Analgesics / Cough 1 & Cold Medicine Ingredients

Transcription

1 Analgesics / Cough & Cold Medicine Ingredients mau H. paracetamol H CH H H. -aobenzoic acid H H H C CH. -hydroxybenzoic acid 7 CH H CH. caffeine 8 9 H. -acetamidophenol 0 H H. -hydroxybenzoic acid H C8-AR 7. salicylamide H H H C 0. aspirin CH H H H 8. acetanilide H H C. salicylic acid C H. benzoic acid H H H 9. phenol H CH H. sorbic acid. phenacetin,, ,, C8. salicylaldehyde 0x.mm, mm Gradient analysis A = 0.% v/v formic acid (aq) B = 0.% v/v formic acid in MeC 0C 0nm.0mL/ T () %B 0 9

2 Pharmaceutically Relevant Mixture UltraCore SuperC8: selectivity with ph: 8,9 7 0 ph 0x.mm,.mm Gradient analysis A= 0mM HCH, ph (aq) B= 0mM HCH, ph in MeC/water 9: v/v A= 0.% H, ph 0.7 (aq) B= 0.% H, ph0.7 in in MeC/water 9: v/v T %B DAD C, Sig=,8 Ref=0,00 (F:\0-MJ\0_LW_PH \LW D) DAD C, Sig=,8 Ref=0,00 (F:\0-MJ\ \HIGH D) 0 ph 0.7 0C 0.0 ml/ nm. Atenolol. Methylphenylsulfoxide. Eserine. Prilocaine. Bupivacaine. Tetracaine 7.,,,-Tetrahydro--naphthol 8. Carvedilol 9. itrobenzene 0. Methdilazine. Amitriptyline. Valerophenone

3 Paraben Preservatives Phenyl, 0 x.mm Isocratic Methanol mm H Ac (0:0), ph.8 Flow rate: 0.ml/ Column temperature: 0 C Detection: UV at 0nm Sample volume: μl. Methylparaben. Ethylparaben. n-propylparaben. i-butylparaben. -Butylparaben. Benzylparaben Reproduced with permission of Trevor Gibson, The Chemical Analysis Facility, University of Reading

4 Pharmaceutically Relevant mixture Separation UltraCore SuperPhenylHexyl: selectivity with ph: 9,,8 ph 0x.mm,.mm Gradient analysis A= 0mM HCH, ph (aq) B= 0mM HCH, ph in MeH/water 9: v/v 0 A= 0.% H, ph 0.7 (aq) B= 0.% H, ph0.7 in in MeH/water 9: v/v 7 T %B C 0.0 ml/ nm 0 78 ph Benzamide. Caffeine. Procainamide. -acetylprocainamide. Propiophenone. Toluene 7. Remacemide 8. Ethylbenzene 9. Carvdilol 0. ortriptyline. Clomiprae

5 Clonidine Hydrochloride Clonidine hydrochloride oral solution containing preservatives Concentration clonidine HCl = 0μg/ml Concentration Preservatives ~.g/ml. Clonidine hydrochloride. Methyl hydroxybenzoate. Propyl hydroxybenzoate UltraCore SuperC8.μm, 0 x.mm Gradient analysis A = 0.% w/v phosphate buffer-ch H- CH C (80:0:0) B = CH C Time (s) %B Flow rate: ml/ Column temperature: 0 C Injection volume: 00μl Detection: UV, 0nm Reproduced with permission of Mary guyen, Guys Hospital, London

6 Procaine and p-aobenzoic acid p-aobenzoic acid (potential degradant) Procaine Procaine sterile manufactured product System suitability tests C8-PFP μm, 00 x.mm Isocratic analysis Methanol - 0.% acetic acid (9:8) (adjusted to ph.7 with 0% ah) Flow rate: ml/ Detection: UV, 79nm Detection limits for S/ = 0 Procaine = 0.000mg/ml p-aobenzoic acid = mg/ml Reproduced with permission of John Peace, Huddersfield Royal Infirmary, UK

