Customer Service About Canadian Life Science Au suject de Canadian Life Science Founded in 1997, Canadian Life Science (CLS) has steadily grown Fondée en 1997, Canadian Life Science (CLS) n’a cessé de croître to Canada’s leading supplier of LC/GC columns, chromatography pour devenir un chef de file canadien dans la vente de colonnes and dissolution accessories as well as 2d long-term sample HPLC / GC, d’accessoires de chromatographie et dissolution, storage tubes and racks for bio-banking and compound ainsi que dans la vente de tubes et systèmes d’entreposage long management. terme pour échantillons. For over 22 years, CLS has provided customers with unparalleled Depuis plus de 22 ans, CLS offre à ses clients un service et service, expertise and a wide selection of quality and cost- une expertise inégalés, en plus d’un large éventail de produits effective products that offer maximum flexibility to solve your économiques de qualité offrant une flexibilité maximale afin de analytical challenges. CLS is your foundation for what matters. résoudre vos problèmes analytique. CLS est votre pilier pour ce qui compte. Everyone is accessible to you Nous sommes très accessible We believe that our customers like our personal touch. Nous avons une approche personnelle et nous répondons à tous We take your calls personally, not a computer, not voicemail . les appels lorsque vous téléphonez au bureau chef. Nous n’avons We have dedicated inside customer service staff who care, and pas de boîte vocale. take care for specific areas. We have knowledgeable outside staff Notre personnel est dévoué au service à la clientèle et ce à based in most of the larger cities accross Canada. travers le Canada. Si vous désirez parler directement à notre We supply world class products Directrice de comptes au Québec, vous pouvez contacter Canadian Life Science distributes for top-quality manufacturers. Genevieve Lemieux au 514.428.8034. Our product offering has been chosen in a way that will give you Nous choisissons les meilleurs produits au monde the maximum flexibility solving your analytical challenges. En tant que distributeur nous avons l’avantage de choisir les Technical Support meilleurs fournisseurs et notre gamme complète de produit vous Our technical staff is happy to respond to customer enquiries. donne l’embarras du choix. We can also supply extensive application information from one Support Technique of the world’s largest data bases. Notre équipe technique se fait toujours un plaisir de vous aider à Plan the best delivery faire le meilleur choix pour vos applications. When you decide to purchase a product from Canadian Life Service et logistique Science our customer service department will find the fastest Lorsque vous placez une commande chez nous, nous nous and most economical way to send your order to you. For assurons de choisir le moyen le plus efficace et économique your convenience we have two warehouse locations, one in d’acheminer la marchandise. Edmonton, AB and one in Peterborough, ON. Nous avons deux entrepôts dont un en Alberta pour servir nos We’re glad to help clients de l’Ouest et un en Ontario pour servir nos clients de l’Est. We are never too busy to take your call. C’est un plaisir de vous servir Try us. You’ll notice the difference. Nous ne sommes jamais trop occupés pour vous répondre. Canadian Life Science, friendly people to do business with! Essayez-nous et vous verrez la différence. Il est agréable de faire affaire avec nous! I-22 CANADIAN Proud member of the Chrom4 buying group Fier membre du groupe dʼacheteur Chrom4 LIFE SCIENCE 1 888-226-2775 :: [email protected] :: www.lifescience.ca
Contents Specifications....................................................................... 3 ACME C8................................................................................43 ACME Column Selection Guide.........................................4 ACME CN (Cyano)................................................................46 Applications.......................................................................... 5 ACME Ph (Phenyl)...............................................................48 Van Deemter......................................................................... 7 ACME PLUS ..........................................................................50 Stability Data - QC Standard.............................................8 ACME PAH............................................................................. 52 ACME C18................................................................................ 9 Preparative Columns......................................................... 53 ACME Cannabis................................................................... 16 Ordering Information....................................................... 55 ACME F5/C18 .......................................................................20 Compound List...................................................................60 ACME Amide/C18 ...............................................................29 ACME silica is based on a new 120 Å ultra-high purity (99.999%) extra-treated porous spherical silica with a narrow particle size distribution and an extremely low metal content (< 10 ppm) to minimize silanol acidity and reduce surface metal sites available for chelation. Our ACME PLUS and PAH silica is based on a new 200 Å version of the same silica. ACME silica is manufactured in a GMP environment under the most rigorously controlled conditions, ensuring lot-to-lot reproducibility, consistent particle size, pore volume and chemical purity. Combined with our proprietary bonding technology this results in columns with optimal efficiency, asymmetry, and minimal back pressure. ACME is available in several bonded phases covering a wide range of reversed-phase applications. • Available in several particle sizes for simple method transfer between HPLC and UHPLC • Ultrapure porous silica particles enable high peak efficiency across all particle sizes • Excellent column-to-column reproducibility • Compatible with HPLC and UHPLC hardware • Consistent and reproducible retention times to allow direct scale-up from the laboratory through process applications phaseanalytical.net ~2~
