6 : 3) to a distance of about
10 cm and air-dry the plate. Spray diluted sulfuric acid TS to the plate, heat the plate at 105 o C for 2 minutes. The spot develops at about 0.4 of Rf value, a reddish brown color followed by a brown color
Loss on Drying Not more than 18.0% (6 hours).
Ash Not more than 3.0%.
Extract Content Dilute ethanol-soluble extract? Not less than 25.0%.
Aster Root
Asteris Radix
Aster Root is the root of Aster tataricus Linné fil. (Compositae)
Description Aster Root is the root, 5 cm to 15 cm in length, 1 mm to 2 mm in diameter. External surface is pale brown to reddish brown, with longitudinal wrin- kles. The fractured surface is fibrous, soft, and easily curved.
Aster Root has characteristic odor, and acrid taste. Identification 1) Weigh 0.2 g of pulverized Aster Root, add 10 mL of water, shake vigorously to mix, and filter. Add 1 to 2 drops of ferric chloride TS to 2 mL of the filtrate; a purple color develops.
2) Add 10 mL of water to 0.5 g of pulverized Aster Root, heat on a water bath and cool. Shake vigorously; a lasting fine foam is produced.
3) Weigh 0.2 g of pulverized Aster Root, add 2 mL of acetate anhydride, shake the solution on a water bath and mix. Heat for 2 minutes and filter. Add slowly 0.5 mL of sulfuric acid to make two layers: a reddish brown color develops at the zone of contact
Purity Foreign matter—Less than 5.0% of stem and other foreign material.
Loss on Drying Not more than 15.0% (6 hours). Ash Not more than 15.0%
Acid-insoluble Ash Not more than 8.0%.
KP VIII 1013
Extract Content Dilute ethanol-soluble extract— Not less than 30.0%.
Astragalus Root
Astragali Radix
Astragalus Root is the root or the root removed the pe- riderm of Astragalus membranaceus Bunge or Astraga- lus membranaceus Bunge var. mongholicus Hsiao (Le- guminosae)
Description Astragalus Root is nearly cylindrical root, 30 cm to 100 cm in length and 7 mm to 20 mm in diameter, with small bases of lateral root dispersed on the surface, twisted near the crown. External surface is pale grayish yellow to pale yellow-brown and covered with irregular, dispersed longitudinal wrinkles and ho- rizontal lenticel-like patterns. Texture is dense and dif- ficult to break and fractured surface is fibrous. Under a magnifying glass, a transverse section reveals an outer layer composed of periderm, cortex is pale yellowish white, xylem is pale yellow and zone near the cambium somewhat brown. Thickness of the cortex is from about one-third to one-half of the diameter of xylem. White medullary ray runs from xylem to cortex in thin root, but often appears as radiating cracks in thick root. Usually pith is unobservable.
Astragalus Root has slightly odor and sweet taste. Purity Root of Hedysarum species and others— Under a microscope, a vertical section of Astragalus Root reveals no crystal fiber containing solitary crystals of calcium oxalate outside the fiber bundle. Loss on Drying Not more than 13.0% (6 hours). Ash Not more than 5.0%.
Acid-insoluble Ash Not more than 1.0%.
Atractylodes Rhizome
Atractylodis Rhizoma
Atractylodes Rhizome is the rhizome of Atractylodes lancea De Candlle or of Atractylodes chinensis Koid- zumi (Compositae).
Description Atractylodes Rhizome is irregularly curved, cylindrical rhizome, 3 cm to 10 cm in length and 10 mm to 25 mm in diameter. External surface is dark grayish-brown to dark yellow-brown. A transverse section reveals nearly orbicular, with pale brown to red-brown secretes as fine points. Often white cotton- like crystals are produced on its surface if Atractylodes
1014 Monographs, Part II
Rhizome is stored long time.
Under a microscope, a transverse section usually re- veals no fiber in parenchyma of cortex, and the end re- gion of medullary rays reveals oil sacs containing pale brown to yellow-brown substances. Xylem exhibits vessels surrounded by fiber bundles and arranged ra- dially on the region adjoining the cambium. Pith and medullary rays exhibit the same oil sacs as in the cortex. Parenchyma cells contain spherocrystals of inulin and fine needles of calcium oxalate.
Atractylodes Rhizome has characteristic odor and slightly bitter taste.
Purity Atractylodes rhizome white—Weigh 0.5 g of pulverized Atractylodes Rhizome, macerate with 5 mL of ethanol by warming on a water-bath for 2 minutes and filter. To 2 mL of the filtrate, add 0.5 mL of vanil- lin-hydrochloric acid TS and shake immediately: no red to red-purple color develops within l minute. Ash Not more than 7.0%.