7 mau Water Soluble Vitas C8-AR 00 H H H H C Pyridoxine (vita B) CH Pantothenic acid (vita B) H H H CH H H H p-aobenzoic acid H Folic acid (vita B9 or vita M) H H D-Biotin (vita B7 or vita H) H H H H H H H H S H H C H C H Cyanocobala (vita B) H Riboflavin (vita B) 0x.mm, mm Gradient analysis A = 0mM KH P, ph.8 (aq) B = 0mM KH P, ph.8 in : v/v MeH:water 0C 0nm.mL/ T () %B H 7 H H. Pyridoxine (vita B). Pantothenic acid (vita B). p-aobenzoic acid. Folic acid (vita B9 or vita M). D-Biotin (vita B7 or vita H). Cyanocobala (vita B) 7. Riboflavin (vita B)

8 mau C8-AR Water Soluble Vitas / Polar Molecules Isonicotinamide H C H H + S H C Thiae or vita B H icotinamide H H H H H 7 H L-Ascorbic acid or vita C H H Hypoxanthine H H H rotic acid 0 H um, 0 x. mm Isocratic analysis Flow rate:.0 ml/ Temperature: C Detection: UV 0 nm MP: 9.:. v/v 0.% HP (aq) : MeH 8 8 H -aobenzoic acid H H C Pyridoxal or H Pyridoxae or Vita B H CH H vita B 9 H H H Pyridoxine or vita B CH H 0 8

9 C8-AR on-steroidal Anti-Inflammatory Drugs CH H 9 mau Ketoprofen H C aproxen CH H Indomethacin Cl 0x.mm, mm Gradient analysis A = 0.% v/ formic acid (aq) B = 0.% v/v formic acid in MeH 0C.0mL/ nm T () %B H F F F H H C Sulindac CH S CH Ibuprofen HCl CH Cl Diclofenac Cl H H CH H C 7 H 8 H C 9 Cl Meclofenamic acid H Cl Mefenamic acid CH H C H H H * H S Bendromethazide S H H C CH H

10 Complex Steroid Mixture Separation 0 C8-AR

11 C8-PFP : Halogenated Positional Isomers Chloroacetophenone halogenated isomers separation

12 Polar Analytes ucleosides & Vitas 00% Aqueous H C H + S H C Thiae or vita B H icotinamide H H H H H H L-Ascorbic acid or vita C C8-PFP, um, 0 x. mm Isocratic analysis Flow rate: ml/ Temperature: C Detection: UV nm Cytosine H Uracil H Mobile phase: 0 mm H P (aq) H H H Cytidine H Pyridoxae or Vita B H H CH H H H 7 8 H H Hypoxanthine 9 -Deoxycytidine H H H

13 Separation of Sulphonamides Excel C8-PFP μm, 0 x.mm Gradient analysis A = Water B = Acetonitrile C = 0% formic acid Time (s) %A %B %C Flow rate: ml/ Detection: UV, nm. Sulfadiazine. Sulfapyridine. Sulfamerazine. Sulfamoxole. Sulfamethazine. Sulfamonomethoxine 7. Sulfachloropyridazine 8. Sulfamethoxazole 9. Sulfadimethoxine Reproduced with permission of Antonio Martin Esteban, ational Research Institute of Agriculture and Food Technology IIA, Spain

14 Aspirin And Related Substances Excel C-ES Alternative selectivity with MeH containing eluents H H H H C H CH CH H H H C H CH H H C-ES 0x.mm, mm Gradient analysis Excel C A = 0.% formic acid B = 0.% FA in MeH 0 C 0. ml/ 0 nm 8% B in.7 s Hold at 8% B until s Excel C ,. -Acetamidophenol. Acetanilide. Salicylamide. Aspirin. Phenacetin. Salicylic acid

15 Small Pharmaceutically Relevant Analytes Excel C-ES Dipole + hydrophobic Interactions C-ES 00xmm, mm Gradient analysis Excel C8-Amide /.00 Polar embedded + hydrophobic Interactions A = 0mM ammonium formate (aq) B = 0mM ammonium formate in MeH 0C 0. ml/ T () %B Excel C8-PFP /.09 Hydrophobic + π-π + dipole + shape / position Interactions Hydrochlorothiazide. Methylphenylsulphoxide.,, Trinitrobenzene. Myricetin. P-Cresol. Sulindac 7. Toluene