Specifications C18* F5/C18 Amide/C18 -C18H37 Bonded Phase -C18H37 –(CH2)3NH(C=O)-C15H37 16 –X-PFP Separation Mode Base Material Reversed-Phase Purity (%) Surface Area Ultrapure Extra-Treated Porous Spherical Silica Particle Size (s) * 99.999, metals < 10 ppm Pore Size 260 m2/g Carbon Load (%) Endcapping 1.9 µm, 3 µm, 5 µm pH Range 120 Å Temperature Limit Aqueous 16 19 Compatibility Yes proprietary USP Listing 1.8 to 9.5 60 °C ≤ 98% 100% 100% L1 L1/L43 L1/L60 * C18, C8 and PLUS 10 µm available for Prep columns PLUS* PAH C8* Ph CN** -R-CN Bonded Phase -C18H37 -(C18H37)x -C8H17 -R-C6H5 Separation Mode Reversed-Phase 7 Yes Base Material Ultrapure Extra-Treated Porous Spherical Silica proprietary Purity (%) 2 to 7.5 99.999, metals < 10 ppm 50 °C Surface Area 100% Particle Size (s) * 200 m2/g 260 m2/g L10 Pore Size 1.9 µm, 3 µm, 5 µm Carbon Load (%) 200 Å 120 Å Endcapping 12 17 10 10 pH Range Temperature Limit Yes No Yes Yes proprietary proprietary proprietary Aqueous Compatibility 1.8 to 9.5 1.8 to 9.5 1.8 to 9.5 1.8 to 9.5 USP Listing 60 °C 60 °C 60 °C 60 °C 100% ≤ 98% ≤ 98% 100% L1 L1 L7 L11 ACME CN** - Separation mode also Normal Phase * C18, C8 and PLUS 10 µm available for Prep columns phaseanalytical.net ~3~
ACME Column Selection Guide 1st Choice ACME C18 Alternate C18-like Retention with Aromatic / Olefinic Speed / Higher MW Selectivity Alternate Selectivity Isomers 2nd Choice ACME F5/C18 ACME Ph • Nitrogen containing analytes ACME PLUS • Geometric Isomers • Aromatic analytes • π-donor (Lewis base) analytes • Fast C18 Applications • pi-Acidic analytes • MWs too large for ACME C18 • Low Hydrophobicity ACME Amide/C18 ACME Cannabis 3rd Choice ACME C8 • H-bonding ACME PAH • Polar Analytes • Cannabinoids • H igher selectivity with • PAHs • C annabis related ACME CN polar analytes using low • Structural isomers, organic mobile phase compounds • HILIC e.g., Carotenoids • Low Hydrophobicity ACME Ph ACME F5/C18 ACME Amide/C18 ACME CN Selectivity ACME C8 ACME PAH ACME Cannabis ACME PLUS ACME C18 Hydrophobicity / Retention phaseanalytical.net ~4~
Applications Application Phase Particle Column Length Column ID Page # Analgesics / Aspirin Mix (Hydrophilic Acids) Size Amide/C18 3 100 4.6 36 Analgesics & Hydrophobic Acid Amide/C18 3 100 4.6 37 Aqueous Conditions Amide/C18 3 100 4.6 32, 33 3 100 2.1 19 Benzodiazepines C18 3 100 4.6 22 F5/C18 3 100 4.6 38 Benzoic Acid / Phenylacetic Acid Amide/C18 3 100 4.6 41 Beta Blockers Amide/C18 1.9 100 2.1 12 Bisphenols 3 100 2.1 42 C18 3 100 4.6 43 Caffeine Metabolites Amide/C18 3 150 4.6 16 3 50 2.1 50 Cannabinoids C8, C18 1.9 100 2.1 28 Cannabis 3 50 4.6 18 Clinical - VMA, HVA & 5-HIAA 1.9 100 2.1 14 Cortisones PLUS 3 100 4.6 25, 26 F5/C18 3 100 4.6 35 Diazepam Metabolites 3 100 4.6 47 Explosives C18 3 100 4.6 40 C18 3 100 4.6 20 Fat Soluble Vitamins F5/C18 3 100 4.6 21 Fluoxetine Metabolites Amide/C18 1.9 50 4.6 13, 37 CN 3 100 4.6 24, 32, 33 Hydrophobic Bases Amide/C18 1.9 50 2.1 15 Hydrophobic Retention F5/C18 5 150 4.6 9 F5/C18 3 100 4.6 48 Methoxy Isomers C18 3 100 4.6 23 NSAIDS / Diuretics F5/C18, Amide/C18 3 100 4.6 30 Nucleosides / Nucleotides C18 3 100 2.1 34 Paracetamol / Aspirin Mix C18 3 100 4.6 52 Ph 3 150 4.6 29 Phenols F5/C18 3 100 4.6 20 Amide/C18 3 100 4.6 48 Phenols & Carboxylic Acids Amide/C18 3 100 4.6 45 Polycyclic Aromatic Hydrocarbons PAH 3 100 4.6 11, 39, 44, 46, 49 Amide/C18 QA Test Mix F5/C18 3 100 4.6 31 Ph 3 100 4.6 10 Selectivity Analytes C8 3 100 4.6 51 THC Metabolites / Isocratic Amide/C18, C18, C8, CN, Ph 3 50 4.6 17 Tricyclic Antidepressants Amide/C18 Vanilla C18 PLUS Water Soluble Vitamins C18 Xanthines phaseanalytical.net ~5~
Technology through years of experience and innovation - Dr. William Campbell William Campbell received his Ph.D. in Chemistry at Montana State University under the direction of Dr. Wynn Jennings. Research included: 1. Transition metal catalysis mechanisms of Group VIII transition metals 2. Metabolism of toxic Furano-sesquiterpenes During his graduate work, Dr. Campbell gained a great deal of expertise in NMR, IR, Mass Spectroscopy and Chromatography. Dr. Campbell received a Post-Doctoral Fellowship at the University of Minnesota and continued working on organo-metallic mechanisms of Zirconocenes and Titanocenes, and organic and inorganic synthesis under the direction of Professor Paul Gassman. Dr. Campbell entered industry as a research chemist in Central Research at the Dow Corning Corporation. Through several years at Dow Corning he gained expertise in surface science and silicone and organo-silane chemistry. His love for chromatography coupled with his experience in silane chemistry lead to a career path in the development of HPLC stationary phases and applications. Early collaborations included: the Mayo Clinic, The University of Michigan Blood Chemistry Laboratory, WARS Analytical in Wisconsin and others. Dr. Campbell moved to ”Vydac” the Separations Group, where he further refined his skills in surface science, silica synthesis and evaluation, protein and peptide chromatographic techniques and development of preparative column technology. After a brief time at a startup company in Michigan, Dr. Campbell took a position at Supelco/Sigma-Aldrich as a Sr. Research Scientist and quickly moved to the position of HPLC R&D Manager. In that role he developed many new HPLC phase chemistries, presented seminars worldwide and worked closely with leading scientists in major pharmaceutical companies. Dr. Campbell is currently Adjunct Faculty for the Forensic Sciences Department and the Chemistry Department at Penn State University and the leading force behind Phase Analytical Technology. SP-180-5 P ACME silica is manufactured in a GMP environment under the most rigorously controlled conditions, Lot No. X170519WQP ensuring lot-to-lot reproducibility, consistent particle size, pore volume and chemical purity. 2.000 x 5.00 µm WD: 9.5mm 3kV 2017/10/04 phaseanalytical.net ~6~
