28
451 Appendix Basic Solvent Systems, reagents and columns for the TLC-, GC- and HPLC-¿ngerprint Analysis of main structure types of natural products Alkaloids 1. Amides 2. Phenolics 3. Flavones a) Procyanidines b) Cumarins c) Anthraquinones d) Essential oils 4. Lignans 5. Triterpene-/Steroidsaponins 6. Other Terpenoids (Diterpenoids) 7. Phenolcarboxylic acids 8. 1. Alkaloids (see Monographs No. 2, 28, 29, 32, 34, 36, 45, 50, 56, 62, 79) TLC-Analysis HPLC-Analysis Ammonia solution 10%; MeOH-Extraction Ammonia solution 10%; MeOH-Extraction Silica gel/HPTLC Silica gel RP-select B column (C-8) Chloroform-Methanol-Water (6 + 3 + 0.65) A: 2 g Hexanesulfonic acid (pH 3) B: Acetonitrile Iodine reagent, VIS 210 nm TLC-Analysis HPLC-Analysis MeOH-Extraction MeOH-Extraction HPTLC Silica gel RP-select B column (C-8) Ethyl acetate-Methyl ethyl ketone-Formic acid-Water (5 + 3 + 1 + 1) A: 0.68 g KH 2 PO 4 /1 l, pH = 9 (KOH) B: Acetonitrile UV 366 nm, Dragendorff reagent, VIS 270 nm

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451

Appendix

Basic Solvent Systems, reagents and columns for the TLC-, GC- and HPLC- ngerprint Analysis

of main structure types of natural productsAlkaloids1. Amides2. Phenolics 3.

Flavones a) Procyanidinesb) Cumarinsc) Anthraquinonesd)

Essential oils4. Lignans5. Triterpene-/Steroidsaponins6. Other Terpenoids (Diterpenoids)7. Phenolcarboxylic acids8.

1. Alkaloids (see Monographs No. 2, 28, 29, 32, 34, 36, 45, 50, 56, 62, 79)

TLC-Analysis HPLC-Analysis

Ammonia solution 10%; MeOH-Extraction Ammonia solution 10%; MeOH-Extraction

Silica gel/HPTLC Silica gel RP-select B column (C-8)

Chloroform-Methanol-Water(6 + 3 + 0.65)

A: 2 g Hexanesulfonic acid (pH 3)B: Acetonitrile

Iodine reagent, VIS 210 nm

TLC-Analysis HPLC-Analysis

MeOH-Extraction MeOH-Extraction

HPTLC Silica gel RP-select B column (C-8)

Ethyl acetate-Methyl ethyl ketone-Formic acid-Water (5 + 3 + 1 + 1)

A: 0.68 g KH2PO4/1 l, pH = 9 (KOH)B: Acetonitrile

UV 366 nm, Dragendorff reagent, VIS 270 nm

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Appendix

452

2. Amides(see Monograph No. 61)

TLC-Analysis HPLC-Analysis

n-hexane-Extraction n-hexane-Extraction

Silica gel RP-18 column

n-Hexane-Ethyl acetate (5 + 3)

A: WaterB: Acetonitrile

UV 254 nmAnisaldehyde sulphuric acid reagent, VIS

254 nm

3a. Flavones (see Monographs No. 20, 27, 43, 48, 51, 55, 59, 62, 63, 67)

TLC-Analysis HPLC-Analysis

MeOH-Extraction MeOH-Extraction

Silica gel/HPTLC Silica gel RP-18 column

Ethyl acetate-Formic acid-Glacial acetic acid-Water (10 + 1.1 + 1.1 + 2.6)

A: 0.001% Phosphoric acidB: Acetonitrile

NP/PEG, UV 366 nm 210/270 nm

3b. Procyanidines(see Monographs No. 77, 80)

TLC-Analysis HPLC-Analysis

Acetone/Water (1:1)-Extraction; Diethylether Acetone/Water (1:1)-Extraction; Diethylether

Silica gel/HPTLC Silica gel RP-18 column

Ethyl acetate-Methanol-Water (10 + 2 + 1)

A: 0.001% Phosphoric acidB: Acetonitrile

Anisaldehyde sulphuric acid reagent, VIS 210/270 nm

3c. Cumarines(see Monographs No. 13, 38, 45, 46, 78)

TLC-Analysis HPLC-Analysis

50% MeOH/Butanol-Extraction 50% MeOH/Butanol-Extraction

Silica gel/HPTLC Silica gel RP-18 column

Toluene-Ethyl acetate-Acetic acid(90 + 10 + 1)

A: 0.001% Phosphoric acidB: Acetonitrile

NP/PEG, UV 366 nm 210/280 nm

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453

Appendix

3d. Anthraquinones(see Monographs No. 40, 71,76)

TLC-Analysis HPLC-Analysis

MeOH-Extraction MeOH-Extraction

HPTLC Silica gel RP-18 column

Light petroleum-Ethyl acetate-Formic acid (75+25+1) for aglycones and glycosidesEthyl acetate-MeOH-Water (100+13.5+10)

A: 0.05% Phosphoric acid B: Acetonitrile

NP/PEG, UV 366 nmPhosphomolybdic acid, VIS

254/280 nm

4. Essential oils(see Monographs No. 31, 36, 46, 52, 60, 65, 80)

TLC-Analysis GC-Analysis

Distillation or n-Hexane-Extraction Distillation (dil. 1:100 oil/tertButylmethylether)

