1018 Monographs, Part II gent taste.
Identification Weigh 2.0 g of pulverized Capsicum, add 5 mL of ethanol, warm on a water-bath for 5 mi- nutes, cool, centrifuge and use the supernatant liquid as the test solution. Separately, dissolve l mg of Capsaicin RS in l mL of ethanol and use this solution as the stan- dard solution. Perform the test with the test solution and the standard solution as directed under the Thin- layer Chromatography. Spot 10 μL each of the test so- lution and the standard solution on a plate of silica gel for thin-layer chromatography. Develop the plate with a mixture of ether and methano1 (19 : 1) to a distance of about 12 cm and air-dry the plate. Spray evenly 2,6- dibromo-N-chloro-1,4-benzoquinonemonoimine TS on the plate and allow to stand in ammonia gas: a spot from the test solution and a blue spot from the standard solution show the same color and the same Rf value. Purity Foreign matter—Less than 1.0%. Ash Not more than 6.0%.
Acid-insoluble Ash Not more than 1.2%. Extract Content Ether-soluble extract—Not less
than 9.0%.
Cardamon
Cardamomi Fructus
Cardamon is the ripe fruit of Elettaria cardamomum Maton (Zingiberaceae). The capsules are removed from the seeds before use.
Description Cardamon is the fruit, long ellipsoidal, 10 mm to 20 mm in length and 5 mm to 10 mm in di- ameter, with three blunt ridges and many longitudinal lines. At one end, 1 mm to 2 mm of small protrusion is present. External surface is pale yellow. Pericarp is thin, light and fibrous. Interior is longitudinally divided into three loculi by thin membranes, each loculus containing 3 to 7 seeds joining by aril. Seed is ovoid to long ovoid or irregularly angular, 3 mm to 4 mm in length, dark brown to blackish brown. The dorsal side is convex, the ventral side is longitudinally grooved and coarsely tu- berculated.
Cardamon has characteristic odor and tastes pungent and slightly bitter. Pericarp is odorless and tasteless. Ash Not more than 6.0% (seed).
Acid-insoluble Ash Not more than 4.0% (seed). Essential Oil Content Not less than 1.0 mL (30.0 g, seed).
Packaging and Storage Preserve in tight containers.
Cassia Seed
Cassiae Semen
Cassia Seed is the ripe seed of Cassia tora Linné or Cassia obtusifolia Linné (Leguminosae). Description (1) Cassia tora - Cassia Seed from Cas- sia tora is short cylindrical seed, 3 mm to 6 mm in length and 2 mm to 4 mm in diameter. Cassia Seed has a acuminate shape at one end and flat at the other. On both sides, yellow-brown longitudinal lines or bands are present. The texture is hard and a transverse section is round or obtuse polygona1. Under a magnifying glass, an albumen reveals a bent, dark-colored cotyle- don.
Cassia Seed has characteristic odor and taste.
(2) Cassia obtusifolia - Cassia Seed from Cassia obtu- sifolia is rectangular or short cylindrical seed. Both end slopes, 3 mm to 7 mm in length and 2 mm to 4 mm in width. External surface is greenish brown or dark brown, flat, slippery, and lustrous, One end is relatively flat and the other is oblique and acuminate. A ridgeline is prominent at the back and belly, symmetrically slip- pery in both sides, fanwisely dented. The texture is tough, hard and difficult to break. The seed coat is thin, and two yellow cotyledons are curved as S shape or overlapped.
Cassia Seed has slightly characteristic odor and a little bitter taste.
Identification Weigh 0.1 g of pulverized Cassia Seed, previously dried in a desiccator (silica gel) for 48 hours, on a slide glass, put a glass ring, 10 mm in both internal diameter and height on it, then cover with moistened filter paper and heat gently the slide glass over a small flame. Take the filter paper when a yellow color has developed on the upper surface of it and place l drop of potassium hydroxide TS on the surface of the filter pa- per where a sublimate is present: a red color develops. Purity Foreign matter—Less than 1.0%. Ash Not more than 5.0%.
Cattle Gallstone
Bovis Calculus
Cattle Gallstone is a stone formed in the gall sac of Bos taurus Linné var. domesticus Gmelin (Bovidae). Cattle Gallstone contains not less than 20.0% of conjugated bilirubin (C33H36N4O6: 584.66).
KP VIII 1019
Description Cattle Gallstone is spherical or massive
stone, 1 cm to 4 cm in diameter, and yellow-brown to red-brown. Texture is light, fragile and brittle. Frac- tured surface shows yellow-brown to red-brown annu- lar rings, often containing white granular substances or thin layers in these annular rings.