Van Deemter Analysis H = A + Bu + Cu Van Deemter Analysis on a Pharmaceutical Compound. ACMVEanSiDliceaemPoterer AStnrualcytsuirse osnhoawPshdarrammaacteicuatlilcyailmCporomvpeodund. performAaCnMceEoSnilriecalPaonraelyStetrsu. cture shows dramatically improved performance on real analytes. O O CH3CH3 NN NN Cl Cl DiDaziaezpeapmam Diazepam Linear Velocity (mm/s) HH HH HH H H HH H H HH HH NaNphatphhatlhenaelene Naphthalene Linear Velocity (mm/s) phaseanalytical.net ~7~
Stability Data - QC Standard Retention time reproducibility and column stability are shown on the ACME column in the figure below. The figure compares the chromatograms shown from the 1st injection compared to the 500th injection on the ACME column. The efficiency and retention factors (k) for all four test compounds are the same, a characteristic essential for long and stable column lifetimes. ACME C18 Flow rate: 1.0 mL/min Sample: 5 µm, 50 x 4.6 mm Temperature: 25 °C 1. Uracil Detection: UV@265 nm 2. Benzophenone Isocratic Mobile Phase: Injection Vol.: 3 µL 3. Naphthalene Methanol:water, 80:20, (v/v) 4. Biphenyl 2 After 500 Injections N = 5810 s = 0.99 k = 2.94 3 4 1 First Injection N = 5815 s = 0.99 k = 2.93 phaseanalytical.net ~8~
ACME C18 Pore Size: 120 Å Carbon Content: 16% Usable pH Range: 1.8 to 9.5 USP Listing: L1 ACME C18 Flow rate: 1.0 mL/min 5 µm, 150 x 4.6 mm Temperature: 25 °C Detection: UV@270 nm Mobile Phase: Injection Vol.: 3 µL A: 0.1% formic acid in water, (v/v) B: 0.1% formic acid in acetonitrile, (v/v) Sample: 5. Methylparaben 1. Uracil 6. p-Nitrophenol Gradient: Profile 2. Resorcinol 7. p-Cresol AB 3. 4-Hydroxybenzaldehyde 8. 3,4-Dimethylphenol Time 75 25 4. Phenol 9. 2,6-Dimethylphenol (min) 30 70 Phenols 0 10 1. Uracil 2. Resorcinol 3. 4-Hydroxybenzaldehyde 4. Phenol 5. Methylparaben 6. p-Nitrophenol 6 7. p-Cresol 8. 3,4-Dimethylphenol 3 9 9. 2,6-Dimethylphenol 2 78 4 5 1 44.0 66.0 88.0 1100.0 1122.0 Time (min) 0 22.0 phaseanalytical.net ~9~
ACME C18 Pore Size: 120 Å Carbon Content: 16% Usable pH Range: 1.8 to 9.5 USP Listing: L1 ACME C18 Flow rate: 1.0 mL/min 3 µm, 100 x 4.6 mm Temperature: 25 °C Isocratic Mobile Phase: Detection: UV@225 nm A: 20 mM ammonium phosphate in water Injection Vol.: 5 µL B: Methanol A:B, (98:2, v/v) Sample: 1. p-Aminobenzoic acid (PABA) Water Soluble Vitamins 2. Pyridoxal 3. Pyridoxine (Vitamin B6) 4. Niacinamide (Nicotinamide, Vitamin B3) 1 1. p-Aminobenzoic acid (PABA) H OH O CH3 N OH 2. Pyridoxal 3 OH HO CH3 4 2 N OH 3. Pyridoxine ON NH2 4. Niacinamide 1.0 2.0 3.0 4.0 5.0 6.0 7.0 Time (min) phaseanalytical.net ~10~
ACME C18 Pore Size: 120 Å Carbon Content: 16% Usable pH Range: 1.8 to 9.5 USP Listing: L1 ACME C18 Flow rate: 1.5 mL/min O 3 µm, 100 x 4.6 mm Temperature: 35 °C Isocratic Mobile Phase: Detection: UV@254 nm CH3 A: 25 mM ammonium phosphate buffer (pH 7.0) Injection Vol.: 5 µL N B: Methanol A:B, (30:70, v/v) Sample: H 1. Nordoxepin Tricyclic Antidepressants 2. Desipramine 1. Nordoxepin 3. Nortriptyline 1 4. Doxepin NH 5. Imipramine N 6. Amitriptyline CH3 2. Desipramine H N CH3 3. Nortriptyline 2O CH3 N CH3 4. Doxepin 3 N CH3 4 N CH3 5 5. Imipramine 6 CH3 N CH3 6. Amitriptyline 1.0 2.0 3.0 4.0 5.0 6.0 7.0 Time (min) phaseanalytical.net ~11~
ACME C18 Pore Size: 120 Å Carbon Content: 16% Usable pH Range: 1.8 to 9.5 USP Listing: L1 ACME C18 Flow rate: 0.5 mL/min 1.9 µm, 100 x 2.1 mm Temperature: 35 °C Detection: UV@225 nm A. Water:25 mM ammonium phosphate (pH 7.0) Injection Vol.: 5 µL B: Methanol Gradient: Sample: 1. Atenolol Time Profile 2. Pindolol (min) AB 3. Acebutolol 75 25 4. Metaprolol 0 5. Propanolol 5 30 70 3 9 30 70 Beta Blockers 1. Atenolol 2. Pindolol 3. Acebutolol 5 4. Metaprolol 1 4 2 5. Propanolol 1.02 02.0 3.04 04.0 5.06 06.0 7.08 08.0 Time (min) phaseanalytical.net ~12~
ACME C18 Pore Size: 120 Å Carbon Content: 16% Usable pH Range: 1.8 to 9.5 USP Listing: L1 ACME C18 Flow rate: 1 mL/min 5. Ketoprofen 1.9 µm, 50 x 4.6 mm Temperature: 30 °C 6. Naproxen (Aleve) Mobile Phase: Detection: UV@230 nm 7. Diflunisal A: 0.1% formic acid in water, (v/v) Injection Vol.: 5 µL 8. Indomethacin B: 0.1% formic acid in acetonitrile, (v/v) 9. Ibuprofen (Advil) Sample: Gradient: 1. Hydrochlorothiazide 2. Acetylsalicylic Acid Time Profile (min) AB (ASA, Aspirin) 85 15 3. Furosemide 0 10 90 4. Piroxicam 5 NSAIDS/Diuretics 6 1. Hydrochlorothiazide 2. Acetylsalicylic Acid 3. Furosemide 4. Piroxicam 5. Ketoprofen 6. Naproxen 7 8 3 7. Diflunisal 8. Indomethacin 9. Ibuprofen 2 45 9 1 11..002 2..00 33..00044 4.0.0 55.0.06 066..00 Time (min) phaseanalytical.net ~13~
ACME C18 Pore Size: 120 Å Carbon Content: 16% ACME C18 Usable pH Range: 1.8 to 9.5 1.9 µm, 100 x 2.1 mm USP Listing: L1 Isocratic Mobile Phase: A: 0.1% formic acid in water Flow rate: 0.3 mL/min B: 0.1% formic acid in acetonitrile Temperature: 25 °C A:B, (60:40, v/v) Detection: UV@254 nm Injection Vol.: 1 µL Sample: 1. Oxazepam 2. Nordiazepam 3. Temazepam 4. Diazepam Diazepam Metabolites 1. Oxazepam 2. Nordiazepam 4 3. Temazepam 4. Diazepam 2 3 1 IMPURITY 1.02 02.0 3.04 04.0 5.06 06.0 7.0 Time (min) phaseanalytical.net ~14~
