Introducition of a new product from Inertsil Series

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2 Introducition of a new product from Inertsil Series is a C8 column developed focusing on superb inertness to basic, acidic, neutral and chelating compounds, which can virtually provide perfect peak shapes for any type of compounds. Physical Properties Silica Purity Particle Size Surface Area Pore Volume Pore Size Bonded Phase End-capping Carbon Loading USP Code : High Purity Spherical Silica Gel : % : 5um : 450 m/g : 00A :.05 ml/g : Octadecyl groups : Yes : % : L

3 Concept of Absolute Inertness for Most Critical Analyses Demands from the market for; analyzing wide variety of compounds because, increase in candidate drug compounds & addition of legally controlled compounds in Environment & Food industry. compounds that were analyzed by GC are now being analyzed by LC as well. high sensitivity because the adsorption of trace amount of compounds causes a problem. change in mobile phase additives due to expanded use of LC/MS which requires symmetrical peak shapes without adding any strong acids (ex. phosphoric acids or highly-concentrated buffers)

4 Pursuit of the Inertness To meet all the requirements, make the packing Inhibit adsorption of basic compounds by deactivating the silanol groups. Inhibit adsorption of acidic compounds by introducing a neutral functional groups. Inhibit adsorption of chelating compounds by adopting a highly pure silica gels. The Highest Inertness has been achieved on silica base HPLC columns for any type of compounds. by

5 Comparison of theorical plate of naphthalene between and commercially ODS columns High theorical plate ) Naphthalene N= ,000/m N = 5,04 Assy. =.06 N = 4,9 Assy. = N = 4,69 Assy. = L-Column ODS N =,667 Assy. = Capcell Pak C8 MGⅢ Conditions Column: 4.6 mm I.D x 50 mm length,5μm Mobile phase: Acetonitrile : HO = 65 : 5 Flow rate: ml / min Column temperature: 5 Detection: UV 54 nm Sample: μl (naphthalene mg/ml) Atlantis T (Waters) Naphthalene (Neutral compound)

6 Highly Pure Base Silica-gel Completely spherical Smooth surface Synthesized from pure ingredients Focused only for chromatography Whole manufacturing process within GLS Inertsil Silica-gel One competitor's Silica-gel

7 Back pressure of commercially available columns Low Column Back Pressure Analytical Conditions Pressure (kgf/cm) :Inertsil ODS- : CHOH conc.(%) Column Size: 50x4.6mmID Flow Rate:.0 ml/min Col.Temp. : 40C

8 Comparison of inertness to pyridine between and commercially ODS columns Assy. =.06 Assy. =.6 ) Pyridine ) Phenol good peak Assy. =. Assy. = L-Column ODS Capcell Pak C8 MGⅢ Atlantis T (Waters) Conditions Column: 4.6 mm I.D x 50 mm length,5μm Mobile phase: Methanol : HO = 0 : 70 Flow rate: ml / min Column temperature: 40 Detection: UV 54 nm Sample: 0.5μL (pyridine 0.09mg/mL, phenol 0.4mg/mL) Pyridine (Basic compound)

9 Comparison of inertness to amitriptyline between and commercially ODS columns good peak Assy. = Conditions Column: 4.6 mm I.D x 50 mm length,5μm Mobile phase: Acetonitrile : 0mM Ammonium acetate =60 : 40 Flow rate: ml / min Col.Tem p. : 40 Detection: UV 0 nm Sample: μl (Amitriptyline hydrochloride 0mg/L)

10 Conditions Column dimensions: 4.6 mm I.D x 50 mm length Mobile phase: Acetonirile / 5mM Phosphate buffer ph7.0 (60/40) Flow rate: ml / min Col.Temp.: 40 Detection: UV 0nm Injection Vol. : μl Interaction with Strong Basic Compounds Amitriptyline (Basic compound) ) Mianserine ) Amitriptyline (Basic compound) ) imypramin 4) Chlomipramine 4 tailing 4 late elute Tailing tailing 4 late elute Tailing 4 late elute tailing Tailing Hypersil GOLD Sunfire Zorbax Eclipse Plus C8