Acid-insoluble Ash Not more than 1.5%. Essential oil Not less than 0.7 mL (50.0 g).
Atractylodes Rhizome White
Atractylodis Rhizoma Alba
Atractylodes Rhizome White is the rhizome, with or without periderm, of Atractylodes japonica Koidzumi or Atractylodes macrocephala Koidzumi (Compositae), or from which the periderm has been removed. Description (1) Atractylodes japonica—Atractylodes Rhizome White from Atractylodes japonica is rhizome, from which periderm is removed, in a irregular mass or irregularly curved cylinder, 3 cm to 8 cm in length and 2 cm to 3 cm in diameter. When periderm is remained, external surface is balckish brown, sometimes in a pro- truding knot-shape, with coarse wrinkles. Texture is difficult to break and the fractured surface is fibrous. Under a microscope, a transverse section reveals peri- derm with stone cell layers, often fiber bundles at the outside of the phloem in the parenchyma of the cortex, and oil sacs containing pale brown to brown substances at the end of medullary rays. The xylem reveals small and radially lined vessels surrounding pith, and distinct fiber bundle surrounding these vessels. The pith and medullary rays contain oil sacs similar to those in cor- tex. The parenchyma tissues contain small crystals of inulin and needle crystals of calcium oxalate.
Atractylodes Rhizome White from Atractylodes japo- nica has characteristic odor and somewhat bitter taste. (2) Atractylodes macrocephala—Atractylodes Rhi- zome White from Atractylodes macrocephala is the rhizome, in a shape of irregularly enlarged mass, 3 cm
to 13 cm in length and 15 mm to 70 mm in diameter. External surface is grayish yellow or dark brown, hav- ing sporadic, knob-like small protrusions, interrupted longitudinal wrinkles and grooves, and scars of fibrous rootlets. Remains of stems and bud scars are attached to the apex. Texture is hard and difficult to be broken. The fractured surface is not flat and yellowish white to pale brown, and scatterd with yellowish brown oil sacs. The fractured surface of dried materials by baking is horn- like shape, relatively deep colored or cracked. Under a microscope, transverse section reveals interrupted band of needle crystals of calcium oxalate between cork cells and the cortex. Oil sacs containing brown substances are scattered in the cortex and medullary rays. The pa- renchyma cells sometimes contain needle crystals of calcium oxalate and inulin.
Atractylodes Rhizome White from Atractylodes macro- cephala has characteristic odor, sweet taste, and viscos- ity on chewing.
Identification Weigh 0.5 g of pulverized Atracty- lodes Rhizome White, add 5 mL of ethanol by warming on a water-bath for 2 minutes and filter. To 2 mL of the filtrate, add 0.5 mL of vanillin-hydrochloric acid TS and shake immediately: a red to reddish purple color develops and persists.
Purity Atractylodes lancea rhizome—Weigh 2 g of pulverized Atractylodes Rhizome White, add 5.0 mL of hexane, shake for 5 minutes, filter and use this filtrate as the test solution. Perform the test with this solution as directed under the Thin-layer Chromatography. Spot 10 μL of the test solution on a plate of silica gel for thin-layer chromatography. Develop the plate with a
mixture of hexane and acetone (7 : 1) to a distance of about 10 cm and air-dry the plate. Spray evenly p- dimethylaminobenzaldehyde TS for spraying on the plate and heat at 100 °C for 5 minutes: no green to grayish green spot appears between R0.3 and 0.6. Ash Not more than 7.0%.
Acid-insoluble Ash Not more than 1.0%.
Essential Oil Content Not less than 0.7 mL (50.0 g).
Belladonna Extract
Belladonna Extract contains not less than 0.85% and not more than 1.05% of total alkaloids [as hyoscyamine (C17H23NO3: 289.37)].
Method of preparation Weigh 1000 g of a coarse
powder of Belladonna Root, add 4 L of 35% Ethanol and digest for 3 days. Press the mixture, add 2000 mL of 35% Ethanol to the residue and digest again for 2 days. Combine all the extract and allow to stand for 2 days. Filter and prepare the viscous extract as directed
under Extract. A appropriate quantity of Ethanol and
Purified Water may be used in place of 35% Ethanol.
Description Belladonna Extract is a dark brown, has characteristic odor and bitter taste.