ACME C18 Pore Size: 120 Å Carbon Content: 16% ACME C18 Usable pH Range: 1.8 to 9.5 1.9 µm, 50 x 2.1 mm USP Listing: L1 Isocratic Mobile Phase: A: 0.1% formic acid in water Sample: B: Methanol 1. Acetaminophen (Paracetamol, Tylenol) A:B, (65:35, v/v) 2. Caffeine (1,3,7-Trimethylxanthine) Flow rate: 0.25 mL/min 3. Salicylamide (o-Hydroxybenzamide) Temperature: 22 °C 4. Acetylsalicylic Acid (ASA, Aspirin) Detection: UV@240 nm 5. Benzoic Acid Injection Vol.: 2 µL 6. Salicylic Acid Paracetamol / Aspirin Mix 1. Acetaminophen 2. Caffeine 3. Salicylamide 4. Acetylsalicylic Acid 5. Benzoic Acid 6. Salicylic Acid 3 5 4 12 6 1.02 02 .0 3.04 04 .0 5.06 06 .0 Time (min) phaseanalytical.net ~15~
ACME Cannabis Pore Size: 100 Å Carbon Content: 22% Usable pH Range: 1.8 to 9.5 USP Listing: L1 ACME Cannabis Sample: 7. Tetrahydrocannabivarin 3 µm, 150 x 4.6 mm 1. Cannabidivarinic Acid (THCV) (CBDVA) 8. Cannabinol (CBN) A: 0.1% Formic Acid in Water, (v/v) 2. Cannabidivarin (CBDV) 9. Δ9-tetrahydrocannabinol B: 0.095% Formic Acid in Acetonitrile, (v/v) 3. Cannabidiolic Acid (CBDA) (THC Δ9) 4. Cannabigerolic Acid (CBGA) 10. Δ8-tetrahydrocannabinol Gradient: 5. Cannabigerol (CBG) (THC Δ8) 6. Cannabidiol (CBD) 11. Cannabichromene (CBC) Time Profile (min) AB 0 30 70 10 10 90 15 10 90 Flow rate: 1.5 mL/min 4. CBGA 5. CBG 6. CBD Temperature: 25 °C Detection: UV@225 nm Injection Vol.: 2 μL Cannabinoids 7. THCV 8. CBN 9. THC Δ9 8 1. CBDVA 10. THC Δ8 11. CBC 11 2. CBDV 2 3 9 1 56 10 4 7 3. CBDA phaseanalytical.net ~16~
ACME C18 Pore Size: 120 Å Carbon Content: 16% ACME C18 Usable pH Range: 1.8 to 9.5 3 µm, 50 x 4.6 mm USP Listing: L1 Isocratic Mobile Phase: A: 1% formic acid in water Sample: B: Methanol 1. Theobromine (3,7-Dimethylxanthine) A:B, (85:15, v/v) 2. Paraxanthine (1,7-dimethylxanthine) 3. Theophylline (1,3-Dimethylxanthine) Flow rate: 1.0 mL/min 4. 1,3-dimethyl-7-(2-hydroxyethyl)-xanthine Temperature: 30 °C 5. Caffeine (1,3,7-Trimethylxanthine) Detection: UV@270 nm Injection Vol.: 2 µL 1. Theobromine 2. Paraxanthine Xanthines 3. Theophylline 4. 1,3-dimethyl-7- 3 (2-hydroxyethyl)xanthine 2 5. Caffeine 5 1 4 1.02 02.0 3.04 04.0 5.06 06.0 Time (min) phaseanalytical.net ~1 7 ~
ACME C18 Pore Size: 120 Å Carbon Content: 16% ACME C18 Usable pH Range: 1.8 to 9.5 3 µm, 50 x 4.6 mm USP Listing: L1 Isocratic Mobile Phase: Sample: 1. Hydrocortisone Acetonitrile: Water 1. Hydrocortisone (30:70, v/v) 2. Cortisone 2. Cortisone Flow rate: 1.5 mL/min 3. Corticosterone Temperature: 25 °C Detection: UV@220 nm Cortisones Injection Vol.: 3 µL 2 1 3. Corticosterone 3 1.0 2.0 3.0 4.0 Time (min ) 04 .0 Isocratic Mobile Phase: 3 Methanol: Water 1 (60:40, v/v) Flow rate: 1.0 mL/min 2 Temperature: 25 °C Detection: UV@220 nm Injection Vol.: 3 µL 1.02 02.0 3.04 Time (min) phaseanalytical.net ~18~
ACME C18 Pore Size: 120 Å Carbon Content: 16% Usable pH Range: 1.8 to 9.5 USP Listing: L1 ACME C18 Flow rate: 0.3 mL/min Sample: 3 µm, 100 x 2.1 mm Temperature: 25 °C 1. Chlordiazepoxide Mobile Phase: Detection: UV@254 nm 2. Nitrazepam A: 0.1% formic acid in water, (v/v) Injection Vol.: 1.5 µL 3. Oxazepam B: 0.1% formic acid in acetonitrile, (v/v) 4. Nordiazepam 5. Flunitrazepam Gradient: 6. Temazepam 7. Diazepam Time Profile 8. Prazepam (min) AB 75 25 0 25 75 10 Benzodiazepines 1 6 4 1. Chlordiazepoxide 2. Nitrazepam 3. Oxazepam 4. Nordiazepam 5. Flunitrazepam 6. Temazepam 7. Diazepam 8. Prazepam 5 2 3 7 8 1.02 02.0 3.04 04.0 5.06 06.0 7.08 08.0 9.0 10.0 Time (min) phaseanalytical.net ~19~
ACME F5/C18 Pore Size: 120 Å Carbon Content: 16% Usable pH Range: 1.8 to 9.5 USP Listing: L1 Bimodal phase combines C18 and PFP functional groups to increase selectivity in the separation of complex mixtures when compared to standard C18 phases alone. • Hydrophobic retention similar to C18 • PFP functionality provides alternate selectivity required for challenging applications Ap• plicFa5t/ioC1n8 Ecxaanmopplee:r Hatyedirnop1h0o0%bica Rqeuteeonutisocno AnCdMitiEo nFs5Ca1n8d vssh. oAwCsMiEm Cp1ro8v ed retention of polar compounds. ns: • Ultra-high purity (99.999%) extra-treated porous spherical silica, for excellent peak shape and reproducibility F5-C18, 3 µm, 100 x 4.6 mm ID C18, 3 µ•m , 1U00ltrxa4-.l6omwmblIeDed phase is suitable for use with UV and MS detection ic Mobile Phase: Sample: 1. Uracil nitrile:WaAAteCCrMM, (EE70FF:553/0/C,Cv11/88v,) 3 μm, 100 x 4.6 mm 2. Benzophenone ate: 1.5 mALC/MmEinC18, 3 μm, 100 x 4.6 mm erature: 2I5so°Ccratic Mobile Phase: 3. Naphthalene ion: UV @Ac2e6t5onnmitrile:Water, (70:30, v/v) 4. Biphenyl on Vol.: 3FµloLw rate: 1.5 mL/min e: Temperature: 25 °C 1. Uracil acil Detection: UV@265 nm nzophenoInnjeection Vol.: 3 μL phthalene henyl Hydrophobic Retention ACME F5/C18 vs. ACME C18 QA Test Mix ACMAECFM5/CE1 8F5-C18 NPe=ak1 5A,7s8y9mpmlaetterys = 1.05 2 4 2. Benzophenone 3 3. Naphthalene 1 4. Biphenyl 1.0 2.0 3.0 ACMAECCM18E C18 2 4 3 N = 15,617 plates Peak Asymmetry = 1.03 1 1.0 2.0 3.0 phaseanalytical.net ~20~
ACME F5/C18 Pore Size: 120 Å Carbon Content: 16% Usable pH Range: 1.8 to 9.5 USP Listing: L1 ACME F5/C18 Sample: ACME F5/C18, 3 μm, 100 x 4.6 mm 1. 1,2,4-Trimethoxybenzene ACME C18, 3 μm, 100 x 4.6 mm 2. 1,2-Dimethoxybenzene 3. 1,2,3-Trimethoxybenzene Isocratic Mobile Phase: 4. 1,4-Dimethoxybenzene Methanol:Water, (52:48, v/v) 5. Methoxybenzene Flow rate: 1.0 mL/min 6. 1,3-Dimethoxybenzene Temperature: 17 °C 7. 1,3,5-Trimethoxybenzene Detection: UV@254 nm Injection Vol.: 3 μL Methoxy Isomers ACME F5/C18 vs. ACME C18 AACCMMEEF F55/-CC1188 1 4 2 5 3 4 6 8 6 7 7. 1,3,5-Trimethoxybenzene 6. 1,3-Dimethoxybenzene 4 10 12 14 4 5. Methoxybenzene 12 14 0 2 AA CMCME EC 1C818 7 6 5 0 2 4 6 8 10 1. 1,2,4-Trimethoxybenzene 2. 1,2-Dimethoxybenzene 3. 1,2,3-Trimethoxybenzene 4. 1,4-Dimethoxybenzene phaseanalytical.net ~21~
