1008 Monographs, Part II
standard solution of Anemarrhena Rhizome RMPM. Separately, weigh 5 mg of Sarsasapogenin RS, dissolve in 1 mL of toluene and use this solution as the standard solution. Perform the test with the test solution, the standard solution of Anemarrhena Rhizome RMPM and the standard solution as directed under the Thin- layer Chromatography. Spot 10 μL each of the test so- lution, the standard solution of Anemarrhena Rhizome RMPM and the standard solution on a plate of silica gel for thin-layer chromatography. Deve1op the plate with a mixture of toluene and acetone (9 : 1) to a distance of about 10 cm and air-dry the plate. Spray the vanillin sulfuric acid TS to the plate, heat the plate at 105 o C for 10 minutes. The spots from the test solution and the spots from the standard solution of Anemarrhena Rhi- zome RMPM show the same color and the same Rf value. One spots among those spots from the test solu- tion and a reddish purple spot from the standard solu- tion show the same color and the same Rf value.
Purity Foreign matter—The amount of fiber, origi- nating from the dead leaves and other foreign matter is not more than 3.0%. Ash Not more than 7.0%.
Acid-insoluble Ash Not more than 2.5%.
Angelica Dahurica Root
Angelicae Dahuricae Radix
Angelica Dahurica Root is the root of Angelica dahuri- ca Bentham et Hooker f. or Angelica dahurica Ben- tham et Hooker f. var. formosana Shan et Yuan (Um- belliferae).
Description Angelica Dahurica Root is a main root from which many long roots are branched out and near- ly fusiform, 10 cm to 25 cm in length and 15 mm to 25 mm in diameter. External surface is grayish brown to dark brown, with longitudinal wrinkles and with nu- merous scars of rootlets laterally elongated and pro- truded. A few remains of leaf sheath at the crown and ring-nodes closely protruded near the crown. In a transverse section, the outer region is grayish white and the central region is sometimes dark brown. Under a microscope, transverse section reveal vessels and me- dullary rays developed radially from the center, much starch grains, and the clusters of calcium oxalate in pa- renchyma cells.
Angelica Dahurica Root has characteristic odor and slightly bitter taste.
Identification Weigh 0.2 g of pulverized Angelica Dahurica Root, add 5 mL of ethanol, allow to stand for 5 minutes with shaking and filter. Examine the filtrate
under ultraviolet light (main wavelength: 365 nm): a blue to bluish purple fluorescence develops.
Purity (1) Leaf sheath—Not more than 3.0%.
(2) Foreign matter—The amount of foreign matter oth- er than leaf sheath contained in Angelica Dahurica Root dose not exceed than 1.0%. Ash Not more than 7.0%.
Acid-insoluble Ash Not more than 2.0%.
Extract Content Dilute ethanol-soluble extract— Not less than 25.0%.
Angelica Gigas Root
Angelicae Gigantis Radix
Angelica Gigas Root is the root of Angelica gigas Na- kai (Umbelliferae). Angelica Gigas Root contains not less than 6.0% of the sum of nodakenin (C20H24O9: 408.40) and total decursin [decursin (C19H20O5: 328.36) and decursenol angelate (C19H20O5: 328.36)].
Description Angelica Gigas Root is thick and short root with the remains of stems and leaf sheaths. Main root is about 3 cm to 7 cm in length and 2 cm to 5 cm in diameter. Branched root is 15 cm to 20 cm in length. External surface is pale yellowish brown to dark brown with longitudinal wrinkles, main root sometimes has transverse wrinkles. Fractured surface is flat. Xylem and cortex are distinguished clearly by cambium ring, with dark yellow color around the cambium, and white in the remaining part. Under a microscope, the trans- verse section reveals cork consisting of 5 to 6 layers of cells, cells aligned transversely, parenchymas from primary cortex to xylem aligned systematically in rec- tangular shape. The cortex has schizogenous intercellu- lar space, secretary canal with yellowish brown ingre- dient and substitute fiber is sparsely scattered. Scalari- form or spiral vessel is observed. Numerous starch grains are observed in parenchyma cells.
Angelica Gigas Root has characteristic odor, and bitter and sweet taste.
Identification Weigh 1 g of pulverized Angelica Gi- gas Root, add 10 mL of ethanol, boil in the water bath for 10 minutes, cool, filter and use the fitrate as the test solution. Separately, dissolve 1 mg each of Decursin RS and Decursinol RS, dissolve with 1 mL each of ethanol and use these solution as the standard solution (1) and (2). Perform the test with the test solution and the standard solutions as directed under the Thin-layer Chromatography. Spot 5 μL each of the test solution and the standard solutions 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 wave- length: 365 nm: two spots among the spots from the test solution and spots from the standard solution (1) and (2) show the same color and the same Rf value.