Silica gel Varian VF-5 ms with 10 m precolumn (deactivated methyl-polysiloxan)

Toluene-Ethyl acetate (93 + 7) Helium

Vanillin sulphuric acid reagent, VIS 270 °C

5. Lignans(see Monographs No. 4, 7, 17, 35, 38, 60, 69)

TLC-Analysis HPLC-Analysis

MeOH-Extraction MeOH-Extraction

Silica gel/HPTLC Silica gel RP-18 column

Toluene-Ethyl acetate-Formic acid (80 + 15 + 10)

A: 0.001% Phosphoric acidB: Acetonitrile

Anisaldehyde sulphuric acid reagent, VIS 210 nm

TLC-Analysis

50% MeOH/Butanol-Extraction

Silica gel/HPTLC Silica gel

Chloroform-MeOH (9+1)

Vanillin phosphoric/sulphuric acid reagent, VIS

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Appendix

454

6. Triterpene-/Steroidsaponins(see Monographs No. 1, 20, 30, 33, 37, 51, 53, 57, 67, 68, 70)

TLC-Analysis HPLC-Analysis

MeOH/Water/Butanol-Extraction MeOH-Extraction

Silica gel/HPTLC Silica gel RP-18 column

Chloroform-MeOH-Water, lower layer A: WaterB: Acetonitrile

Vanillin phosphoric/sulphuric acid reagent or Anisaldehyde sulphuric acid reagent, VIS

210 nm

7. Other Terpenoids (Diterpenoids)(see Monographs No. 25, 41, 49, 54, 59, 64, 73, 74, 75)

TLC-Analysis HPLC-Analysis

MeOH/Ethyl acetate/Water-Extraction MeOH/Ethyl acetate/Water-Extraction

Silica gel/HPTLC Silica gel RP-18 column

Ethyl formate-Toluene-Formic acid (50 + 50 + 15)

A: 0.001% Phosphoric acidB: Acetonitrile

Anisaldehyde sulphuric acid reagent, VIS 205 nm

TLC-Analysis HPLC-Analysis

Diethyl ether-Extraction Diethyl ether-Extraction

Silica gel RP-18 column

Petroleum ether-Ethyl acetate-Cyclohexane (5 + 3 + 2)

A: 0.001% Phosphoric acidB: Acetonitrile

Anisaldehyde sulphuric acid reagent, VIS 270 nm

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455

Appendix

8. Phenolcarboxylic acids(see Monographs No. 49, 51, 57, 59, 74, 78)

TLC-Analysis HPLC-Analysis

MeOH-Extraction MeOH-Extraction

Silica gel RP-18 column

Ethyl acetate-Formic acid-Glacial acetic acid-Water (10 + 1.1 + 1.1 + 2.6)

A: 0.001% Phosphoric acidB: Acetonitrile

NP/PEG, UV 366 nm 220 nm

TLC-Analysis HPLC-Analysis

acidi ed MeOH-Extraction acidi ed MeOH-Extraction

Silica gel RP-18 column

Chloroform-Ethyl acetate-Toluene-Formic acid-MeOH (15 + 20 + 10 + 10 + 1)

A: 0.001% Phosphoric acidB: Acetonitrile

UV 254 nm 281 nm

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457

AAconitine, 980–982, 984, 985, 988, 989actein, 560, 561, 563, 564, 567acteoside, 24, 29–31, 33, 428, 431–434, 436alisol A, 468, 469Alkamides, 46, 49, 52, 192andrographolide, 274–278anthraguinone, 212Anthraquinone, 440, 444, 445, 448, 858, 859,

861, 863, 865, 866, 868, 873, 936, 942, 943, 949

Aristolochiae radix, 313, 319, 320, 322, 323, 364, 365, 367, 376–379

aristolochic acid, 56, 319, 321–323, 364–367, 376–379

asarinin, 46, 49, 51–53, 56, 192, 194, 730asperosaponin, 678, 679, 681, 684, 688Astragalosides, 84, 89–91, 96atractylon, 114–117, 119–122, 124, 693,

695–698, 701, 702aucubin, 24, 26–30, 428, 431, 432, 832, 833,

835–838, 841

BBaicalin, 302, 756, 760, 762, 764, 905-asarone, 779–786, 788

berberine, 302–308, 498, 575–580, 582, 584, 585

betulinic acid, 142–145, 326, 328, 329, 331–333, 382, 385, 387, 389, 390, 938

-eudesmol, 693, 695–699, 704, 705, 877

Ccarotenoids, 522, 525, 526, 529, 532, 556carthamin, 476, 477, 479–482catechin, 212, 216–218, 344–347, 349, 861,

867, 868, 952, 953, 955–958, 960, 963, 964Chrysophanol, 440, 859–863, 865–868, 873,

936, 939, 941, 942, 945, 948, 949cinnamaldehyde, 992, 993, 995, 997, 998,

1001–1003, 1006

coptisine, 302–308, 666corydaline, 666–668, 670, 672, 674crocetin, 246, 249–252curcumin I, 605, 606, 611

Ddioscin, 619–621, 623, 624, 626, 629, 806,

807, 809, 811, 813, 814, 820, 822, 825diosgenin, 617, 619–625, 806, 807, 809, 810,