ACME F5/C18 Pore Size: 120 Å Carbon Content: 16% Usable pH Range: 1.8 to 9.5 USP Listing: L1 ACME F5/C18 Sample: (elution order as per methanol conditions) 3 μm, 100 x 4.6 mm 1. 2,6-Dimethylphenol 2. Clonazepam HPLC Conditions 1: 3. Oxazepam Isocratic Mobile Phase: 4. Temazepam Methanol:Water, (55:45, v/v) Flow rate 1: 1.0 mL/min HPLC Conditions 2: Isocratic Mobile Phase: Acetonitrile:Water, (50:50, v/v) Flow rate 2: 1.5 mL/min Temperature: 25 °C Detection: UV@230 nm Injection Vol.: 3 μL Retention of Benzodiazepines – Methanol vs. Acetonitrile Mobile Phase: 1 1. 2,6-Dimethylphenol Methanol:Water, (55:45, v/v) 2. Clonazepam Flowrate: 1.0 mL/min 4 2 3 0 2 4 6 8 10 12 4 1 Mobile Phase: 3 2 Acetonitrile:Water, (50:50, v/v) Flowrate: 1.5 mL/min 3. Oxazepam 0 1.0 2.0 Structures 4. Temazepam 2,6-Dimethylphenol Clonazepam Oxazepam Temazepam phaseanalytical.net ~22~
Pore Size: 120 Å Carbon Content: 16% Columns: Usable pH Range: 1.8 to 9.5 USP Listing: L1 ACME F5-C18, 3 µm, 100 x 4.6 mm ID ACME CA18C, 3MµmE, 1F050 x/4C.61m8m ID Isocratic Mobile Phase: Methanol:Water, (45:55, v/v) Flow ratAeC: 1M.0EmF5L//Cm18in Sample: (elution order as per ACME C18) 1. 4-Methoxyphenol TemperAatCuMreE: 2F55/°CC18, 3 μm, 100 x 4.6 mm 2. Phenol DetectioAnC:MUEV C@182,543 nμmm, 100 x 4.6 mm 3. 4-Nitrophenol InjectionIsVooclr.:a3tiµcLMobile Phase: 4. 4-Methylphenol 21S..amP4p-hMleene:FMTo(telehoelmlotwuhxptiyaroepannrhtaoeeotl:nru:dW1or.eel0ar:tmae2s5rL,p/°(e4mCr5iA:n5C5M, vE/vC)18) 3. 4-NiDtroeptehcetniooln: UV@254 nm 4. 4-MeInthjeylcpthioennoVl ol.: 3 μL Retention of Polar Compounds (Phenols) ACME F5/C18 vs. ACME C18 2 AACMCME FE5 /FC51-8C18 1 4 3 2.0 3.0 4.0 5.0 6.0 7.0 2 3 1 4 1.0 AACMCME CE1 8C18 1.0 2.0 3.0 4.0 5.0 6.0 7.0 1. 4-Methoxyphenol 2. Phenol 2. 4-Nitrophenol 2. 4-Methylphenol phaseanalytical.net ~23~
Application Example: 100% Aqueous Conditions Column: Pore Size: 120 Å Carbon Content: 16% ACMAE CF5M-C1E8, 3Fµ5m/, 1C010 8x 4.6 mm ID Usable pH Range: 1.8 to 9.5 USP Listing: L1 Isocratic Mobile Phase: 25 mM Ammonium Acetate (pH 7.0) Flow rate: 1.5 mL / min TempAeCrMatEurFe5: /2C51°8C Sample: 3 μm, 100 x 4.6 mm 1. Cytosine 2. Uracil Detection: UV @ 254 nm 3. Cytidine 4. Hypoxanthine Isocratic Mobile Phase: 5. Thymine InjecBtiounffVeor:l2.:53mµLM Ammonium Acetate (pH 7.0) 6. Adenine SampFlleo:w rate: 1.5 mL/min 1. CTyetomsipneerature: 25 °C 2. UCHDIryynatpeijcdoetielixcncateitnoitohnninV:eoUlV.:@3 2μ5L4 nm 3. 4. 5. Thymine 6. A1d0e0n%ineAqueous Conditions Nucleosides & Nucleotides 1 ←Void Time = 0.62 min 2 5 4 3 6 0 2 4 6 8 10 1. Cytosine 2. Uracil 3. Cytidine 4. Hypoxanthine 5. Thymine 6. Adenine phaseanalytical.net ~24~
Isocratic Mobile Phase: Methanol:Water, (50:50, v/v) Pore Size: 120 Å Carbon Content: 16% Flow rate: 1.0 mL / min Usable pH Range: 1.8 to 9.5 USP Listing: L1 Temperature: 30 °C ACME F5/C18Detection: UV @ 254 nm Injection Vol.: 3 µL Sample: 1. HMX 2. R1,DA3X,C5-MTriEnitFro5b/eCn1z8ene Sample: 3. 1. HMX 2. RDX 4. 1,34-Dμimnit,ro1b0e0nzxe4ne.6 mm 3. 1,3,5-Trinitrobenzene 10. 4-Amino-2,6-Dinitrotoluene 4. 1,4-Dinitrobenzene 11. 2,4-Dinitrotoluene 5. 1,3-Dinitrobenzene 5. 1,3-Dinitrobenzene 12. 2-Nitrotoluene 6. Tetryl 13. 2,6-Ditrotoluene 6. TeItsryolcratic Mobile Phase: 7. Nitrobenzene 14. 4-Nitrobenzene 7. N3,Mi5tr-oDebitnehitnarozneanonelil:inWeater, (50:50, v/v) 8. 3,5-Dinitroaniline 15. 3-Nitrotoluene 8. 9. 2-Amino-4,6-Dinitrotoluene 9. 2-FAlmowinor-a4,t6e-D: i1n.i0tromtoLlu/emnein 10. 24-,T4Ae-mDmiinnpiotre-o2rt,o6a-ltuDueinrnieetr:o3to0lu°eCne 11. 12. 2-DNeitrtoetocltuieonne: UV@254 nm 13. 42-,I6Nn-iDtjreiotcrbotetionolzuneennVeeol.: 13. 3 μL 15. 3-Nitrotoluene Explosives 3 45 1 7 1. HMX 2 8 9 11 14 15 12 13 6 10 0 5 10 15 20 25 2. RDX 3. 1,3,5-Trinitrobenzene 4. 1,4-Dinitrobenzene 5. 1,3-Dinitrobenzene 6. Tetryl 7. Nitrobenzene 8. 3,5-Dinitroaniline 9. 2-Amino-4,6-Dinitrotoluene 10. 4-Amino-2,6-Dinitrotoluene 11. 2,4-Dinitrotoluene 12. 2-Nitrotoluene 13. 2,6-Ditrotoluene 14. 4-Nitrobenzene 15. 3-Nitrotoluene phaseanalytical.net ~25~
Time (min) A B 0 70 30 Pore Size: 120 Å Carbon Content: 16% 30 25 75 Usable pH Range: 1.8 to 9.5 ACME F5/C18 USP Listing: L1 Flow rate: 1.0 mL / min Temperature: 30 °C Detection: UV @ 215 nm ACME F5/C1In8jection Vol.: 3 µL Sample: 3 μm, 100 xSa4m.6pmle:m 1. HMX 10. 2-Amino-4,6-Dinitrotolu1e0n.e2-Amino-4,6-Dinitrotoluene 11. 42-,4A-mDiinniotr-o2t,o6-luDeinnietrotolue1n1e. 4-Amino-2,6-Dinitrotoluene 1. HMX 2. RDX 12. Mobile Pha2s.e:RDX 3. 1,3,5-Trinit1ro3.b2e-Nniztreontoeluene 12. 2,4-Dinitrotoluene A:Water, 3. 1,3,5-Trinitrobenzene 4. 1,4-Dinitro11b54e.. n42-,z6Ne-iDtnrioetrboetonlzueennee 13. 2-Nitrotoluene 4. 1,4-Dinitrobenzene 5. 1,3-Dinitro1b6e. n3-zNeitnroetoluene 14. 2,6-Ditrotoluene B:Methano5l . 1,3-Dinitrobenzene Gradient: 6. Tetryl 6. Tetryl 17. PETN 15. 4-Nitrobenzene 7. Nitrobenzene 8. Nitroglycerin 7. Nitrobenzene 16. 3-Nitrotoluene Time 9. 3P,r5o-Dfiinleitroaniline 8. Nitroglycerin 17. PETN (min) A B 9. 3,5-Dinitroaniline 0 70 30 3 30 25 75 1 Flow rate: 1.0 mL/min 9 10 13 16 Temperature: 30 °C Detection: UV@215 nm 7 14 15 1. HMX Injection Vol.: 3 μL 2 45 2. RDX 11 25 Explosives 12 6 8 17 05 10 15 20 3. 1,3,5-Trinitrobenzene 4. 1,4-Dinitrobenzene 5. 1,3-Dinitrobenzene 6. Tetryl 7. Nitrobenzene 8. Nitroglycerin 9. 3,5-Dinitroaniline 10. 2-Amino-4,6-Dinitrotoluene 11. 4-Amino-2,6-Dinitrotoluene 12. 2,4-Dinitrotoluene 13. 2-Nitrotoluene 14. 2,6-Ditrotoluene 15. 4-Nitrobenzene 16. 3-Nitrotoluene 17. PETN phaseanalytical.net ~26~