Purity (1) Stem and woody root—Angelica Gigas
Root contains less than 5.0 % of stem and woody root. (2) Foreign matter—Angelica Gigas Root contains less than 1.0% of foreign matter other than stems and woo- dy root.
Ash Not more than 6.0%.
Essential Oil Content Not less than 0.1 mL (50.0 g). Assay Weigh accurately about 0.5 g of pulverized Angelica Gigas Root, add 20 mL of methanol , ex- tract under a reflux condensor for 1 hours, and filter. To the residue, add 20 mL of methanol, and proceed in the same manner. Combine all the filtrates, add methanol to make exactly 50 mL and use this solution as the test so- lution. Separately, weigh accurately about 10 mg of Nodakenin RS, dissolve in methanol to make 20 mL, take exactly 5 mL of this solution, dissolve acucurately about 10 mg of Decursin RS, add methanol to make exactly 50 mL, and use this solution as the standard so- lutions. Pipet 10 μL each of the test solution and the standard solutions, and perform the test as directed un- der the Liquid Chromatography according to the fol- lowing operating conditions. Determine the peak areas, ATN, ATD and ATDA, of nodakenin, decursin and decursi- nol angelate (the relative retention time to decursin is about 1.02), respectively, the test solution and ASN and ASD, of nodakenin and decursin, respectively, the stan- dard solution.
Amount (mg) of nodakenin (C 20 H 24 O 9 ) = amount (mg) of Nodakenin RS × A TN A × 1
SN 4
Amount (mg) of total decursin [decursin (C 19 H 20 O 5 ) and decursinol angelate (C 19 H 20 O 5 )]
= amount (mg) of Decursin RS × A TD + A TDA
A SD
Operating conditions
Detector: An ultraviolet absorption photometer (wavelength: 330 nm).
Column: A stainless steel column, 4.6 mm in inside diameter and 25 cm in length, packed with octadecyl- silyl silica gel for liquid chromatography (5 μm in par- ticle diameter).
Column temperature: An ordinary temperature.
Mobile phase: Control gradually or concentration- gradiently with mobile phase A and B as follows.
Mobile phase A – acetonitrile Mobile phase B – water
KP VIII 1009
Time Mobile phase A Mobile phase B
(min)
(%) (%)
0 20 80 3 20 80
8
30
70
18
30
70
19
50
50
40 50 50 41
90
10
50 90 10 Flow rate: 1.0 mL/min System suitability
System performance: When the procedure is run with 10 μL of this solution under the above operating conditions, nodakenin, decursin and decursinol ange- late are eluted in this order, clearly dividing each peak.
System repeatability: When the test is repeated 6 times with 10 μL of the standard solution under the above operating conditions, the relative standard devia- tion of each peak area of nodakenin, decursin and de- cursinol angelate is not more than 1.5%.
Apricot Kernel
Armeniacae Semen
Apricot Kernel is the well ripe seed of Prunus arme- niaca Linné var. ansu Maximowicz, Prunus mandshu- rica Koehne var. glabra Nakai, Prunus sibirica Linnéor Prunus armeniaca Linné (Rosaceae). Apricot Kernel, when dried, contains not less than 3.0% of amygdalin (C 20 H 27 NO 11 : 457.43). Description Apricot Kernel is flattened, somewhat asymmetric ovoid seed, 10 mm to 18 mm in length, 8 mm to 13 mm in width and 4 mm to 7 mm in thickness. Apricot Kernel is sharp at one end and rounded at the other end where chalaza situated. Seed coat is thin, brown and its surface is powdery with rubbing easily detachable stone cells of epidermis. Numerous vascular bundles run from chalaza throughout the seed coat, ap- pearing as thin vertical furrows. Seed coat and thin semi-transparent white albumen easily separate from cotyledon when soaked in boiling water. Cotyledons are two, milky white and oily.
Under a microscope, surface of epidermis reveals stone cells on veins protruded by vascular bundles, forming angular circle to ellipse and approximately uniform in shape, with uniformly thickened walls and 60 μm to 90 μm in diameter. In lateral view, stone cell appears ob- tusely triangular and its wall is extremely thickened at the apex.