Cattle Gallstone has slight odor and slightly bitter, fol- lowed by slight sweetness taste.
Identification (1) Weigh 0.1 g of pulverized Cattle Gallstone, add 10 mL of petroleum ether, shake for 30 minutes, filter and wash the residue with 10 mL of pe- troleum ether. Shake 10 mg of the residue with 3 mL of acetic anhydride for 1 to 2 minutes, add a mixture of 0.5 mL of acetic anhydride and 2 drops of sulfuric acid and shake: a yellow-red to deep red color develops and changes through dark red-purple to dark red-brown.
(2) Weigh 10 mg of Cattle Gallstone, add 10 mL of chloroform, shake well and discard extracted chloro- form. Shake well the residue with 1 mL of hydroch- loric acid and 10 mL of chloroform, separate the chlo- roform layer when it acquires a yellow-brown color and shake with 5 mL of barium hydroxide TS: a yellow- brown precipitate is produced.
Purity (1) Curcuma Root, Curcuma Longa Rhizome —Weigh 0.1 g of pulverized Cattle Gallstone, add 50 mL of methanol and heat for 30 minutes in a water-bath Amount (mg) of total bilirubin or free bilirubin with reflux condensor. Filter after cooling, concentrate
A by evaporating the filtrate to 1 mL and use this as the = amount (mg) of Bilirubin RS × T × 2 AS
test solution. Seperately weigh 1 mg of Curcumin RS, disslve in methanol to make 5 mL and use this as the
standard solution. Perform the test with the test solution Amount (mg) of conjugated bilirubin (C33H36N4O6) and the standard solution as directed under the Thin-
layer Chromatography. Spot 10 μL each of the test so- = amount (mg) of total bilirubin - amount (mg) of free lution and the standard solution on a plate of silica gel bilirubin with fluorescent indicator for thin-layer chromatogra- phy. Develop the plate with a mixture of chloroform, ethyl acetate, anhydrous acetic acid and water (100 : Operating conditions 30 : 2 : 3) to a distance of about 10 cm and air-dry the Detector: A visible absorption photometer (wave- plate. Examine under ultraviolet light (main wave- length: 436 nm). length: 365 nm): the spot from the test solution dose Column: A stainless steel column, about 4 mm to 6 not show a yellowish fluorescent spot at the same Rf mm in inside diameter and 15 cm to 30 cm in length,
packed with octadecylsilyl silica gel for liquid chroma- value of the standard solution.
tography (5 μm to 10 μm in particle diameter). (2) Synthesized pigments—Weigh 2 mg of pulve-
Column temperature: A constant temperature of rized Cattle Gallstone and add 1 mL of dilute hydroch-
loric acid: the solution does not show purple color. about 25 o C .
(3) Starch— Weigh 5 mg of pulverized Cattle Gall- Mobile phase: A mixture of methanol, water and stone, add 2 mL of water, heat for 5 minutes in a water- acetic acid (900 : 98 : 2). bath. After cooling, add 2 to 3 drops of iodine TS: the Flow rate: Adjust the flow rate so that the retention solution does not show bluish purple color. time of bilirubin is about 10 minutes. (4) Sucrose— Weigh 20 mg of pulverized Cattle Gallstone, add 2 mL of water, shake for 15 minutes and filter. To 1 mL of the filtrate, add 2 mL of anthrone TS and shake: the solution does not show deep bluish green to dark green color.
Polyporus
Ash Not more than 10.0%.
Chuling is the sclerotium of Polyporus umbellatus Fries (Polyporaceae). Assay Proceed under the dark place as fast as possi-
ble. Weigh accurately about 0.1 g of the fine powder of Cattle Gallstone to a Erlenmeyer flask, add 10 mL of diluted hydrochloric acid (1 in 5) and 200 mL of chlo- roform, mix well, heat for 1.5 hours in a water-bath at 61 ± 2 o C and allow to stand. Transfer the chloroform extract into a separatory funnel. The flask is washed with a small volume of chloroform and place the chlo- roform layer into the separatory funnel. Allow to stand for 10 minutes and take the chloroform layer. The re- maining water layer is back extracted with chloroform. Combine all of the chloroform layer, add 5 g of an- hydrous sodium sulfate, mix well and filter. Add chlo- roform to the filtrate to make 200 mL and use this solu- tion as test solution for total bilirubin. Separately, weigh accurately about 0.1 g of pulverized Cattle Gall- stone, dissolve in 200 mL of chloroform, filter and use this filtrate as test solution for free bilirubin. Separately, Weigh accurately about 20 mg of Bilirubin RS, dis- solve in chloroform to make 100 mL, use this solution as standard solution. Pipet 5 μL each of the test solu- tion and the standard solution and perform the test as directed under the Liquid Chromatography according to the following operating conditions. Determine the peak areas, AT and AS, of bilirubin for the test solution and the standard solution, respectively.