ACME F5/C18 Pore Size: 120 Å Carbon Content: 16% Usable pH Range: 1.8 to 9.5 USP Listing: L1 ACME F5/C18 Sample: 8. Verapamil ACME F5/C18, 3 µm, 100 x 4.6 mm 1. Uracil 9. Propranolol ACME PLUS, 3 µm, 100 x 4.6 mm 2. Adenine 10. Oxazepam 3. Atenolol 11. Fentanyl Mobile Phase: 4. Pindolol 12. Tolbutamide A: 25 mM Ammonium Formate in water 5. Codeine 13. Diazepam B: Acetonitrile 6. Norfentanyl 14. Δ9-Tetrahydrocannabinol 7. Acebutolol Gradient: 7 Time Profile (min) AB 0 100 0 ACME PLUS 10 35 65 11 10 90 15 10 90 Drug Mix 1 - ACME F5/C18 vs. ACME PLUS 3 5 Flow rate: 1.5 mL/min 13 Temperature: 25 °C Detection: UV@245 nm 2 Injection Vol.: 3 µL 1 8 10 12 9 11 4 6 14 7 1. Uracil 2. Adenine 3. Atenolol ACAMCEMFE5 F/5CC1188 13 3 5 2 10 8 4. Pindolol 5. Codeine 6. Norfentanyl 6 4 1 9 12 11 14 7. Acebutolol 8. Verapamil 9. Propranolol 10. Oxazepam 11. Fentanyl 12. Tolbutamide 13. Diazepam 14. Δ9-Tetrahydrocannabinol phaseanalytical.net ~27~
ACME F5/C18 Pore Size: 120 Å Carbon Content: 16% Usable pH Range: 1.8 to 9.5 USP Listing: L1 ACME F5/C18 Flow rate: 0.3 mL/min 1 .9 µm, 100 x 2.1 mm Temperature: 25 °C Detection: UV@245 nm Mobile Phase: Injection Vol.: 0.5 µL Mobile Phase A: 0.1% formic acid in water, (v/v) Mobile Phase B: 0.1% formic acid in acetonitrile, (v/v) Gradient: Sample: 1. Vanillylmandelic Acid (VMA) Time Profile 2. Homovanillic Acid (HVA) (min) AB 3. 5-Hydroxyindoleacetic Acid (5-HIAA) 100 0 0 60 40 10.0 Clinical Application Vanillylmandelic acid (VMA) and Homovanillic acid (HVA) and Hydroxyindoleacetic acid (5-HIAA) 23 1 phaseanalytical.net ~28~
ACME Amide/C18 Pore Size: 120 Å Carbon Content: 19% Usable pH Range: 1.8 to 9.5 USP Listing: L1/L60 Bimodal phase combines C18 and an embedded Amide functional group to increase selectivity in the separation of complex mixtures when compared to standard C18 phases alone. • Hydrophobic retention similar to C18 • Amide functionality provides alternate selectivity required for challenging applications • Amide/C18 can operate in 100% aqueous conditions and shows improved retention of polar compounds. • Ultra-high purity (99.999%) extra-treated porous spherical silica, for excellent peak shape and reproducibility • Ultra-low bleed phase is suitable for use with UV and MS detection • Similar retention window with ACME C18 ACME Amide/C18 Sample: Excellent Efficiency ACME Amide/C18, 3 μm, 150 x 4.6 mm 1. Uracil Excellent Peak Shape ACME C18, 3 μm, 150 x 4.6 mm 2. Benzophenone 3. Naphthalene 4 Isocratic Mobile Phase: 4. Biphenyl N = 23,893 plates Acetonitrile:Water, (65:35, v/v) Peak Asymmetry = 1.01 Flow rate: 1.5 mL/min 2 Temperature: 25 °C Detection: UV@265 nm Injection Vol.: 3 μL QA Test Mix ACME Amide/C18 vs ACME C18 ACME Amide/C18 3 1 1. Uracil 2. Benzophenone ACME C18 2 4 1 3 N = 23,412 plates Peak Asymmetry = 1.07 3. Naphthalene 4. Biphenyl phaseanalytical.net ~29~
ACME Amide/C18 Pore Size: 120 Å Carbon Content: 19% ACME Amide/C18 Sample: Usable pH Range: 1.8 to 9.5 ACME Amide/C18, 3 μm, 100 x 4.6 mm 1. 4-Methoxyphenol USP Listing: L1/L60 ACME C18, 3 μm, 100 x 4.6 mm 2. Phenol 3. 4-Nitrophenol 1. 4-Methoxyphenol Isocratic Mobile Phase: 4. 4-Methylphenol Acetonitrile: 0.1% Formic Acid in Water, 2. Phenol (35:65, v/v) Flow rate: 1.5 mL/min Temperature: 25 °C Detection: UV@225 nm Injection Vol.: 3 μL 4-Phenols Mix (Weak Acids) ACME Amide/C18 vs ACME C18 ACME Amide/C18 2 1 3 4 ACME C18 2 14 3. 4-Nitrophenol 3 4. 4-Methylphenol phaseanalytical.net ~30~
ACME Amide/C18 Pore Size: 120 Å Carbon Content: 19% Usable pH Range: 1.8 to 9.5 USP Listing: L1/L60 ACME Amide/C18 Sample: 1. Vanillic Acid ACME Amide/C18, 3 μm, 100 x 4.6 mm 1. Vanillic Acid 2. Vanillin ACME C18, 3 μm, 100 x 4.6 mm 2. Vanillin 3. 4-Hydroxybenzoic Acid 3. 4-Hydroxybenzoic Acid Isocratic Mobile Phase: 4. 4-Hydroxybenzaldehyde 4. 4-Hydroxybenzaldehyde Acetonitrile:Water, (20:80, v/v) 5. Guaiacol Flow rate: 1.5 mL/min 6. Ethylvanillin Temperature: 25 °C 7. Benzoic Acid Detection: UV@220 nm Injection Vol.: 3 μL Vanilla Test Mix ACME Amide/C18 vs ACME C18 showing radically alternate selectivity 3 ACME Amide/C18 1 7 2 6 4 5 3 ACME C18 2 7 1 6 4 5 5. Guaiacol 6. Ethylvanillin 7. Benzoic Acid phaseanalytical.net ~31~
ACME Amide/C18 Pore Size: 120 Å Carbon Content: 19% ACME Amide/C18 Sample: Usable pH Range: 1.8 to 9.5 3 μm, 100 x 4.6 mm 1. Cytosine USP Listing: L1/L60 2. Uracil Isocratic Mobile Phase: 3. Cytidine 6 25 mM Ammonium Formate in Water 4. Hypoxanthine Flow rate: 1.5 mL/min 5. Thymine Temperature: 25 °C 6. Adenine Detection: UV@254 nm Injection Vol.: 3 μL 100% Aqueous Conditions Nucelosides & Nucleotides 1 2 5 3 4 Void Time = 0.62 min 1. Cytosine 2. Uracil 3. Cytidine 4. Hypoxanthine 5. Thymine 6. Adenine phaseanalytical.net ~32~
ACME Amide/C18 Pore Size: 120 Å Carbon Content: 19% Usable pH Range: 1.8 to 9.5 USP Listing: L1/L60 ACME Amide/C18 Sample: 3 μm, 100 x 4.6 mm 1. Cytosine 2. Uracil Isocratic Mobile Phase: 3. Cytidine 25 mM Ammonium Formate in Water 4. Hypoxanthine Flow rate: 1.5 mL/min 5. Thymine Temperature: 25 °C 6. Adenine Detection: UV@254 nm Injection Vol.: 3 μL Standard C18 phases normally show phase dewetting leading to loss of retention in 100% aqueous mobile phases with time. This phenomenon Aqueous Compatibility causes loss of retention from one injection to the next and will show total Nucelosides & Nucleotides collapse of the separation upon flow stop/start cycles. The ACME Amide shows complete stability in 100% aqueous conditions with no loss of 1 retention even after flow stop/start cycles. 2 5 3 4 6 Tenth Injection After Stop/Start First Injection After Stop/Start Tenth Injection First Injection 1. Cytosine 2. Uracil 3. Cytidine 4. Hypoxanthine 5. Thymine 6. Adenine phaseanalytical.net ~33~