Apricot Kernel is almost odorless and has bitter and
1010 Monographs, Part II oily taste.
Identification Weigh 1 g of pulverized Apricot Ker- nel, add 10 mL of methanol, heat for 10 minutes on a water bath with a reflux condenser. Filter after cooling and use this as the test solution. Separately, dissolve 2 mg of Amygdalin RS 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 solution on a plate of silica gel for thin-layer chromatography. Develop the plate with a mixture of ethyl acetate, methanol and wa- ter (7 : 3 : l) to a distance of about 10 cm and air-dry the plate. Spray evenly sulfuric acid TS for spray and heat for 10 minutes at 105 o C : one spot among the spots from the test solution and a brown to dark brown spot from the standard solution show the same color and the same Rf value. Purity (1) Rancidity—Grind Apricot Kernel with hot water: no unpleasant odor of rancid oil is perceptible. (2) Foreign matter—Apricot Kernel does not con- tain fragments of endocarp and other foreign matter. Assay Weigh accurately about 0.5 g of pulverized Apricot Kernel, add 50 mL of methanol, extract with a reflux condenser for 2 hours and filter. Repeat the above procedure with the residue using 50 mL of me- thanol. Combine the whole filtrates and evaporate to dryness under reduced pressure. Add 70 mL of water and 70 mL of hexane to the residue, shake well and discard the hexane layer. Add 70 mL of ether to the wa- ter layer, shake and discard the ether layer. The remain- ing water layer is filtered, adjust the total volume to make exactly 100 mL and use this solution as the test solution. Separately, dry the Amygdalin RS for 24 hours in the desiccator (silica gel) and weigh accurately about 10 mg, dissolve in 100 mL of water and use this solution 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 accord- ing to the following operating conditions and determine the peak areas, AT and AS, of amygdalin for the test so- lution and the standard solution, respectively.
Amount (mg) of amygdalin (C20H27NO11)
= amount (mg) of Amygdalin RS × A TA S
Operating conditions
Detector: An ultraviolet absorption photometer (wavelength: 214 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 gel (5 μm to 10 μm in particle diameter).
Column temperature: A room temperature.
Mobile phase: A mixture of methanol and water
(20 : 80).
Flow rate: 1.0 mL/minute.
Aralia Continentalis Root
Araliae Continentalis Radix
Aralia Continentalis Root is the root of Aralia conti- nentalis Kitakawa (Araliaceae).
Description Aralia Continentalis Root is the root, long cylindrical to rod shaped, 10 cm to 30 cm in length and 5 mm to 20 mm in diameter. External sur- face is grayish-white to grayish-brown, with longitu- dinal wrinkles and sparse rootlet scars. Fractured sur- face is fibrous with pale yellow pith and texture is light and loose.
Under a microscope, transverse section reveals small resin canal with secretary cells in collenchyma. The clear cambium consists of 3 to 5 rows, is clearly. xy- lem fibers is developed around vessles in xylem, me- dullary rays consisting of 3 to 5 rows, are connected from the pith to the phloem.
Aralia Continentalis Root has characteristic odor and tastes unpleasant and slightly bitter.
Identification Weigh 0.5 g of pulverized Aralia Con- tinentalis Root, add 10 mL of chloroform, extract for 1 hr with agitating, stand for 15 minutes and filter. Take 1.0 mL of the filtrate, add 0.5 mL of anhydrous acetic anhydride, vortex and add carefully 0.5 mL of sulfuric acid to make two layers: a red to dark red color devel- ops at the zone of contact and the upper layer produces yellowish-red to dark yellowish red.
Loss on Drying Not more than 12.0%. (6 hours). Ash Not more than 9.0%.
Acid-insoluble Ash Not more than 2.0%.
Arctium Fruit
Arctium Fructus
Arctium Fruit is the fruit of Arctium lappa Linné (Compositae).
Description Arctium Fruit is slightly curved, long ob- ovate achene, 5 to 7 mm in length, 2.0 to 3.2 mm in width, 0.8 to 1.5 mm in thickness. External surface is grayish brown to brown, with black spots. Arctium Fruit is hollow about 1 mm in diameter at one broad end, and is flat, indistinct, longitudinal ridge at the oth- er narrow end. About 100 fruits of Arctium Fruit weigh 1.0 to 1.5 g.
Under a microscope, a transverse section reveals an ex-
ocarp of single-layered epidermal tissue, mesocarp of
slightly sclerified parenchyma containing parenchy- matous cells with a brown substance, endocarp of a single layer of stone cells containing solitary, discrete crystals of calcium oxalate, and seed coat composed of parenchyma several cells thick, and cotyledons with starch grains, oil drops, aleurone grains, and minute crystals of calcium oxalate.