813, 814, 820–822, 824, 825, 829

Eeleutheroside, 416–423emodin, 440–445, 447, 448, 859–863,

865–867, 873, 936, 939, 941, 942, 945, 948, 949

epimedins A, 487epimedins B, 486, 487ergosterol, 634–636, 638, 639, 643, 925evocarpine, 392–396evodiamine, 392–396, 398, 400

Fforsythoside, 382, 388, 390fukinolic acid, 560–562, 565furanocoumarins, 100, 104, 105, 110, 152,

155, 165, 169, 172, 174, 175, 178, 500furanocoumasin, 693

Gganoderic acid, 634–636, 638, 639, 643gardenoside, 246, 248, 249, 251–253gastrodin, 256–260, 262ginsenoside, 844, 845, 847–850, 853, 854,

877–879, 883–887, 890

Hharpagoside, 428, 431–434, 436hederageninglycosides, 356, 590, 678hesperidin, 649–652, 654, 655, 657, 661, 662honokiol, 204–206, 208, 209

Index

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Index

458

Iicariin, 486–488, 490, 491, 493, 497indigo, 792–798, 801indigotin, 792, 793, 801iridin, 128–133, 138Iso avone, 84, 96, 129, 130, 138, 222, 224,

226–228, 292iso avonoids, 128, 222

Jjujuboside A, 326–330, 332, 333jujuboside B, 326, 327, 329, 330, 332

Kkirenol, 894–899, 901kuwanone, 536

Lleonurine, 708, 709lignan, 39, 41, 43, 44, 46, 49, 52, 56, 60, 73,

74, 81, 192, 198, 382, 390, 416, 418–420, 423, 487, 510, 575, 720, 722, 723, 725, 726, 730, 832, 836

ligustilide, 162limonin, 302, 392, 394, 575, 576, 578,

580–582, 584, 650loganin, 428, 590, 593, 595–597, 678–681,

684, 688luteolin-7-O- -D-glucoside, 142, 145, 590luteolinglucoside, 590

Mmagno orine, 302, 369, 371–374, 376, 488,

575, 577–580, 582, 584, 720magnolin, 720, 722, 723, 725, 726magnolol, 204–206, 208, 209mangiferin, 128–130, 132, 133, 138, 404–406,

408, 410, 412maslinic acid, 326, 768, 773matrine, 744, 745, 747, 749, 753Mesaconitine, 980–982, 984, 985, 988, 989

Nnaringin, 212–218, 649, 650, 652, 654, 655,

657, 661, 662

Oophiopogonin A, 820, 821osthol, 100, 102, 103, 106, 110, 500–506, 693

Ppachymic acid, 924, 925, 928paeoni orin, 283–286, 288, 289palmatine, 302–308, 575–577, 579, 580, 582,

584, 666–668, 670–672, 674, 675phillyrin, 382, 385, 386, 388, 390physalien, 522, 523, 525, 526, 530, 532physcion, 212, 440–445, 447, 448, 859, 860,

862, 863, 866–868, 873, 936, 939, 941, 942, 945, 948

pinoresinol, 73–77, 79, 234, 382, 385, 387, 389, 390, 832, 833, 835, 836, 838, 840, 841

piperine, 730–739polyacetylene, 2, 6, 7, 9, 100, 110, 114, 117,

120, 121, 124, 125, 152, 159, 162, 172, 178, 182, 234, 264, 476, 693, 844, 850, 854, 878, 886, 887, 890, 975

pomolic acid, 768, 770–773Processing, 71, 311, 391, 439, 616, 618, 977,

978, 982, 988, 989Procyanidins, 859, 992–994, 1000, 1005pteropodine, 344, 347, 349, 350puerarin, 222, 224, 226–230

Rresveratrol, 128–133, 138, 859rhynchophylline, 344–348, 350, 353rosmarinic acid, 142, 145, 905–908, 912, 914rutaecarpine, 392–396, 398, 400

Ssaf or yellow A, 476, 479, 481, 483saikosaponin, 2, 4–7, 9–11salvianolic acid, 905–908, 912, 914, 920sarsasapogenin, 404–406, 408, 409, 412schisandrin, 39–44scopoletin, 100, 114, 172, 173, 370–373,

510–513, 516, 522, 524, 525, 527, 528, 536, 539, 541, 551, 552, 968, 969, 971–973, 975

Scutellarin, 756, 760sesamin, 46, 49, 51–53, 56, 60, 192–194, 416,

730

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459

Index

Sinomenine, 369–374, 376, 379sophora avanone, 744, 745, 747, 748, 750,

752stilbene, 128, 129, 131, 132, 138, 440, 444,

859, 861, 873syringaresinol, 416, 417, 488, 490, 491, 575,

832, 833, 835

Ttangshenoside I, 234, 237–239, 441, 444tanshinones, 904, 908, 909, 912, 914–916,

918, 920tectoridin, 128–133, 138

tectorigenin, 128–130, 133, 138tetrandrine, 311–315, 317–319, 321, 323tumulosic acid, 924, 925

Vverticine, 14, 15, 17, 18, 20

Wwedelolactone, 264–267, 269, 270

ZZ-ligustilide, 163, 165–167, 169, 182–186,

188

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461

Drug monograph, Marker compounds, Chemical classifi cation, Processing

Drug monograph Marker compounds

Chemical classi cation

Processing

1 Bupleuri radix Saikosaponin Polyacetylenes

Phyto-Fungi 2 Fritillariae bulbus Verticine 3 Rehmanniae radix Aucubin Acteoside 4 Schisandrae fructus Schisandrin 5 Asari radix et rhizoma Asarinin