11 Interaction with Strong Basic Compounds Conditions Column dimensions: 4.6 mm I.D x 50 mm length Mobile phase: Acetonirile / 5mM Phosphate buffer ph7.0 (60/40) Flow rate: ml / min Col.Temp.: 40 Detection: UV 0nm Injection Vol. : μl Amitriptyline (Basic compound) ) Mianserine ) Amitriptyline (Basic compound) ) imypramin 4) Chlomipramine 4 tailing 4 late elute Tailing tailing 4 late elute Tailing tailing 4 late elute Tailing Atlantis T Symmetry C8 Luna 5u C8()

12 Interaction with Strong Basic Compounds Conditions Column dimensions: 4.6 mm I.D x 50 mm length Mobile phase: Acetonirile / 5mM Phosphate buffer ph7.0 (60/40) Flow rate: ml / min Col.Temp.: 40 Detection: UV 0nm Injection Vol. : μl Amitriptyline (Basic compound) ) Mianserine ) Amitriptyline (Basic compound) ) imypramin 4) Chlomipramine 4 tailing 4 late elute Tailing tailing 4 late elute Tailing 4 late elute tailing Tailing Capcell Pak MGⅢ YMC-Pack Pro C8 TSK-GEL ODS-00V

13 Comparison of inertness to dextromethorphan between and commercially ODS columns good peak N = 9,600 Assy. = Dextromethorphan (Basic compound) Conditions Column: 4.6 mm I.D x 50 mm length,5μm Mobile phase: Acetonitrile : 5mM Phosphate buffer(ph7.0) =40 : 60 Flow rate: ml / min Column temperature: 40 Detection: UV 0 nm Sample:.0μL (Dextromethorphan hydrobromide 0.mg/mL)

14 Conditions Column dimensions: 4.6 mm I.D x 50 mm length Mobile phase: Acetonirile / 5mM Phosphate buffer ph7.0 (40/60) Flow rate: ml / min Col.Temp.: 40 Detection: UV 0nm Sample: μl ) phenol Interaction with Strong Basic Compounds ) Dextromethorphan Dextromethorphan (Basic compound) adosorption adosorption adosorption Hypersil GOLD Sunfire Zorbax Eclipse Plus C8

15 Conditions Column dimensions: 4.6 mm I.D x 50 mm length Mobile phase: Acetonirile / 5mM Phosphate buffer ph7.0 (40/60) Flow rate: ml / min Col.Temp.: 40 Detection: UV 0nm Sample: μl ) phenol Interaction with Strong Basic Compounds ) Dextromethorphan Dextromethorphan (Basic compound) adosorption adosorption adosorption Atlantis T Symmetry C8 Luna 5u C8()

16 Conditions Column dimensions: 4.6 mm I.D x 50 mm length Mobile phase: Acetonirile / 5mM Phosphate buffer ph7.0 (40/60) Flow rate: ml / min Col.Temp.: 40 Detection: UV 0nm Sample: μl ) phenol Interaction with Strong Basic Compounds ) Dextromethorphan Dextromethorphan (Basic compound) adosorption adosorption adosorption Capcell Pak MGⅢ YMC-Pack Pro C8 TSK-GEL ODS-00V

17 Comparison of inertness to strong acidic compounds between Inertsil ODS-4 and commercially ODS columns ) Brilliant Blue FCF ) Phenol ) Salicylic acid Assy. = Conditions Column: 4.6 mm I.D x 50 mm length,5μm Mobile phase: Acetonitrile : 0.%(v/v) Phosphoric acid = 5 : 75 Flow rate: ml / min Col.Tem p. : 40 Detection: UV 54 nm Sample: μl (Brilliant Blue FCF 0.05mg/mL, Phenol 0.mg/mL, Salicylic acid 0.mg/mL)

18 Interaction with Strong Acidic Compounds Conditions Column dimensions: 4.6 mm I.D x 50 mm length Mobile phase: 0.%(v/v) Phosphoric acid in 5% Acetonitrile Flow rate: ml / min Col.Temp.: 40 Detection: UV 54 nm Sample: μl ) Brilliant Blue FCF ) Phenol ) Salicylic acid Brilliant Blue FCF adosorption adosorption not elute adosorption not elute Hypersil GOLD Sunfire Zorbax Eclipse Plus C8