Identification Mix 0.5 g of Belladonna Extract with 30 mL of ammonia TS in a flask, transfer the mixture to a separatory funnel, then add 40 mL of ethyl acetate and shake the mixture. Drain off the ethyl acetate layer, add 3 g of anhydrous sodium sulfate to the ethyl acetate, shake and filter after the ethyl acetate become clear. Evaporate the filtrate to dryness in vaccum, dissolve the residue in 1 mL of ethanol and use this solution as the test solution. Proceed as directed in the Identifica- tion under Belladonna Root.
Assay Weigh accurately about 0.4 g of Belladonna Extract, place in a glass-stopperd centrifuge tube, add 15 mL of ammonia TS and shake. Add 25 mL of ether, stopper tightly, shake for 15 minutes, centrifuge and separate the ether layer. Repeat this procedure twice with the water layer, using 25 mL each of ether. Com- bine the extracts and evaporate the ether on a water- bath. Dissolve the residue in 5 mL of the mobile phase, add 3.0 mL of the internal standard solution and add the mobile phase to make exactly 25 mL. Proceed as di- rected in the Assay under Belladonna Root.
Amount (mg) of hyoscyamine (C17 H 23 NO3 ) = amount (mg) of Atropine Sulfate RS, calculated on the dried basis × Q T 1
Q× 5 × 0.8551
S Internal standard solution—A solution of brucine dihyrate in the mobile phase (1 in 2500)
Packaging and Storage Preserve in light-resistant, tight containers. Store in a cold place.
Belladonna Root
Belladonnae Radix
Belladonna Root is the root of Atropa belladonna Linné (Solanaceae). Belladonna Root, when dried, con- tains not less than 0.4% of total alkaloids [as hyoscya- mine (C17-H23NO3: 289.37)].
Description Belladonna Root is the root, cylindrical, with longitudinal wrinkles, 10 cm to 30 cm in length and 5 mm to 40 mm in diameter. Belladonna Root is often cut crosswise or lengthwise. External surface is grayish brown to grayish yellow-brown. Periderm of Belladonna Root is often removed. Fractured surface is pale yellow to pale yellow-brown and much powdery.
KP VIII 1015
Belladonna Root is almost odorless and has bitter taste. Identification Weigh 2 g of pulverized Belladonna Root in a glass-stoppered centrifuge tube, add 30 mL of ammonia TS, sonicate for 5 minutes and centrifuge. Pi- pet the supernatant in separatory funnel, add 40 mL of ethyl acetate, shake, separate the ethyl acetate layer, add 3 g of anhydrous sodium sulfate, shake and filter after the solution is clear. Evaporate ethyl acetate in vaccum, dissolve the residue in 1 mL of ethanol and use this solution as the test solution. Separately, weigh 2 mg of Atropine Sulfate RS, dissolve in 1 mL of etha- nol and use this solution as the standard solution. Per- form the test with the test solution and the standard sol- tuion as directed under the Thin-layer Chromatography. Spot 5 μL each of the test solution and the standard so- lution on a plate of silica gel for thin-layer chromato- graphy. Develop the plate with a mixture of acetone, water and ammonia water (90 : 7 : 3) to a distance of about 10 cm and dry the plate at 80 °C for 10 minutes. Spray evenly Dragendorff’s TS for spraying: one spot among the spots from the test solution and a yellowish red spot from the standard solution show the same col- or and the same Rf value.
Purity (1) Stem and crown—Less than 10.0%.
(2) Foreign matter—The amount of foreign matter oth- er than stems and crowns contained in Belladonna Root is not more than 2.0%. Ash Not more than 6.0%.
Acid-insoluble Ash Not more than 4.0%.
Assay Dry the pulverized Belladonna Root at 60 °C for 8 hours, weigh accurately about 0.7 g of pulverized Belladonna Root, place in a sotppered centrifuge tube and moisten with 15 mL of ammonia TS. Add 25 mL of ether, stopper, shake for 15 minutes, centrifuge and take the ether layer. To the residue, repeat this operation twice with 25 mL of ether. Combine all extracts and evaporate the ether layer on a water-bath. Dissolve the residue in 5 mL of mobile phase, add 3.0 mL of the in- ternal standard solution and add mobile phase to make exactly 25 mL. Filter this solution with filter paper (not more than 0.8 m in diameter), discard 2 mL of first filtrate and use the subsequent filtrate as the test solu- tion. Separately, weigh accurately about 25 mg of Atro- pine Sulfate RS, previously determine loss on drying, dissolve in mobile phase to make 25 mL and use this solution as the standard stock solution. Pipet 5.0 mL of the standard stock solution, add 3.0 mL of the internal standard solution, add mobile phase to make exactly 25 mL and use this solution as the standard solution. Per- form the test with l0 μL each of the test solution and the standard solution as directed under the Liquid Chromatography according to the following operating conditions. Determine the peak areas, QT and QS, of hyoscyamine (atropine) for the test solution and the standard solution, respectively.