Chuling
1020 Monographs, Part II
Description Chuling is the sclerotium, and irregular- ly shaped mass, usually 5 cm to 10 cm in length. Exter- nal surface is grayish brown to blackish brown, with numerous dents and coarse wrinkles. Chuling is break- able. Fractured surface is cork-like and almost white to pale brown and a white speckled pattern on the inner region. Texture is light.
Chuling is odorless and tasteless.
Identification Weigh 0.5 g of pulverized Chuling, add 5 mL of acetone and heat on a water-bath for 2 minutes, filter and evaporate the filtrate to dryness. Dissolve the residue in 5 drops of acetic anhydride and add 1 drop of sulfuric acid: a red-purple color develops and imme- diately changes to dark green. Ash Not more than 16.0%.
Acid-insoluble Ash Not more than 4.0%.
Cibot Rhizome
Cibotii Rhizoma
Cibot Rhizome is the rhizome of Cibotium barometz J. Smith (Dicksoniaceae).
Description Cibot Rhizome is the rhizome, irregular- ly long mass-shaped, 10 cm to 30 cm in length and 2 cm to 10 cm in diameter. External surface is deep brown, with remains of golden hairs. The upper part is exhibiting several reddish brown woody petioles and the lower part is showing remains of black fibrous roots. Texture is hard and uneasily broken.
Cibot Rhizome is odorless and the taste is weak and slightly astringent.
Identification 1) Weigh 1 g of pulverized Cibot Rhi- zome, add 10 mL of methanol, boil in the water bath for 15 minutes and filter. Drop the filtrate on the filter paper and examine under a ultraviolet light (365 nm): fluorescence of bluish white color develp.
2) Weigh 1 g of pulverized Cibot Rhizome, add 10 mL of water, boil in the water bath for 15 minutes and filter. Drop the 1% ferric chloride solution to 2 mL of the fil- trate:: the filtrate turn to dark green. Loss on Drying Not more than 11.0% . Ash Not more than 2.5%.
Extract Content Dilute ethanol-soluble extract— Not less than 22.0%.
Cimicifuga Rhizome
Cimicifugae Rhizoma
Cimicifuga Rhizome is the rhizome of Cimicifuga he- racleifolia Komarov, Cimicifuga simplex Wormskjord, Cimicifuga dahurica Maximowicz or Cimicifuge foeti- da Linné (Ranunculaceae). Description Cimicifuga Rhizome is the rhizome, knotted, irregularly shaped, 6 cm to 18 cm in length and 10 mm to 25 mm in diameter. External surface is dark brown to grayish black, with many remains of roots, sometimes with scars of terrestrial stems. The center of the scar is dented and the circumference of the scar is pale and shows a radial pattern. Texture is light and hard and the fractured surface is fibrous. Pith is dark brown and often hollow.
Cimicifuga Rhizome is odorless and has bitter and slightly astringent taste.
Purity Rhizome of Astilbe species—Under a micro- scope, powdered Cimicifuga Rhizome does not contain crystal druses in the parenchyma. Ash Not more than 9.0%.
Acid-insoluble Ash Not more than 1.5%.
Extract Content Dilute ethanol-soluble extract— Not less than 18.0%.
Cinnamon Bark
Cinnamomi Cortex
Cinnamon Bark is the bark of the trunk of Cinnamo- mum cassia Presl or other species of the same genus (Lauraceae), or such bark from which a part of the pe- riderm has been removed. Cinnamon Bark contains not less than 0.03% of cinnamic acid (C9H8O2: 148.16), calculated on the dried basis.
Description Cinnamon Bark is usually semi-tubular or tubularly rolled pieces of bark, 5 cm to 50 cm in length and 15 cm to 50 cm in diameter, 1 mm to 5 mm in thickness. External surface is dark red-brown and the inner surface is red-brown and smooth. Cinnamon Bark is brittle and the fractured surface is slightly fibrous, red-brown, exhibiting a pale brown, thin layer. Under a microscope, a transverse section reveals a primary cor- tex and a secondary cortex divided by an almost conti- nuous ring consisting of stone cells. Nearly round bun- dles of fibers are in the outer region of the ring and wall of each stone cell is often thickened in a U-shape. Sec- ondary cortex of Cinnamon Bark lacks stone cells and
is with a small number of sclerenchymatous fibers
coarsely scattered. Parenchyma tissue is scattered with oil cells, mucilage cells and cells containing fine needles of calcium oxalate and parenchyma cell con- tains starch grains.