19 Interaction with Strong Acidic Compounds Conditions Column dimensions: 4.6 mm I.D x 50 mm length Mobile phase: 0.%(v/v) Phosphoric acid in 5% Acetonitrile Flow rate: ml / min Col.Temp.: 40 Detection: UV 54 nm Sample: μl ) Brilliant Blue FCF ) Phenol ) Salicylic acid Brilliant Blue FCF adosorption adosorption not elute tailing adsorption adosorption not elute Atlantis T Symmetry C8 Luna 5u C8()

20 Conditions Column dimensions: 4.6 mm I.D x 50 mm length Mobile phase: 0.%(v/v) Phosphoric acid in 5% Acetonitrile Flow rate: ml / min Col.Temp.: 40 Detection: UV 54 nm Sample: μl ) Brilliant Blue FCF ) Phenol ) Salicylic acid Interaction with Strong Acidic Compounds adosorption not elute Brilliant Blue FCF adosorption not elute Base is Bad Capcell Pak MGⅢ YMC-Pack Pro C8 TSK-GEL ODS-00V

21 Comparison of inertness to chelating test sample between and commercially ODS columns good peak β- Thujaplicin (Hinokitiol) Conditions Column dimensions: 4.6 mm I.D x 50 mm length Mobile phase: Acetonitrile : 0.%(v/v) Phosphoric acid = 5 : 75 Flow rate: ml / min Col.Temp.: 40 Detection: UV 54 nm Sample: μl (β- Thujaplicin(Hinokitiol) 0.mg/mL)

22 Highly Pure Base Silica-gel Amount of Metals are inspected by Atomic Emission and ICP. Manufacturer's Validation Certificate Atomic Emissi on ppm Specification Results Fe <0 5 Na <0 4 Al <0 Ti < <0.5

23 Interaction with chelating Compounds Conditions Column dimensions: 4.6 mm I.D x 50 mm length Mobile phase: Acetonitrile : 0.%(v/v) Phosphoric acid = 40 :60 Flow rate: ml / min Col.Temp.: 40 Detection: UV 54 nm Sample: μl (β- Thujaplicin(Hinokitiol) 0.mg/mL) β- Thujaplicin (Hinokitiol) adosorption tailing adosorption tailing adosorption not elute Hypersil GOLD Sunfire Zorbax Eclipse Plus C8

24 Interaction with chelating Compounds Conditions Column dimensions: 4.6 mm I.D x 50 mm length Mobile phase: Acetonitrile : 0.%(v/v) Phosphoric acid = 40 :60 Flow rate: ml / min Col.Temp.: 40 Detection: UV 54 nm Sample: μl (β- Thujaplicin(Hinokitiol) 0.mg/mL) β- Thujaplicin (Hinokitiol) adosorption not elute adosorption not elute adosorption not elute Atlantis T Symmetry C8 Luna 5u C8()

25 Interaction with chelating Compounds Conditions Column dimensions: 4.6 mm I.D x 50 mm length Mobile phase: Acetonitrile : 0.%(v/v) Phosphoric acid = 40 :60 Flow rate: ml / min Col.Temp.: 40 Detection: UV 54 nm Sample: μl (β- Thujaplicin(Hinokitiol) 0.mg/mL) β- Thujaplicin (Hinokitiol) adosorption tailing adosorption not elute adosorption not elute Capcell Pak MGⅢ YMC-Pack Pro C8 TSK-GEL ODS-00V

26 Reversed phase columns often show Methanol 00% Water 00% Typical Alkyl C8 De-wetting Conditions Column:4.6 mmi.d x 50mm Mobile Phase: 0mM Phosphate Buffer (ph6.8) Flow Rate: Column Temp.: Detection:.Cytosine. Uracil.Thymine ml/ min 40C UV 65 nm

27 Explanation for Dewetting Stop and Flow Test using a typical Alkyl C8 Column At flow, with pressure 00% aqueous mobile phase Stopped flow, with no pressure Wash with Solvent (Methanol.etc) Restart flow -Pores dewet -analytes never enter pores resulting in no retention. Pore - re-wet hydrophobic bonded phase

28 No Dewetting on 00% aqueous mobile phase Restart flow No dewetting -analytes can enter pores - resulting in retention. At flow, with pressure 00% aqueous mobile phase Pore Stopped flow, No Dewetting Pore At flow, with pressure 00% aqueous mobile phase Ideally bonded phase Ideally bonded phase