Sesamin Alkamides

Lignans 6 Houttuyniae cordatae herba Sesamin Lignans 7 Pinelliae rhizoma Pinoresinol

Lignans processing8 Astragali radix Astragaloside Iso avones 9 Angelicae pubescentis radix Furanocoumarins

Phyto-Fungi Polyacetylenes 10 Atractylodis macrocephalae rhizoma Polyacetylenes Phyto-Fungi 11 Belamcandae sinensis rhizoma Iridin

Tectoridin Resveratrol Iso avonoids

Stilbenes

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Drug monograph, Marker compounds, Chemical classi cation, Processing

462

12 Lycopi lucidi herba Luteolin--glucoside

Betulinic acid Rosmarinic acid 13 Notopterygii rhizoma seu radix Furanocoumarins

Phyto-Fungi Polyacetylenes 14 Angelicae sinensis radix Ligustilide

Phyto-Fungi Polyacetylenes 15 Angelicae dahuricae radix Scopoletin

Furonacoumarins Phyto-Fungi

Polyacetylenes 16 Ligustici chuanxiong radix Ligustilide

Phyto-Fungi Polyacetylenes

17 Zanthoxyli pericarpium Sesamin Alkamides

Lignans 18 Magnoliae of cinalis cortex Magnolol Honokiol 19 Drynariae rhizoma Naringin Anthraquinones 20 Puerariae radix Puerarin Iso avonoids

21 Codonopsis pilosulae radix Tangshenoside 22 Gardeniae fructus Gardenoside Crocetin 23 Gastrodiae rhizoma Gastrodin 24 Ecliptae herba Wedelolactone

Polyacetylenes Phyto-Fungi 25 Andrographis herba Andrographolide 26 Paeoniae albae/rubrae radix Paeoni orin

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463

Drug monograph, Marker compounds, Chemical classi cation, Processing

27 Sophorae os Iso avone 28 Coptidis rhizoma Berberine Coptisine

29 Stephaniae tetrandrae radix Tetrandrine Aristolochia acid

30 Ziziphi spinosae semen Jujuboside 31 Amomi rotundus fructus 32 Uncariae cum Uncis ramulus Rhychnophylline

Pteropodine Catechins 33 Clematidis radix Hederagenin-

glycosides

Aristolochia acid 34 Sinomenii caulis Magno orine

Aristolochia acid Sinomenine

35 Forsythiae fructus Forsythoside Phillyrin (Forsythin)

Pinoresinol Lignans 36 Evodiae fructus Evodiamine

Rutaecarpine Evocarpine

37 Anemarrhenae rhizoma Sarsasapogenin Magniferin

Lignans 38 Acanthopanacis radix Eleutheroside

Syringaresinol Lignans 39 Scrophulariae radix Harpagoside

Aucubin Loganin 40 Polygoni multi ori radix Emodin

Physcion

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Drug monograph, Marker compounds, Chemical classi cation, Processing

464

Anthraquinones Stilbenes

41 Alismatis rhizoma Alisol 42 Carthami os Carthamin Saf or yellow

43 Epimedii herba Icariin Epimedin 44 Cnidii fructus Osthol Furanocoumarins 45 Lycii radicis cortex Scopoletin Lignans 46 Fructus Lycii Scopoletin

Physalien Carotenoids 47 Mori radicis cortex Kuwanone 48 Mori folium 49 Cimicifugae rhizoma Actein Fukinolic acid 50 Phellodendri cortex Berberine

Palmatine Limonin 51 Lonicerae os, caulis Loganin

Hederagenin-glycosides

Luteolin-glucoside

52 Curcumae longae rhizoma/radix Curcumin 53 Dioscoreae ssp. rhizoma Dioscin Diosgenin 54 Ganoderma Ganoderic acids Ergosterol

55 Citri reticulatae pericarpium Hesperidin Limonin

Naringin 56 Corydalis rhizoma Palmatine

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465

Drug monograph, Marker compounds, Chemical classi cation, Processing

Coptisine Corydaline

57 Dipsaci radix Loganin Hederagenin-glycosides

Asperosaponin 58 Atractylodis lanceae rhizoma Eudesmol

Atractylon Phyto-Fungi

Polyacetylenes Furanocoumarins 59 Leonuri herba Leonurine 60 Magnoliae os Magnolin Lignans 61 Piperis longi fructus Piperine

Sesamin Lignans 62 Sophorae avescentis radix Matrine Sophora avanone 63 Scutellariae radix Baicalin Scutellarin 64 Chaenomelis fructus Pomolic acid Maslinic acid 65 Acori rhizoma -Asarone 66 Isatidis radix Indigo Indigotin 67 Tribuli fructus Diosgenin Dioscin 68 Ophiopogonis radix Ophiopogonines 69 Eucommiae cortex Pinoresinol

Syringaresinol Aucubin

Lignans 70 Notoginseng radix et rhizoma Ginsenoside

Polyacetylenes

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Drug monograph, Marker compounds, Chemical classi cation, Processing