Cinnamon Bark has characteristic aroma, sweet and pungent taste at first, later rather mucilaginous and slightly astringent.
Identification Weigh 2 g of pulverized Cinnamon Bark, add 10 mL of ether, shake for 3 minutes, filter and use the filtrate as the test solution. Separatlely weigh 1 mg each of Cinnamic Acid RS and 1 mg of Cinnamaldehyde RS, add 1 mL of methanol, respec- tively, and use each of these solutions as the standard solution (1) and the standard solution (2). 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 with fluorescent indicator for thin- layer chromatography. Develop the plate with a mixture of hexane and ethyl acetate (2 : 1) to a distance of about 10 cm and air-dry the plate. Examine under ultraviolet light (main wavelength: 254 nm): the two spots among several spots of the test solution and the spots of the standard solution (1) and the standard solution (2) show the same color and the same Rf value.
Loss on Drying Not more than 15.5% (6 hours). Ash Not more than 5.0%.
Assay Weigh accurately about 2 g of pulverized Cin- namon Bark in a Soxhlet extractor, add 60 mL of ether, extract for 2 hours and the extract is put into a separato- ry funnel. To the residue, add 60 mL of ether and pro- ceed in the same manner. Combine all the extracts, wash with water and dehydrated with anhydrous so- dium sulfate. The ether is evaporated in vacuum. To the residue, add methanol to make exactly 10 mL and use this solution as the test solution. Separately, weigh ac- curately about 10 mg of Cinnamic Acid RS, previously dried more than 12 hours in the desiccator, add metha- nol to make exactly 100 mL and use this solution as the standard solution. Perform the test with 10 μL each of the test solution and the standard solution as directed under the Liquid Chromatography according to the fol- lowing operating conditions. Determine the peak areas, AT and AS, of cinnamic acid of the test solution and the standard solution, respectively.
Amount (mg) of cinnamic acid (C9H8O2) = amount (mg) of Cinnamic Acid RS × A T 1 A× S 10
Operating conditions
Detector: An ultraviolet absorption photometer (wavelength: 280 nm).
Column: A stainlees steel column, 4 mm to 6 mm in inside diameter and 15 cm to 25 cm in length, packed
KP VIII 1021
with octadecylsilyl silica gel for liquid chromatography (5 μm to 10 μm in particle diameter).
Column temperature: A ordinary temperature.
Mobile phase: A mixture of methanol, water and anhydrous acetic acid (12 : 88 : 1).
Flow rate: 2.0 mL/minute.
Citrii Unshiu Immature Peel
Citri Unshius Pericarpium Immaturus
Citrii Unshiu Immature Peel is the unripe pericarp of Citrus unshiu Markovich or Citrus reticulata Blanco (Rutaceae).
Description Citrii Unshiu Immature Peel is the globu- lar pericarp, 5 mm to 20 mm in diameter. External sur- face is grayish green to bluish green, rough and wrin- kled, with sharp pedurcle scars in apex, with globular fruit stalk scars. Under a microscope, a transverse sec- tion reveals secretive parenchymatous cells are lined, yellowish white to pale yellowish brown, 15 mm to 40 mm in thickness.
Citrii Unshiu Immature Peel has characteristic odor, bitter and slightly pungent tastes.
Identification 1) Weigh 0.3 g of pulverized Citrii Unshiu Immature Peel, add 10 mL of methanol, extract for 20 minutes under a reflux condenser and filter. Add small amount of magnesium powder to 1 ml of the fil- trate and add 3 to 5 droplets of hydrochloric acid: a scarlet color slowly appears.
2) Evaporate 5 mL of the filtrate of 1) to about 1 mL, use this solution as the test solution. Separately, use the saturated solution of Hesperidin RS in methanol as the standard solution. Perform the test with the test solution and the standard solution as directed under Thin-layer Chromatography. Spot 5 μL each of the test solution and the standard solution on a plate of silica gel with fluorescent indicator for thin-layer chromatography. Develop the plate with a mixture of toluene, ethyl ace- tate, formic acid and water (20 : 10 : 1 : 1) to a distance of about 10 cm and air-dry the plate. Repeatedly, de- velop the plate with a upper layer of a mixture of tolu- ene, ethyl acetate, formic acid and water (20 : 10 : 1 :
1) to a distance of about 8 cm and air-dry the plate. Spray 5% solution of the aluminium chloride TS to a plate and examine under ultraviolet light (main wave- length: 365 nm): a fluorescent spot among the several spots dard solution form the show test solution the same and color a spot and from the some the stan- R f value.