29 De-wetting TEST Analytical Conditions Column Size : mmi.d. 5μm Eluent : HO Flow rate : ml/min Detector : UV 54nm Col.Temp. : 40. Cytosine. Uracil. Guanine 4. Thymine 5. Adenine 4 5 Stop the pump for 5min, then analyze again 98.6%.% General ODS

30 Characterization of,ods- and ODS-SP % ( CH ) CH 5%. n-butylbenzene ( CH ) 4 CH 8.5% 4. n-amylbenzene

31 Comparison of durability between and commercial ODS columns Relative retention time of naphthalene(%) (Carbon: %) Inertsil ODS- (Carbon: 5%) Inertsil ODS-X (Carbon: 9%) Inertsil ODS-Y (Carbon: 8.5%) Flow time 0.% TFA (ph) ( hours ) Durability test condition Column: 4.6 mm I.D. x 50 mm Test mobile phase:acetonitrile : 0.% TFA(pH.0) =0 : 90 Flow rate:.0ml / min Column temperature: R.T.

32 Analysis of food additives Analytical Conditions Column Size : mmi.d. 5μm 4 Eluent : A=CHCN ; B=5mM Acetate Buffer (ph4.6) A/B=0/90(4min Hold) ---6min /60 Flow rate : ml/min Detector : UV 8nm Col.Temp. : 40 Sample size : 0 μl (each 50μg / ml) Sodium Saccharin. p-hydroxy benzoic acid. Sorbic acid 4. Benzoic acid 5. p-hydorxy benzoic acid methyl ester 6. Dehydroacetic Acid 7. p-toluic acid 8. p-hydroxy benzoic acid ethyl ester 9. p-hydroxy benzoic acid n-propyl ester Inertsil ODS

33 Features of Perfect End-capping technique A newly developed state-of-the-art end-capping technology ideally deactivates the residual silanol groups, resulting in preventing adsorption of highly basic compounds. In addition, since the surface of the packing material is neutral, adsorption of neutral and highly acidic compounds does not occur. Intensive elimination of trace metals has been acheeved on the silica gel surface. When analyzing chelating compounds, it can be analyzed without any masking operations to those metals that are exposed on the surface of the packing material. Extreme durability to acidic mobile phase conditions High stability to 00% aqueous mobile phase conditions

34 Ordering Information Analytical / Preparative Column ID (mm) Length (mm) Cat.No Cat.No Cat.No Cat.No Cat.No Cat.No ID (mm) Length (mm) Cat.No Cat.No Cat.No Cat.No Guard * End-fitting is Waters /6 type. * For other column sizes, please send us an enquiry. (Upon request) um and um to be released in early 009!

35 Inertsil Series ODS columns Specification of various ODS columns Packing Material Base Silica gel (Spherical) Surface Area Pore Size Purity Carbon Loading Chemical Treatment Bonded-phase Structure End-capping 450 m /g 00A % % Monomeric Inertsil ODS- 450 m /g 00A % 5% Monomeric Inertsil ODS-P 450 m /g 00A % 9% Polymeric No Inertsil ODS-EP 450 m /g 00A % 9% Embedded No Inertsil ODS-SP 450 m /g 00A % 8.5% Monomeric Inertsil ODS- 0 m /g 50A % 8.5% Intermediate Inertsil ODS-80A 450 m /g 80A 99.99% 7.5% Monomeric

36 Selectivity of various ODS (C8) columns Mixture of samples: Alkylbenzene & PAHs ODS-4 ODS- ODS- ODS-EP ODS-SP ODS-P

37 Analysis of cold drugs Analytical Conditions Column Size : mmi.d. 5μm Eluent : A=CHCN ; B=0.% HPO4 A/B=/ min /5 Flow rate : ml/min 5 Detector : UV 0nm Col.Temp. : 40 Sample size : 0 μl (each 0μg / ml) Maleic acid. Acetaminophen. Caffeine 4. Chlorpheniramine 5. Ethenzamide 6. Bromovalerylurea 7. Apronalide 8. Isopropylantipyrine 9. Ibuprofen +4 5 Inertsil ODS