1016 Monographs, Part II
Amount (mg) of hyoscyamine (C17 H 23 NO3 ) = amount (mg) of Atropine Sulfate RS, calculated on the dried basis × Q T 1
Q× × 0.8551
S 5 Internal standard solution?A solution of brucine in mobile phase (1 in 2500). Operating conditions
Detector: An ultraviolet absorption photometer (wave- length: 210 nm).
Column: A stainless steel column, about 4 mm in inside diameter and about 15 cm in length, packed with octa- decylsilyl silica ge1 (5 μm in particle diameter). Column temperature: A Room temperature.
Mobile phase: Dissolve 6.8 g of potassium dihyrogen- phosphate in 900 mL of water, add 10 mL of triethyla- mine, adjust pH to 3.5 with phosphoric acid and add water to make 1000 mL. Use a mixture of this solution and acetonitrile (9 : 1).
Flow rate: Adjust the flow rate so that the retention time of atropine is about 14 minutes.
Selection of column: When the procedure is run with 10 μL of the standard solution under the above operat- ing conditions, atropine and the internal standard are eluted in this order with a resolution between their peaks being not less than 4.0.
Benzoin
Benzoinum
Benzoin is the resin obtained from Styax benzoin Dryander or Styrax tonkinensis Craib ex Hart. (Styraca- ceae)
Description Benzoin is the resin, grayish brown to dark red-brown block varying in size. The fractured surface exhibits white to pale yellow-red grains in the matrix. Benzoin is hard and tender at ordinary tempera- ture but softened by heat.
Benzoin has characteristic odor and slightly pungent and acrid taste.
Identification (1) Heat a fragment of Benzoin in a test tube: it evolves an irritating vapor and a crystalline sublimate is produced.
(2) Weigh 0.5 g of Benzoin, add 10 mL of ether, take 1 mL of the solution on a porcelain dish and add 2 to 3 drops of sulfuric acid: a deep red-brown to deep red-purple color develops.
Purity Ethanol-insoluble substances—Weigh gently 1 g of Benzoin, boil with 30 mL of ethanol on a water- bath for 15 minutes under a reflux condenser. After cooling, collect the insoluble substances through a tared glass filter (G3) and wash three times with 5 mL vo-
lumes of ethanol. Dry the residue at 105 o C for 4 hours: the residue is not more than 0.3 g. Ash Not more than 2.0%.
Acid-insoluble Ash Not more than 1.0%.
Bitter Cardamon
Alpiniae Oxyphyllae Fructus
Bitter Cardamon is the fruit of Alpinia oxyphylla Mi- quel (Zingiberaceae).
Description Bitter Cardamon is spherical to fusiform fruit, with both ends somewhat pointed; 1 to 2 cm in length, and 7 to 10 mm in width. External surface is brown to dark brown, with numerous longitudinal, knob-like protruding lines. Pericarp is 0.3 to 0.5 mm in thickness. Inside of the Bitter Cardamon is divided ver- tically into three loculi by thin membranes, each locu- lus containing 5 to 8 seeds adhering by aril. Seeds are irregularly polygonal, about 3.5 mm in diameter, brown to dark brown, and texture is hard.
Bitter Cardamon has characteristic odor and slightly bitter taste.
Ash Not more than 10.0%.
Acid-insoluble Ash Not more than 2.5%.
Essential Oil Content Not less than 0.4 mL (50.0 g).
Bupleurum Root
Bupleuri Radix
Buplerum Root is the root of Bupleurum falcatum Linné or its varieties (Umbelliferae). Buplerum Root, when dried, contains not less than 0.3% of saikosapo- nin a (C42H68O13: 780.97).
Description Bupleurum Root is the root, in long cone or column-shape, single or branched, 10 cm to 15 cm in length and 5 mm to 15 mm in diameter. Upper part is thick and lower part thin. Apex has numerous hairy fi- bres from withered leaves. External surface is pale brown to brown with deep wrinkles. Texture is easily broken and the fractured surface is somewhat fibrous. Under a microscope, a transverse section reveals the thickness of cortex reaching 1/3 to 1/2 of the radius, tangentially extended clefts in cortex. Cortex is scat- tered with a good many intercellular schizogenous oil canals 15 μm to 35 μm in diameter. In xylem, vessels are lined radially or step-wise and fiber groups are scat- tered. The pith at the crown reveals the same oil canals,
as in the cortex. Parenchyma cells contain fully starch
grains and oil droplets.