466

Phyto-Fungi 71 Rhei radix et rhizoma Emodin

Physcion Resveratrol

Stilbenes Anthraquinones 72 Ginseng/Quinquefolii radix/rhizoma Ginsenosides

Polyacetylenes Phyto-Fungi 73 Siegesbeckiae herba Kirenol 74 Salviae miltiorrhizae radix/rhizoma Tanshinone

Rosmarinic acid Salvianolic acid 75 Poria Pachymic acid Tumulosic acid 76 Cassiae semen Emodin

Chrysophanol Physcion

Anthraquinones 77 Camelliae folium Catechins 78 Artemisiae scopariae herba Scopoletin 79 Aconiti radix praeparata Aconitine

Mesaconitine processing80 Cinnamomi cortex Cinnamaldehyde Procyanidins

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1009

Appendix

Basic Solvent Systems, reagents and columns for the TLC-, GC- and HPLC- ngerprint Analysis

of main structure types of natural productsAlkaloids1. Amides2. Phenolics 3.

Flavones a) Procyanidinesb) Cumarinsc) Anthraquinonesd)

Essential oils4. Lignans5. Triterpene-/Steroidsaponins6. Other Terpenoids (Diterpenoids)7. Phenolcarboxylic acids8.

1. Alkaloids (see Monographs No. 2, 28, 29, 32, 34, 36, 45, 50, 56, 62, 79)

TLC-Analysis HPLC-Analysis

Ammonia solution 10%; MeOH-Extraction Ammonia solution 10%; MeOH-Extraction

Silica gel/HPTLC Silica gel RP-select B column (C-8)

Chloroform-Methanol-Water(6 + 3 + 0.65)

A: 2 g Hexanesulfonic acid (pH 3)B: Acetonitrile

Iodine reagent, VIS 210 nm

TLC-Analysis HPLC-Analysis

MeOH-Extraction MeOH-Extraction

HPTLC Silica gel RP-select B column (C-8)

Ethyl acetate-Methyl ethyl ketone-Formic acid-Water (5 + 3 + 1 + 1)

A: 0.68 g KH2PO4/1 l, pH = 9 (KOH)B: Acetonitrile

UV 366 nm, Dragendorff reagent, VIS 270 nm

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Appendix

1010

2. Amides(see Monograph No. 61)

TLC-Analysis HPLC-Analysis

n-hexane-Extraction n-hexane-Extraction

Silica gel RP-18 column

n-Hexane-Ethyl acetate (5 + 3)

A: WaterB: Acetonitrile

UV 254 nmAnisaldehyde sulphuric acid reagent, VIS

254 nm

3a. Flavones (see Monographs No. 20, 27, 43, 48, 51, 55, 59, 62, 63, 67)

TLC-Analysis HPLC-Analysis

MeOH-Extraction MeOH-Extraction

Silica gel/HPTLC Silica gel RP-18 column

Ethyl acetate-Formic acid-Glacial acetic acid-Water (10 + 1.1 + 1.1 + 2.6)

A: 0.001% Phosphoric acidB: Acetonitrile

NP/PEG, UV 366 nm 210/270 nm

3b. Procyanidines(see Monographs No. 77, 80)

TLC-Analysis HPLC-Analysis

Acetone/Water (1:1)-Extraction; Diethylether Acetone/Water (1:1)-Extraction; Diethylether

Silica gel/HPTLC Silica gel RP-18 column

Ethyl acetate-Methanol-Water (10 + 2 + 1)

A: 0.001% Phosphoric acidB: Acetonitrile

Anisaldehyde sulphuric acid reagent, VIS 210/270 nm

3c. Cumarines(see Monographs No. 13, 38, 45, 46, 78)

TLC-Analysis HPLC-Analysis

50% MeOH/Butanol-Extraction 50% MeOH/Butanol-Extraction

Silica gel/HPTLC Silica gel RP-18 column

Toluene-Ethyl acetate-Acetic acid(90 + 10 + 1)

A: 0.001% Phosphoric acidB: Acetonitrile

NP/PEG, UV 366 nm 210/280 nm

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1011

Appendix

3d. Anthraquinones(see Monographs No. 40, 71,76)

TLC-Analysis HPLC-Analysis

MeOH-Extraction MeOH-Extraction

HPTLC Silica gel RP-18 column

Light petroleum-Ethyl acetate-Formic acid (75+25+1) for aglycones and glycosidesEthyl acetate-MeOH-Water (100+13.5+10)

A: 0.05% Phosphoric acid B: Acetonitrile

NP/PEG, UV 366 nmPhosphomolybdic acid, VIS

254/280 nm

4. Essential oils(see Monographs No. 31, 36, 46, 52, 60, 65, 80)

TLC-Analysis GC-Analysis

Distillation or n-Hexane-Extraction Distillation (dil. 1:100 oil/tertButylmethylether)

Silica gel Varian VF-5 ms with 10 m precolumn (deactivated methyl-polysiloxan)

Toluene-Ethyl acetate (93 + 7) Helium

Vanillin sulphuric acid reagent, VIS 270 °C

5. Lignans(see Monographs No. 4, 7, 17, 35, 38, 60, 69)

TLC-Analysis HPLC-Analysis

MeOH-Extraction MeOH-Extraction

Silica gel/HPTLC Silica gel RP-18 column

Toluene-Ethyl acetate-Formic acid (80 + 15 + 10)