Arctium Fruit has odorless, bitter taste and oily.
Identification Weigh 0.5 g of pulverized Arctium Fruit, add 20 mL of methanol, shake for 10 minutes, filter, and use filtrate as the sample solution. Perform the test with the sample solution as directed under thin-layer chromatography. Spot 5 μL of the sample solution on a plate of silica gel for thin-layer chromatography, devel- op the plate with a mixture of acetone, ethyl acetate and water (15:10:1) to a distance of about 10 cm, and air- dry the plate. Spray evenly diluted sulfuric acid TS on the plate, and heat at 105 o C for 10 minutes: a red
purple spot appears at around Rvalue 0.4.
Loss on Drying Not more than 12.0% (6 hours). Ash Not more than 7.0%.
Acid-insoluble Ash Not more than 1.0%.
Extract Content Dilute ethanol-soluble extract— not less than 15.0 %
Areca
Arecae Semen
Areca is the ripe seed of Areca catechu Linné (Palmae), which is collected, boiled in water and removed from pericarp.
Description Areca is the seed, rounded-conical or flattened nearly spherica1, l5 mm to 35 mm in height and 15 mm to 30 mm in diameter. Hilum is present at the center of its base and usually forms a dent. External surface is grayish reddish brown to grayish yellowish brown, with a network of pale lines and texture is hard. Cross section is dense in texture, exhibiting a marble appearance of grayish brown seed coat alternating with white albumen. The interior of the seed is often hollow. Areca has slightly characteristic odor and astringent and slightly bitter taste.
Identification Weigh 3 g of pulverized Areca in stoppered centrifuge tube, add 30 mL of ether and 5 ml of sodium hydroxide TS, stoppered, shake for 5 mi- nutes, centrifuge and pipet the supernatant. Evaporate ether in water-bath, dissolve the residue in 1.5 mL of
KP VIII 1011
methanol and use this solution as the test solution. Sep- arately, weigh 5 mg of Arecoline Bromide RS, dissolve it in 1 mL of methanol and use this as the standard so- lution. Perform the test with the test solution and the standard solution as directed under the Thin-layer Chromatography. Spot 5 μL each of the test solution and the standard solution on a plate of silica gel for thin-layer chromatography. Develop the plate with a mixture of acetone, water and acetic anhydride (10 : 6 : l) to a distance of about 10 cm and air-dry the plate. Spray evenly iodine TS on the plate: one spot among the spots from the test solution and a reddish brown spot from the standard solution show the same color and the same Rf value.
Purity (1) Pericarp—Areca contains less than 2.0% of pericarp.
(2) Foreign matter—Areca contains less than 1.0% of foreign matter other than the pericarp. Ash Not more than 2.5%.
Areca Peel
Arecae Pericarpium
Acera Peel is the pericarp of Areca catechu Linné (Palmae), from which the fruit is unripe after boiled. The pericarp from unripe fruit is known as Daebokpi, and the one from the ripe fruit is known as Daebokmo. Description (1) Daebokpi – Areca Peel is the peri- carp, usually elliptical or long ovoid gourd-shaped, 4 cm to 7 cm in length, 20 cm to 35 cm in width and 2 mm to 5 mm in thickness. Epicarp is deep brown to black, with irregular longitudinal wrinkles, raised transverse lines on the surfaces, stalk scars at apex, re- mains of fruit stalk and calyx at the base. Endocarp is dented, brown to deep brown, lustrous, smooth and hard shell-shaped. Texture is light and hard and meso- carp fibers visible torn longitudinally.
Areca Peel has slight characteristic odor and slightly astringent taste.
(2) Daebokmo – Areca Peel is the pericarp, usually el- liptical or gourd-shaped. Epicarp is mostly lost or re- mained. Mesocarp is fibrous, yellowish white or pale brown, sparce and soft. Endocarp is hard shell-shaped, yellowish brown to deep brown. Inner surface is lustr- ous, smooth, and sometimes broken in longitudinal.
Areca Peel has slight characteristic odor and weak taste. Identification Weigh 0.5 g of pulverized Areca Peel, add 5 mL of water, shake for 2 minutes to 3 minutes and filter. To 2 mL of the filtrate, add 1 mL of lead sub- acetate TS: the filtrate turns pale yellow with turbidity and yellow precipitation are slowly occurred. Purity
Foreign matter—Areca Peel contains less
1012 Monographs, Part II
than 10.0% of Areca and foreign matters.