Bupleurum Root has characteristic order and slightly bitter taste.
Identification (1) Weigh 0.5 g of pulverized Bupleu- rum Root, add 10 mL of water and shake vigorously: the lasting fine foam is produced.
(2) Weigh 2.0 g of pulverized Bupleurum Root or Bup- leurum Root RMPM, add 10 mL each of methanol, boil gently under a reflux condenser on a water-bath for 15 minutes, cool, filter and use the filtrate as the test solu- tion and Bupleurum Root RMPM standard solution. Separately, weigh l mg of Saikosaponin a RS and Sai- kosaponin d RS, dissolve each in l mL of methanol and use these solutions as the standard solutions (1) and (2). Perform the test with the test solution, Bupleurum Root RMPM standard solution and the standard solutions (1) and (2) as directed under the Thin-layer Chromatogra- phy. Spot 10 μL each of the test solution, Bupleurum Root RMPM standard solution and the standard solu- tions (1) and (2) on a plate of silica gel for thin-layer chromatography. Develop the plate with a mixture of dichloromethane, methanol and water (30 : 10 : l) to a distance of about 10 cm and air-dry the plate. Spray evenly diluted sulfuric acid TS on the plate and warm at 105 o C for 10 minutes: the spots from the test solu- tion and the spots from Bupleurum Root RMPM stan- dard solution show the color and the same Rf value and 2 spots among these spots from the test solution and the purple spots from the standard solutions (1) and (2) show the color and the same Rf value. Purity (1) Stem and leaf—Less than 10.0%.
(2) Foreign matter—The amount of foreign matter oth- er than sterns and leaves is not more than 1.0%. Ash Not more than 6.5%.
Acid-insoluble Ash Not more than 2.0%.
Assay Weigh accurately about 0.5 g of pulverized Bupleurum Root, add 50 mL of a mixture of ammo- nium hydroxide and methanol (1 in 20), sonicate to ex- tract for 2 hours and filter. To the filtrate, add methanol to make exactly 50 mL. Take 30.0 mL of this solution and evaporate. Add methanol to the residue to make exactly 5 mL and use this solution as the test solution. Separately, weigh accurately about 10 mg of Saikosa- ponin a RS (previously dried in a desiccator of silica gel for 24 hours), add methanol to make exactly 20 mL and use this solution as standard solution. Perform the test with 5 μL each of the test solution and the standard solution as directed under the Liquid Chromatography according to the following operating conditions and de- termine the peak areas, AT and AS, for the test solution and the standard solution, respectively.
KP VIII 1017
Amount (mg) of saikosapon in a (C 42 H 68 O13 ) = amount (mg) of Saikosapon in a RS ×
A T 5
A × S 12
Operating conditions
Detector: An ultraviolet absorption photometer (wave- length: 203 nm).
Column: A stainless steel column, 4 mm to 6 mm in in- side diameter and 15 cm to 25 cm in length, packed with octadecylsilyl silica ge1 for liquid chromatogra- phy (5 μm to l0 μm in particle diameter). Column temperature: A room temperature.
Mobile phase: A mixture of acetonitrile and water (35 : 65).
Flow rate: 0.8 mL/minute.
Capsicum Tincture
Method of preparation Capsicum in medium cutting 100 g Ethanol a sufficient quantity ????????????????????
To make 1000 mL
Prepare as direction under Tinctures, with the above in- gredients.
Description Capsicum Tincture is yellowish red liq- uid and has extreamly pungent taste.
Specific gravity? d20 20
: About 0.82. Identification Proceed as directed in the Identifica-
tion under Capsicum. Spot 20 μL each of the solution and the standard solution.
Alcohol Number Not less than 9.7 (Method 2) Packaging and Storage Preserve in light-resistant, tight containers.
Capsicum, Chilly Pepper
Capsici Fructus
Capsicum is the fruit of Capsicum annuum Linné or its varieties (Solanaceae).
Description Capsicum is elongated conical to fusi- form fruit, often bent, about 3 cm to 10 cm in length and about 0.8 cm in width. External surface of pericarp is lustrous and dark red to dark yellow-red. Interior of pericarp is hollow and usually divided into two loculi, containing numerous pale yellow-red seeds nearly cir- cular and compressed, about 5 mm in diameter. Capsi- cum usually has remains of calyx and peduncle.
Capsicum has characteristic odor and extremely pun-