A: 0.001% Phosphoric acidB: Acetonitrile

Anisaldehyde sulphuric acid reagent, VIS 210 nm

TLC-Analysis

50% MeOH/Butanol-Extraction

Silica gel/HPTLC Silica gel

Chloroform-MeOH (9+1)

Vanillin phosphoric/sulphuric acid reagent, VIS

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Appendix

1012

6. Triterpene-/Steroidsaponins(see Monographs No. 1, 20, 30, 33, 37, 51, 53, 57, 67, 68, 70)

TLC-Analysis HPLC-Analysis

MeOH/Water/Butanol-Extraction MeOH-Extraction

Silica gel/HPTLC Silica gel RP-18 column

Chloroform-MeOH-Water, lower layer A: WaterB: Acetonitrile

Vanillin phosphoric/sulphuric acid reagent or Anisaldehyde sulphuric acid reagent, VIS

210 nm

7. Other Terpenoids (Diterpenoids)(see Monographs No. 25, 41, 49, 54, 59, 64, 73, 74, 75)

TLC-Analysis HPLC-Analysis

MeOH/Ethyl acetate/Water-Extraction MeOH/Ethyl acetate/Water-Extraction

Silica gel/HPTLC Silica gel RP-18 column

Ethyl formate-Toluene-Formic acid (50 + 50 + 15)

A: 0.001% Phosphoric acidB: Acetonitrile

Anisaldehyde sulphuric acid reagent, VIS 205 nm

TLC-Analysis HPLC-Analysis

Diethyl ether-Extraction Diethyl ether-Extraction

Silica gel RP-18 column

Petroleum ether-Ethyl acetate-Cyclohexane (5 + 3 + 2)

A: 0.001% Phosphoric acidB: Acetonitrile

Anisaldehyde sulphuric acid reagent, VIS 270 nm

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1013

Appendix

8. Phenolcarboxylic acids(see Monographs No. 49, 51, 57, 59, 74, 78)

TLC-Analysis HPLC-Analysis

MeOH-Extraction MeOH-Extraction

Silica gel RP-18 column

Ethyl acetate-Formic acid-Glacial acetic acid-Water (10 + 1.1 + 1.1 + 2.6)

A: 0.001% Phosphoric acidB: Acetonitrile

NP/PEG, UV 366 nm 220 nm

TLC-Analysis HPLC-Analysis

acidi ed MeOH-Extraction acidi ed MeOH-Extraction

Silica gel RP-18 column

Chloroform-Ethyl acetate-Toluene-Formic acid-MeOH (15 + 20 + 10 + 10 + 1)

A: 0.001% Phosphoric acidB: Acetonitrile

UV 254 nm 281 nm

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1015

AAconitine, 980–982, 984, 985, 988, 989actein, 560, 561, 563, 564, 567acteoside, 24, 29–31, 33, 428, 431–434, 436alisol A, 468, 469Alkamides, 46, 49, 52, 192andrographolide, 274–278anthraguinone, 212Anthraquinone, 440, 444, 445, 448, 858, 859,

861, 863, 865, 866, 868, 873, 936, 942, 943, 949

Aristolochiae radix, 313, 319, 320, 322, 323, 364, 365, 367, 376–379

aristolochic acid, 56, 319, 321–323, 364–367, 376–379

asarinin, 46, 49, 51–53, 56, 192, 194, 730asperosaponin, 678, 679, 681, 684, 688Astragalosides, 84, 89–91, 96atractylon, 114–117, 119–122, 124, 693,

695–698, 701, 702aucubin, 24, 26–30, 428, 431, 432, 832, 833,

835–838, 841

BBaicalin, 302, 756, 760, 762, 764, 905-asarone, 779–786, 788

berberine, 302–308, 498, 575–580, 582, 584, 585

betulinic acid, 142–145, 326, 328, 329, 331–333, 382, 385, 387, 389, 390, 938

-eudesmol, 693, 695–699, 704, 705, 877

Ccarotenoids, 522, 525, 526, 529, 532, 556carthamin, 476, 477, 479–482catechin, 212, 216–218, 344–347, 349, 861,

867, 868, 952, 953, 955–958, 960, 963, 964Chrysophanol, 440, 859–863, 865–868, 873,

936, 939, 941, 942, 945, 948, 949cinnamaldehyde, 992, 993, 995, 997, 998,

1001–1003, 1006

coptisine, 302–308, 666corydaline, 666–668, 670, 672, 674crocetin, 246, 249–252curcumin I, 605, 606, 611

Ddioscin, 619–621, 623, 624, 626, 629, 806,

807, 809, 811, 813, 814, 820, 822, 825diosgenin, 617, 619–625, 806, 807, 809, 810,

813, 814, 820–822, 824, 825, 829

Eeleutheroside, 416–423emodin, 440–445, 447, 448, 859–863,

865–867, 873, 936, 939, 941, 942, 945, 948, 949

epimedins A, 487epimedins B, 486, 487ergosterol, 634–636, 638, 639, 643, 925evocarpine, 392–396evodiamine, 392–396, 398, 400

Fforsythoside, 382, 388, 390fukinolic acid, 560–562, 565furanocoumarins, 100, 104, 105, 110, 152,

155, 165, 169, 172, 174, 175, 178, 500furanocoumasin, 693

Gganoderic acid, 634–636, 638, 639, 643gardenoside, 246, 248, 249, 251–253gastrodin, 256–260, 262ginsenoside, 844, 845, 847–850, 853, 854,