Loss on Drying Not more than 12.0% Ash Not more than 5.0%
1022 Monographs, Part II
Acid-insoluble Ash Not more than 1.0%
Essential Oil Content Not less than 0.2 mL (50 g) Extract Content Dilute ethanol-soluble extract— Not less than 12.0%
Citrus Unshiu Peel
Citrus Unshiius Pericarpium
Citrus Unshiu Peel is the ripe pericarp of Citrus unshiu Markovich or Citrus reticulate Blanco (Rutaceae). Ci- trus Unshiu Peel contains not less than 4.0% of hespe- ridin (C28H34O15: 610.56), calculated on the dried basis. Description Citrus Unshiu Peel is irregular, plate- shaped pieces of pericarp, about 2 mm in thickness. Ex- ternal surface is yellow-red to dark yellow-red to dark yellow-brown, with numerous small dents associated with oil sacs. Interior is white to pale grayish yellow- brown. Texture is light and brittle.
Citrus Unshiu Peel has characteristic aroma odor and bitter and slightly pungent taste.
Identification 1) Weigh 0.5 g of pulverized Citrus Unshiu Peel, add 10 mL of methanol, warm on a water- bath for 2 minutes and filter. To 5 mL of the filtrate, add 0.1 g of magnesium and 1 mL of hydrochloric acid and allow to stand: a red-purple color develops.
2) Weigh 0.5 g of pulverized Citrus Unshiu Peel., add 10 mL of methanol, sonicate for 20 minutes and filter. Use the filterate as the test solution. Separately, weigh 1 mg of Hesperidin RS, dissolve in 1 mL of methanol and use this solution as the standard solution. Perform the test with the test solution and the standard solution as directed under the Thin-layer Chromatography. Spot 10 μL each of the test solution and the standard solu- tion on a plate of silica gel with a fluorescent indicator
for thin-layer chromatography. Deve1op the plate with a mixture of ethyl acetate, methanol and water (100 : 17.5 : 3) to a distance of about 10 cm and air-dry the plate. Spray the aluminium chloride TS to the plate and examine under ultraviolet light (main wavelength: 365 nm): One spot among several spots from the test solu- tion and the bluish white spot from the standard solu- tion of the standard solution show the same color and the same Rvalue.
Loss on Drying Not more than 13.0% (6 hours). Ash Not more than 4.0%.
Assay Weigh accurately about 0.5 g of pulverized Ci- trus Unshiu Peel, add 60 mL of methanol, extract under a reflux condenser for 2 hours and filter. To the residue, add 30 mL of methanol and proceed in same manner.
Combine all filtrates, add methanol to make exactly 100 mL and use this solution as the test solution. Weigh accurately about 20 mg of Hesperidin RS, dis- solve in methanol to make 100 mL and use this solu- tion as the standard solution. Perform 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, AT and AS, of hesperidin for the test solution and the standard solution, respectively. Amount (mg) of hesperidin (C28H34O15) = amount (mg) of Hesperidin RS × A TA S
Operating conditions
Detector: An ultraviolet absorption photometer (wavelength: 280 nm).
Column: A stainless steel column, 4 mm to 6 mm in inside diameter and 15 cm to 25 cm in length, packed with octadecylsilyl silica ge1 (5 μm to l0 μm in particle diameter).
Column temperature: A ordinary temperature.
Mobile phase: A mixture of methanol and water (40 : 60).
Flow rate: 1.0 mL/minute.
Clove
Syzygii Flos
Clove is the flowering bud of Syzygium aromaticum Merrill et Perry (Myrtaceae).
Description Clove is paddle-shaped, dark brown to dark red buds, 10 mm to 18 mm in length, consists of slightly compressed and four-sided receptacle, crowned by 4 thick sepals and 4 nearly spherical, membranous, imbricated petals, enclosing numerous stamens and a single style.
Under a microscope, a transverse section reveals irre- gular, long ovoid oil sacs in the outer surrounding sur- face, two layered vascular bundles surrounded by col- lenchyma in the inner surface, bast fiber in phloem, and spongy tissue in vascular bundles. Parenchyma cell sur- rounded by vascular bundles contains aggregate crys- tals of calcium oxalates and oil droplets of essential oil. Clove has strong, characteristic odor and pungent taste, followed by a slight numbness of the tongue.
Identification Take 0.1 mL of the mixture of xylene and essential oi1, obtained in the Essential oil content, add 2 mL of ethanol and add l to 2 drops of ferric chlo- ride TS: a green to blue color develops.
Purity (1) Stem—Less than 5.0%.
(2) Foreign matter—The amount of foreign matter other than the stem is not more than 1.0%.