ACME Amide/C18 Pore Size: 120 Å Carbon Content: 19% Usable pH Range: 1.8 to 9.5 USP Listing: L1/L60 ACME Amide/C18 Sample: ACME Amide/C18, 3 μm, 100 x 2.1 mm 1. Void marker ACME C18, 3 μm, 100 x 2.1 mm 2. Resorcinol 3. 4-Methoxyphenol Isocratic Mobile Phase: 4. Phenol Acetonitrile:Water:Formic Acid, (30:70:0.1, v/v/v) 5. 4-Methoxybenzoic Acid Flow rate: 0.3 mL/min 6. 4-Methylphenol Temperature: 25 °C 7. 4-Methylbenzoic Acid Detection: UV@254 nm 8. 4-Nitrophenol Injection Vol.: 3 μL 9. 3,4-Dimethylphenol Phenols and Carboxylic Acids Dramatically enhanced retention and selectivity is noted on the Amide/C18 for phenolic and carboxylic acid analytes. This can be particularly important in analysis of drug metabolites and similar analyses. ACME C18 3 2 8 9 1 46 5 7 OH 2 3 OH OH OH OH OH O CH3 O OH ACME Amide/C18 CH3 O- N+ CH3 1 OH 6 O CH3 4 CH3 8 9 HO O 7 5 O CH3 phaseanalytical.net ~34~
ACME Amide/C18 Pore Size: 120 Å Carbon Content: 19% ACME Amide/C18 Usable pH Range: 1.8 to 9.5 3 μm, 100 x 4.6 mm USP Listing: L1/L60 Isocratic Mobile Phase: Methanol:Water, (97:3, v/v) Sample: Flow rate: 1.5 mL/min 1. Void marker Temperature: 25 °C 2. Vitamin A Detection: UV@240 nm 3. Vitamin D2 Injection Vol.: 5 μL 4. Vitamin D3 5. Vitamin E Fat Soluble Vitamins 6. Vitamin K Lipophilic analytes show reduced retention, but very good selectivity on the ACME Amide/C18. ACME Amide/C18 5 2. Vitamin A 3. Vitamin D2 2 5. Vitamin E 4 4. Vitamin D3 6. Vitamin K 1 3 6 ACME C18 2 5 1 6 4 3 phaseanalytical.net ~35~
ACME Amide/C18 Pore Size: 120 Å Carbon Content: 19% Usable pH Range: 1.8 to 9.5 USP Listing: L1/L60 ACME Amide/C18 Sample: 3 μm, 100 x 4.6 mm 1. Acetaminophen (Paracetamol, Tylenol) 2. Salicylamide (o-Hydroxybenzamide) Isocratic Mobile Phase: 3. Aspirin (acetylsalicylic acid) Acetonitrile: 0.1% Formic Acid in Water (v/v), (30:70, v/v) 4. Benzoic Acid Flow rate: 1.5 mL/min Temperature: 25 °C Detection: UV@240 nm Injection Vol.: 5 μL Analgesics – Aspirin Mix (Hydrophilic Acids) Enhanced retention and selectivity is noted on the Amide/C18 for phenols and carboxylic acid analytes. ACME Amide/C18 13 4 2 ACME C18 1 4 3 2 phaseanalytical.net ~36~
ACME Amide/C18 Pore Size: 120 Å Carbon Content: 19% Usable pH Range: 1.8 to 9.5 USP Listing: L1/L60 ACME Amide/C18 Sample: ACME Amide/C18, 3 μm, 100 x 4.6 mm 1. Acetylsalicylic Acid (ASA, Aspirin) ACME C18, 3 μm, 100 x 4.6 mm 2. Piroxicam 3. Ketoprofen Isocratic Mobile Phase: 4. Naproxen (Aleve) Acetonitrile: 0.1% Formic Acid in Water (v/v), (50:50, v/v) 5. Indomethacin Flow rate: 1.5 mL/min 6. Ibuprofen (Advil) Temperature: 25 °C Detection: UV@225 nm Injection Vol.: 5 μL Analgesics – NSAIDS (Hydrophobic Acids) 1 N O OH NH OO H N H 3C S OO ACME Amide/C18 OC H 3 2 CH 3 O O HO O O Cl N H 3C O CH 3 CH 3 HO HO 3 5 O O CH 3 O CH 3 CH 3 CH 3 HO 4 O 6 1 ACME C18 2 5 3 6 4 phaseanalytical.net ~37~
ACME Amide/C18 Pore Size: 120 Å Carbon Content: 19% Usable pH Range: 1.8 to 9.5 USP Listing: L1/L60 ACME Amide/C18 Sample: ACME Amide/C18, 5 μm, 150 x 4.6 mm 1. Alprazolam ACME C18, 5 μm, 150 x 4.6 mm 2. Oxazepam 3. Flunitrazepam Isocratic Mobile Phase: 4. Diazepam Acetonitrile: 0.1% Formic Acid in Water (v/v), (40:60, v/v) Flow rate: 1.5 mL/min Temperature: 25 °C Detection: UV@254 nm Injection Vol.: 8 μL Benzodiazepines Selectivity reversal is often a powerful attribute of the Amide/C18. Here the more polar Oxazepam is preferentially retained on the Amide/C18 verses a standard C18 chemistry. Diazepam shows shorter retention on the Amide/C18 to bring the complete separation into a shorter retention window. ACME Amide/C18 1 3 2 4 3 ACME C18 1 4 2 Peak Order Reversal phaseanalytical.net ~38~
ACME Amide/C18 Pore Size: 120 Å Carbon Content: 19% Usable pH Range: 1.8 to 9.5 USP Listing: L1/L60 ACME Amide/C18 Sample: 3 μm, 100 x 4.6 mm 1. Nordoxepin 2. Desipramine Isocratic Mobile Phase: 3. Doxepin Methanol:20mM Ammonium Phosphate 4. Imipramine (Monobasic), (52:48, v/v) Flow rate: 1.0 mL/min Temperature: 30 °C Detection: UV@254 nm Injection Vol.: 5 μL Tricyclic Antidepressants The Amide/C18 shows exceptional peak shape on hydrophobic basic molecules. These typically show dramatic tailing with most C18s on the market. In this example we see peak asymmetry values of less than 1.5. N H 12 N CH 3 O O CH 3 4 N CH 3 N CH 3 H 3 ACME Amide/C18 N CH 3 N CH 3 phaseanalytical.net ~39~
ACME Amide/C18 Pore Size: 120 Å Carbon Content: 19% Usable pH Range: 1.8 to 9.5 USP Listing: L1/L60 ACME Amide/C18 Sample: 3 μm, 100 x 4.6 mm 1. Diphenhydramine 2. Norfluoxetine Isocratic Mobile Phase: 3. Fluoxetine Methanol:20mM Ammonium Phosphate (Monobasic), (58:42, v/v) Flow rate: 1.0 mL/min Temperature: 30 °C Detection: UV@254 nm Injection Vol.: 5 μL Hydrophobic Bases The Amide/C18 shows exceptional peak shape on hydrophobic basic molecules. These typically show dramatic tailing with most C18s on the market. In this example we see peak asymmetry values of less than 1.5. 1 3 2 phaseanalytical.net ~40~
ACME Amide/C18 Pore Size: 120 Å Carbon Content: 19% ACME Amide/C18 Usable pH Range: 1.8 to 9.5 3 μm, 100 x 4.6 mm USP Listing: L1/L60 Isocratic Mobile Phase: Acetonitrile: 0.1% Formic Acid in Water Sample: (v/v), (30:70, v/v) 1. Phenylacetic Acid, pKa = 4.3 Flow rate: 1.5 mL/min 2. Benzoic Acid, pKa = 4.2 Temperature: 25 °C Detection: UV@230 nm O 2 O OH Injection Vol.: 5 μL OH Benzoic Acid / Phenylacetic Acid Retention on the Amide/C18 is stronger due to the ACME Amide/C18 1 combination of the C18 and the amide group. The stronger acid retains longer on the Amide/C18 when compared to the ACME C18. 2 O OH Retention due to hydrophobicity alone. ACME C18 O 1 OH phaseanalytical.net ~41~