877–879, 883–887, 890

Hharpagoside, 428, 431–434, 436hederageninglycosides, 356, 590, 678hesperidin, 649–652, 654, 655, 657, 661, 662honokiol, 204–206, 208, 209

Index

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Index

1016

Iicariin, 486–488, 490, 491, 493, 497indigo, 792–798, 801indigotin, 792, 793, 801iridin, 128–133, 138Iso avone, 84, 96, 129, 130, 138, 222, 224,

226–228, 292iso avonoids, 128, 222

Jjujuboside A, 326–330, 332, 333jujuboside B, 326, 327, 329, 330, 332

Kkirenol, 894–899, 901kuwanone, 536

Lleonurine, 708, 709lignan, 39, 41, 43, 44, 46, 49, 52, 56, 60, 73,

74, 81, 192, 198, 382, 390, 416, 418–420, 423, 487, 510, 575, 720, 722, 723, 725, 726, 730, 832, 836

ligustilide, 162limonin, 302, 392, 394, 575, 576, 578,

580–582, 584, 650loganin, 428, 590, 593, 595–597, 678–681,

684, 688luteolin-7-O- -D-glucoside, 142, 145, 590luteolinglucoside, 590

Mmagno orine, 302, 369, 371–374, 376, 488,

575, 577–580, 582, 584, 720magnolin, 720, 722, 723, 725, 726magnolol, 204–206, 208, 209mangiferin, 128–130, 132, 133, 138, 404–406,

408, 410, 412maslinic acid, 326, 768, 773matrine, 744, 745, 747, 749, 753Mesaconitine, 980–982, 984, 985, 988, 989

Nnaringin, 212–218, 649, 650, 652, 654, 655,

657, 661, 662

Oophiopogonin A, 820, 821osthol, 100, 102, 103, 106, 110, 500–506, 693

Ppachymic acid, 924, 925, 928paeoni orin, 283–286, 288, 289palmatine, 302–308, 575–577, 579, 580, 582,

584, 666–668, 670–672, 674, 675phillyrin, 382, 385, 386, 388, 390physalien, 522, 523, 525, 526, 530, 532physcion, 212, 440–445, 447, 448, 859, 860,

862, 863, 866–868, 873, 936, 939, 941, 942, 945, 948

pinoresinol, 73–77, 79, 234, 382, 385, 387, 389, 390, 832, 833, 835, 836, 838, 840, 841

piperine, 730–739polyacetylene, 2, 6, 7, 9, 100, 110, 114, 117,

120, 121, 124, 125, 152, 159, 162, 172, 178, 182, 234, 264, 476, 693, 844, 850, 854, 878, 886, 887, 890, 975

pomolic acid, 768, 770–773Processing, 71, 311, 391, 439, 616, 618, 977,

978, 982, 988, 989Procyanidins, 859, 992–994, 1000, 1005pteropodine, 344, 347, 349, 350puerarin, 222, 224, 226–230

Rresveratrol, 128–133, 138, 859rhynchophylline, 344–348, 350, 353rosmarinic acid, 142, 145, 905–908, 912, 914rutaecarpine, 392–396, 398, 400

Ssaf or yellow A, 476, 479, 481, 483saikosaponin, 2, 4–7, 9–11salvianolic acid, 905–908, 912, 914, 920sarsasapogenin, 404–406, 408, 409, 412schisandrin, 39–44scopoletin, 100, 114, 172, 173, 370–373,

510–513, 516, 522, 524, 525, 527, 528, 536, 539, 541, 551, 552, 968, 969, 971–973, 975

Scutellarin, 756, 760sesamin, 46, 49, 51–53, 56, 60, 192–194, 416,

730

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1017

Index

Sinomenine, 369–374, 376, 379sophora avanone, 744, 745, 747, 748, 750,

752stilbene, 128, 129, 131, 132, 138, 440, 444,

859, 861, 873syringaresinol, 416, 417, 488, 490, 491, 575,

832, 833, 835

Ttangshenoside I, 234, 237–239, 441, 444tanshinones, 904, 908, 909, 912, 914–916,

918, 920tectoridin, 128–133, 138

tectorigenin, 128–130, 133, 138tetrandrine, 311–315, 317–319, 321, 323tumulosic acid, 924, 925

Vverticine, 14, 15, 17, 18, 20

Wwedelolactone, 264–267, 269, 270

ZZ-ligustilide, 163, 165–167, 169, 182–186,

188

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1019

Drug monograph, Marker compounds, Chemical classifi cation, Processing

Drug monograph Marker compounds

Chemical classi cation

Processing

1 Bupleuri radix Saikosaponin Polyacetylenes

Phyto-Fungi 2 Fritillariae bulbus Verticine 3 Rehmanniae radix Aucubin Acteoside 4 Schisandrae fructus Schisandrin 5 Asari radix et rhizoma Asarinin

Sesamin Alkamides

Lignans 6 Houttuyniae cordatae herba Sesamin Lignans 7 Pinelliae rhizoma Pinoresinol

Lignans processing8 Astragali radix Astragaloside Iso avones 9 Angelicae pubescentis radix Furanocoumarins

Phyto-Fungi Polyacetylenes 10 Atractylodis macrocephalae rhizoma Polyacetylenes Phyto-Fungi 11 Belamcandae sinensis rhizoma Iridin