Loss on Drying Not more than 12.0% (6 hours). Ash Not more than 7.0%.
Extract Content Dilute ethanol-soluble extract— Not less than 5.0%.
Arisaema Rhizome
Arisaematis Rhizoma
Arisaema Rhizome is the tuber of Arisaema amurense Maximowicz, Arisaema erubescens Schott or Arisaema heterophyllum Blume (Araceae), from which the cork layer has been removed.
Description Arisaema Rhizome is irregular oblate rhizome, 15 mm to 65 mm in diameter and 1 cm to 2 cm in height. External surface is pale yellowish brown to pale brown and slightly smooth. The top is with dented stem scars and the bottom is crumpled, encir- cled with numerous pitted fibrous root scars. Some tu- bers are surrounded by small oblate lateral buds. Tex- ture is hard and uneasily broken. A fractured surface is milky white and starchy.
Under a microscope, the transverse section shows pa- renchymatous cells filled with starch grains and muci- lage cells filled with mucilage duct and fine needles of calcium oxalate.
Arisaema Rhizome has slight pungent odor and taste. Identification (1) Weigh 0.5 g of pulverized Arisae- ma Rhizome, add 10 mL of water, macerate and shake vigorously: a lasting fine foam is produced.
(2) Weigh 0.2 g of pulverized Arisaema Rhizome, add 2 mL of acetic anhydride, warm for 2 minutes on a water-bath, filter and add carefully 0.5 mL of sulfuric acid to the filtrate: a pale brown color develops at the zone of contact.
(3) On a section of Arisaema Rhizome, add dilute iodine TS drop-wise: a dark bluish purple color is pro- duced on the surface.
Loss on Drying Not more than 15.0% (6 hours). Ash Not more than 5.0%.
Acid-insoluble Ash Not more than 1.0%.
Asiasarum Root and Rhizome
Asiasari Radix et Rhizoma
Asiasarum Root and Rhizome is the root and rhizome of Asiasarum heteropoides F. Maekawa var. mandshu-
ricum F. Maekawa or Asiasarum sieboldi Miquel var.
seoulense Nakai (Aristolochiaceae).
Description Asiasarum Root and Rhizome is the root and rhizome, like irregularly curved string in shape. The rhizome is 2 cm to 4 cm in length and 2 mm to 3 mm in diameter with yellowish brown nodes and nu- merous root about 15 cm in length and about 1 mm in diameter. External surface is pale brown to dark brown with extremely thin longitudinal wrinkles on the sur- face. The upper end of rhizome is sometimes with peti- oles, peduncles or buds. Each node has several scars of petiole and peduncle, and internode has several thin and long roots.The texture is easy to be broken and the fractured surface is yellowish white and not flat. Under a microscope, transverse section reveals parenchyma cells and oil drops in endoderm.
Asiasarum Root and Rhizome has characteristic odor and pungent taste with a slight numbness on the tongue. Purity (1) Terrestrial part—Asiasarum Root and Rhizome contains less than 10.0% of its terrestrial part such as leaves and petioles.
(2) Foreign matter— Asiasarum Root and Rhizome contains less than 1.0% of foreign matter other than ter- restrial part.
Ash Not more than 10.0%.
Acid-insoluble Ash Not more than 3.0%.
Essential Oil Content Not less than 0.6 mL (30.0 g).
Asparagus Tuber
Asparagi Tuber
Asparagus Tuber is the tuber of Asparagus cochinchi- nensis Merill (Liliaceae). The cork layer has been re- moved and dried after boiling or steaming by hot water. Description Asparagus Tuber is a fusiform to globu- lar tuber, somewhat curved, 5 cm to 15 cm in length and 5 mm to 20 mm in diameter. External surface is pale yellowish white to pale brown, semi-translucent, sometimes with longitudinal wrinkles. The texture is mostly soft or hard, easy to be fractured, the fractured surface is grayish yellow, sleek and horny.
Under a microscope, the transverse section shows stone cells or clusters of stone cells are scattered outside of cortex. Mucilage cells filled with fine needles of cal- cium oxalate are observed in the parenchymatous cells of cortex and the central cylinder. Starch grains don’t exist.
Asparagus Tuber has a slight characteristic odor and tastes sweet followed by bitter taste.
Identification 1) Weigh 0.5 g of pulverized Aspara- gus Tuber, add 10 mL of water, warm for 2 to 3 minutes