ACME Amide/C18 Pore Size: 120 Å Carbon Content: 19% Usable pH Range: 1.8 to 9.5 USP Listing: L1/L60 ACME Amide/C18 Sample: 7. Bisphenol AP 3 μm, 100 x 2.1 mm 1. Void Marker 8. Bisphenol C2 2. Bisphenol S 9. Bisphenol AF Mobile Phase: 3. Bisphenol F 10. Bisphenol M A: 0.1% Formic Acid in Water, (v/v) 4. Bisphenol E 11. Bisphenol P B: 0.085% Formic Acid in Acetonitrile, (v/v) 5. Bisphenol A 12. Bisphenol TC 6. Bisphenol B Gradient: CH3 3. Bisphenol F Time Profile HO OH (min) AB CH3 HO OH 4. Bisphenol E 0.0 60 40 CH3 CH3 15.0 25 75 2. Bisphenol S HO OH 6. Bisphenol B Flow rate: 0.4 mL/min 5. Bisphenol A 7. Bisphenol AP Temperature: 25 °C Detection: UV@230 nm Injection Vol.: 5 μL 8. Bisphenol C2 9. Bisphenol AF 10. Bisphenol M Bisphenols HO H3C CH3 CH3 HO 3 H3C CH3 CH3 H3C OH HO 11. Bisphenol P 12. Bisphenol TC 10 2 6 4 11 12 15 9 7 8 phaseanalytical.net ~42~
ACME C8 Pore Size: 120 Å Carbon Content: 10% Usable pH Range: 1.8 to 9.5 USP Listing: L7 ACME C8 Sample: 3 µm, 100 x 4.6 mm 1. Theobromine (3,7-Dimethylxanthine) 2. Paraxanthine (1,7-dimethylxanthine) Isocratic Mobile Phase: 3. Theophylline (1,3-Dimethylxanthine) A: 0.1% formic acid in water 4. 1,3-Dimethyl-7-(2-hydroxyethyl)xanthine B: Methanol 5. Caffeine (1,3,7-Trimethylxanthine) A:B, (80:20, v/v) Caffeine Metabolites Flow rate: 1.0 mL/min Temperature: 30 °C 1. Theobromine 2. Paraxanthine Detection: UV@270 nm Injection Vol.: 2 µL 3 2 3. Theophylline 4. 1,3-dimethyl-7- (2-hydroxyethyl)xanthine 5 1 ACME C8 4 5. Caffeine 3 5 2 1 4 ACME C18 phaseanalytical.net ~43~
ACME C8 Pore Size: 120 Å Carbon Content: 10% ACME C8 Sample: Usable pH Range: 1.8 to 9.5 3 µm, 100 x 4.6 mm 1. Nordoxepin USP Listing: L7 2. Desipramine Isocratic Mobile Phase: 3. Nortriptyline 1. Nordoxepin A: 25 mM ammonium phosphate buffer 4. Doxepin (pH 7.0) 5. Imipramine 2. Desipramine B: Methanol 6. Amitriptyline A:B, (35:65, v/v) 3. Nortriptyline Flow rate: 1.5 mL/min Temperature: 35 °C Detection: UV@254 nm Injection Vol.: 2 µL Tricyclic Antidepressants 1 ACME C8 23 65% Methanol 4 6 5 ACME C18 4. Doxepin 70% Methanol 5. Imipramine 6. Amitriptyline 1 2 3 4 5 6 1.0 2.0 3.0 4.0 5.0 6.0 7.0 Time (min) phaseanalytical.net ~44~
ACME C8 Pore Size: 120 Å Carbon Content: 10% Usable pH Range: 1.8 to 9.5 USP Listing: L7 ACME C8 Sample: 3 µm, 100 x 4.6 mm 1. 11-Nor-9-carboxy-Δ9-tetrahydrocannabinol Isocratic Mobile Phase: (11-COOH-THC, THC-COOH) A: 0.1% formic acid in water, (v/v) 2. 11-Hydroxy-Δ9-tetrahydrocannabinol B: 0.1% formic acid in methanol, (v/v) A:B, (20:80, v/v) (11-Hydroxy-THC , 11-OH-THC) 3. Δ9-Tetrahydrocannabinol (THC) Flow rate: 1.0 mL/min 1. 11-COOH-THC Temperature: 25 °C Detection: UV@220 nm THC Metabolites / Isocratic Injection Vol.: 2 µL 2 3 ACME C8 1 2. 11-Hydroxy-THC 2 3. Δ9-Tetrahydrocannabinol (THC) 1 THC elutes ACME C18 much later phaseanalytical.net ~45~
ACME CN (Cyano) Pore Size: 120 Å Carbon Content: 7% Usable pH Range: 2 to 7.5 USP Listing: L10 ACME CN Sample: 3 µm, 100 x 4.6 mm 1. Nordoxepin 2. Desipramine Isocratic Mobile Phase: 3. Doxepin A: 100 mM ammonium acetate in water 4. Imipramine B: Acetonitrile A:B, (10:90, v/v) O Flow rate: 1.5 mL/min CH3 Temperature: 30 °C N Detection: UV@245 nm Injection Vol.: 5 µL H Tricyclic Antidepressants 1. Nordoxepin under HILIC conditions NH 1 N CH3 3 2. Desipramine 2 4 O CH3 N CH3 3. Doxepin N CH3 N CH3 4. Imipramine phaseanalytical.net ~46~
ACME CN (Cyano) Pore Size: 120 Å Carbon Content: 7% Usable pH Range: 2 to 7.5 USP Listing: L10 ACME CN Sample: 3 µm, 100 x 4.6 mm 1. Norfluoxetine Isocratic Mobile Phase 2. Fluoxetine Flow rate: 1.5 mL/min Temperature: 30 °C Fluoxetine and Metabolite Detection: UV@230 nm Injection Vol.: 2 µL HILIC Mode: Acetonitrile:100 mM ammonium Reversed Phase Mode: acetate in water, (90:10, v/v) Acetonitrile:25 mM ammonium phosphate in water, (45:55, v/v) 1 1 2 1. Norfluoxetine 2. Fluoxetine 2 phaseanalytical.net ~47~
ACME Ph (Phenyl) Pore Size: 120 Å Carbon Content: 10% Usable pH Range: 1.8 to 9.5 USP Listing: L11 ACME Ph 3 Phenols 3 µm, 100 x 4.6 mm 2 45 Isocratic Mobile Phase: 6 A: 0.1% formic acid in water, (v/v) B: 0.1% formic acid in methanol, (v/v) 7 A:B, (75:25, v/v) 1 Flow rate: 1.0 mL/min ACME Ph 8 9 Temperature: 25 °C ACME C18 Detection: UV@270 nm 3 6 Injection Vol.: 3 µL 2 Sample: 45 1. Uracil 2. Resorcinol 17 3. 4-Hydroxybenzaldehyde 4. Phenol 8 9 5. Methylparaben 6. p-Nitrophenol 7. p-Cresol 8. 3,4-Dimethylphenol 9. 2,6-Dimethylphenol ACME Ph Selectivity Analytes 3 µm, 100 x 4.6 mm 4 3 Isocratic Mobile Phase: A: Water 2 3. Trinitrobenzene B: Acetonitrile 1 A:B, (50:50, v/v) 4 1. Ethyl paraben Flow rate: 1.5 mL/min 4. Anisole Temperature: 25 °C ACME Ph Detection: UV@220 nm Injection Vol.: 5 µL 3 Sample: 2. Acetophenone 2 1. Ethylparaben ACME C18 1 2. Acetophenone 3. Trinitrobenzene 4. Anisole phaseanalytical.net ~48~
ACME Ph (Phenyl) Pore Size: 120 Å Carbon Content: 10% Usable pH Range: 1.8 to 9.5 USP Listing: L11 ACME Ph Flow rate: 1.5 mL/min Sample: 4. Doxepin 1. Nordoxepin 5. Imipramine 3 µm, 100 x 4.6 mm Temperature: 35 °C 2. Desipramine 6. Amitriptyline 3. Nortriptyline Isocratic Mobile Phase: Detection: UV@254 nm A: 25 mM ammonium phosphate buffer Injection Vol.: 2 µL (pH 7.0) B: Methanol A:B, (30:70, v/v) Tricyclic Antidepressants 1 23 ACME Ph 46 5 Nor-Methyl Analytes 4 N-Methyl Analytes 12 56 3 ACME C18 The more polar analytes show enhanced retention on the ACME Phenyl while the less polar analytes show decreased retention. This has the advantage of bringing separations of mixed analyte systems into a smaller separation window. phaseanalytical.net ~49~
ACME PLUS Pore Size: 200 Å Carbon Content: 12% ACME PLUS Usable pH Range: 1.8 to 9.5 3 µm, 50 x 2.1 mm USP Listing: L1 Isocratic Mobile Phase: Methanol: Water, (83:17, v/v) Sample: Flow rate: 0.5 mL/min 1. Cannabidiol (CBD) Temperature: 25 °C 2. Cannabichromene (CBC) Detection: UV@215 nm 3. Δ8-Tetrahydrocannabinol (THC-Δ8) Injection Vol.: 0.5 µL 4. Δ9-Tetrahydrocannabinol (THC-Δ9) 5. Cannabinol (CBN) Fast Cannabinoids 1. CBD 2. CBC 1 3. THC Δ8 4. THC Δ9 2 3 5. CBN 4 5 1.02 02.0 3.0 Time (min) phaseanalytical.net ~50~
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