16 Salicylic acid in cell extracts Extract from genetically engineered bacteria cells targeted analysis for salicylic acid UltraCore SuperC8, μm, 0 x.mm Gradient analysis (shown above) A = 0.% TFA in water B = 0.% TFA in acetonitrile Flow rate: ml/ Detection: UV, 0nm Reproduced with permission of Trong Khoa Pham, University of Sheffield, UK

17 USP Guaifenesin 7 Key: Guaifenesin Benzoic acid mau 0.0. UltraCore SuperC8,. μm, 0 x.0 mm Isocratic analysis H /MeH/Glacial acetic acid (0:0:. v/v) Flow rate: 0.8 ml/ Column temperature: Ambient ( C) Detection: UV at 7 nm Injection volume:. μl Translated method according to USP <> guidance. Always check the latest and official method information from the relevant pharmacopoeia prior to analysis.

18 USP Hydrocortisone 8 Key: Hydrocortisone Propylparaben Ultracore SuperC8,. μm, 00 x. mm Isocratic analysis MeC/MeH/H (::0 v/v) Flow rate: ml/ Column temperature: Ambient ( C) Detection: UV at nm Injection volume:.8 μl mau Translated method according to USP <> guidance. Always check the latest and official method information from the relevant pharmacopoeia prior to analysis.

19 USP Estradiol 9 Key: Ethylparaben Estrone Estradiol Ultracore SuperC8,. μm, 00 x. mm Isocratic analysis H /MeC (: v/v) Flow rate:.9 ml/ Column temperature: Ambient ( C) Detection: UV at 0 nm Injection volume: 0. μl mau Translated method according to USP <> guidance. Always check the latest and official method information from the relevant pharmacopoeia prior to analysis.

20 USP 7a-Ethinylestradiol 0 Key: Ethylparaben 7α-Ethinylestradiol Ultracore SuperC8,. μm, 0 x.0 mm Isocratic analysis MeC/H (0:0 v/v) Flow rate: 0. ml/ Column temperature: Ambient ( C) Detection: UV at 80 nm Injection volume:. μl mau Translated method according to USP <> guidance. Always check the latest and official method information from the relevant pharmacopoeia prior to analysis.

21 USP aproxen Key: aproxen Butyrophenone Ultracore SuperC8,. μm, 0 x.0 mm Isocratic analysis H with glacial acetic acid (9:)/MeC (0:0 v/v) Flow rate: 0. ml/ Column temperature: Ambient ( C) Detection: UV at nm Injection volume:.8 μl mau Translated method according to USP <> guidance. Always check the latest and official method information from the relevant pharmacopoeia prior to analysis.

22 USP Paracetamol / Aspirin / Caffeine Key: Paracetamol Caffeine Aspirin Benzoic acid Salicylic acid Ultracore SuperC8,. μm, 0 x. mm Isocratic analysis H with glacial acetic acid (9:)/MeH (7:8 v/v) Flow rate: ml/ Column temperature: C Detection: UV at 7 nm Injection volume:. μl mau Translated method according to USP <> guidance. Always check the latest and official method information from the relevant pharmacopoeia prior to analysis.

23 USP Hydroquinone Key: Hydroquinone Excel C8, μm, 0 x.0 mm Isocratic analysis H /MeH (: v/v) Flow rate: 0. ml/ Column temperature: Ambient ( C) Detection: UV at 80 nm Injection volume: 0.9 μl mau 0.0 H 80 H Translated method according to USP <> guidance. Always check the latest and official method information from the relevant pharmacopoeia prior to analysis.

24 USP Doxepin Key: Doxepin isomer Doxepin isomer mau 7. C8, μm, 0 x. mm Isocratic analysis 0. M Monobasic ah P in water ph.:meh (0:70 v/v) Flow rate: 0. ml/ Column temperature: 0 C Detection: UV at nm Injection volume:. μl 0.9 H C CH Translated method according to USP <> guidance. Always check the latest and official method information from the relevant pharmacopoeia prior to analysis.

25 USP Metronidazole Key: Metronidazole mau H CH.0 C8, μm, 7 x. mm Isocratic analysis H /MeH (: v/v) Flow rate.0 ml/ Column temperature: 0 C Detection: UV at 9 nm Injection volume: μl Translated method according to USP <> guidance. Always check the latest and official method information from the relevant pharmacopoeia prior to analysis.