Tectoridin Resveratrol Iso avonoids

Stilbenes

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Drug monograph, Marker compounds, Chemical classi cation, Processing

1020

12 Lycopi lucidi herba Luteolin--glucoside

Betulinic acid Rosmarinic acid 13 Notopterygii rhizoma seu radix Furanocoumarins

Phyto-Fungi Polyacetylenes 14 Angelicae sinensis radix Ligustilide

Phyto-Fungi Polyacetylenes 15 Angelicae dahuricae radix Scopoletin

Furonacoumarins Phyto-Fungi

Polyacetylenes 16 Ligustici chuanxiong radix Ligustilide

Phyto-Fungi Polyacetylenes

17 Zanthoxyli pericarpium Sesamin Alkamides

Lignans 18 Magnoliae of cinalis cortex Magnolol Honokiol 19 Drynariae rhizoma Naringin Anthraquinones 20 Puerariae radix Puerarin Iso avonoids

21 Codonopsis pilosulae radix Tangshenoside 22 Gardeniae fructus Gardenoside Crocetin 23 Gastrodiae rhizoma Gastrodin 24 Ecliptae herba Wedelolactone

Polyacetylenes Phyto-Fungi 25 Andrographis herba Andrographolide 26 Paeoniae albae/rubrae radix Paeoni orin

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1021

Drug monograph, Marker compounds, Chemical classi cation, Processing

27 Sophorae os Iso avone 28 Coptidis rhizoma Berberine Coptisine

29 Stephaniae tetrandrae radix Tetrandrine Aristolochia acid

30 Ziziphi spinosae semen Jujuboside 31 Amomi rotundus fructus 32 Uncariae cum Uncis ramulus Rhychnophylline

Pteropodine Catechins 33 Clematidis radix Hederagenin-

glycosides

Aristolochia acid 34 Sinomenii caulis Magno orine

Aristolochia acid Sinomenine

35 Forsythiae fructus Forsythoside Phillyrin (Forsythin)

Pinoresinol Lignans 36 Evodiae fructus Evodiamine

Rutaecarpine Evocarpine

37 Anemarrhenae rhizoma Sarsasapogenin Magniferin

Lignans 38 Acanthopanacis radix Eleutheroside

Syringaresinol Lignans 39 Scrophulariae radix Harpagoside

Aucubin Loganin 40 Polygoni multi ori radix Emodin

Physcion

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Drug monograph, Marker compounds, Chemical classi cation, Processing

1022

Anthraquinones Stilbenes

41 Alismatis rhizoma Alisol 42 Carthami os Carthamin Saf or yellow

43 Epimedii herba Icariin Epimedin 44 Cnidii fructus Osthol Furanocoumarins 45 Lycii radicis cortex Scopoletin Lignans 46 Fructus Lycii Scopoletin

Physalien Carotenoids 47 Mori radicis cortex Kuwanone 48 Mori folium 49 Cimicifugae rhizoma Actein Fukinolic acid 50 Phellodendri cortex Berberine

Palmatine Limonin 51 Lonicerae os, caulis Loganin

Hederagenin-glycosides

Luteolin-glucoside

52 Curcumae longae rhizoma/radix Curcumin 53 Dioscoreae ssp. rhizoma Dioscin Diosgenin 54 Ganoderma Ganoderic acids Ergosterol

55 Citri reticulatae pericarpium Hesperidin Limonin

Naringin 56 Corydalis rhizoma Palmatine

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1023

Drug monograph, Marker compounds, Chemical classi cation, Processing

Coptisine Corydaline

57 Dipsaci radix Loganin Hederagenin-glycosides

Asperosaponin 58 Atractylodis lanceae rhizoma Eudesmol

Atractylon Phyto-Fungi

Polyacetylenes Furanocoumarins 59 Leonuri herba Leonurine 60 Magnoliae os Magnolin Lignans 61 Piperis longi fructus Piperine

Sesamin Lignans 62 Sophorae avescentis radix Matrine Sophora avanone 63 Scutellariae radix Baicalin Scutellarin 64 Chaenomelis fructus Pomolic acid Maslinic acid 65 Acori rhizoma -Asarone 66 Isatidis radix Indigo Indigotin 67 Tribuli fructus Diosgenin Dioscin 68 Ophiopogonis radix Ophiopogonines 69 Eucommiae cortex Pinoresinol

Syringaresinol Aucubin

Lignans 70 Notoginseng radix et rhizoma Ginsenoside

Polyacetylenes

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Drug monograph, Marker compounds, Chemical classi cation, Processing

1024

Phyto-Fungi 71 Rhei radix et rhizoma Emodin

Physcion Resveratrol

Stilbenes Anthraquinones 72 Ginseng/Quinquefolii radix/rhizoma Ginsenosides

Polyacetylenes Phyto-Fungi 73 Siegesbeckiae herba Kirenol 74 Salviae miltiorrhizae radix/rhizoma Tanshinone

Rosmarinic acid Salvianolic acid 75 Poria Pachymic acid Tumulosic acid 76 Cassiae semen Emodin

Chrysophanol Physcion

Anthraquinones 77 Camelliae folium Catechins 78 Artemisiae scopariae herba Scopoletin 79 Aconiti radix praeparata Aconitine

Mesaconitine processing80 Cinnamomi cortex Cinnamaldehyde Procyanidins