RP C18 column with feature of a silanol group

Transcription

1 RP C8 column with feature of a silanol group lanol Activity Controlled C8 Column Sunrise ctacosyl C8) Sunrise ctadecyl C8) Sunrise ctadecyl-sac C8-SAC has an interaction of silanol groups ChromaNik

2 Sunrise C8 Sunrise C8 PLC column Name Stationary phase Carbon content Ligand density Particle size C8 ctadecyl %. µmol/m µm, µm C8 ctacocyl 8%.7 µmol/m µm, µm lica support Surface area: m /g Pore volume:. ml/g Pore diameter: nm End-capping Trimethylsilyl group (TMS) p range of C8 and dc8: p~p8 End-capping type Sunrise series の特徴 C8: A long alkyl chain improves both separation of fat-soluble compounds to compare with C8 phase and an excellent reproducibility in retention under high aqueous conditions. Furthermore, a suitable ligand density of C8 allows to be obtained a shape peak shape even if more than % aqueous mobile phase is used. Different selectivity Separation of Basic compounds Sunrise C8 8 8 retention time / min Suniest PhE Reverse Column size: x. mm 8/=C /mm P.B. p7. Flow rate:. ml/min Temperature: ºC Sample: = uracil = propranolol = toluene = nortriptyline = amitriptyline C N C N C C8: Conventional C8 phase with full end-capping 7 8 retention time / min C N C PhE: (Sunrise PhE has stopped production. Sunniest PhE is recommended as a replacement) Interaction based with p-electron such as p-p interaction p-electron also interacts with a polar site of a compound, so that phenyl phase improves separation of polar compounds. Ethylene chain between silica surface and phenyl group allows a movable sphere of a phenyl group to be wide. A chain with more than three carbons shows more hydrophobic interaction, so that p-electron interaction decreases relatively. Phenethyl (PhE) group is a suitable phenyl phase. Separation of Vitamin E Sunrise C8 Conventional C8, Isomer can be separated by C8 Column size: x. mm 97/=C / Flow rate:. ml/min Temperature: ºC Detection: UV at 9nm Sample: =δ-tocopherol =γ-tocopherol =β-tocopherol =α-tocopherol

3 Sunrise C8 Sunrise C8 PLC column Comparison of stationary phases Sunrise C8 7% C Sunrise C8 9% C Column size: x. mm / Flow rate:. ml/min Temperature: C Sample: = Methylparaben = Ethylparaben = Benzene = Toluene = Naphthalene = Ethylbenzene SunnistPhE % C Retention increased due to π- π interaction. Sunrise C8-SAC % C Retention increased due π electron interaction between naphthalene and silanol groups. Comparison of separation of α, β - carotene Conventional C8 Column size: x. mm C CN/CCl = 8: Flow rate:. ml/min Temperature: ºC Detection: UV at nm Sample: = α-carotene The mobile phase including chroloform makes alkyl chains brash up because chroloform can enter among alkyl chains. Consequently retention times of C8 became times longer than C8. C C C C C C C C C C Sunrise C8 = β-carotene C C C C C C C C C C

4 Sunrise C8 Separation of xylene isomers ºC Column: Sunrise C8, µm x. mm C/=7: Flow rate:.7 ml/min Temperature: ºC and ºC Detection: Sample: BTEX = Benzene = Toluene C = Ethylbenzene = o-xylene C = m-xylene = p-xylene ºC Sunrise C8 can separate xylene isomers although conventional C8 can t. The lower a temperature, the better a separation of isomers. Separation of ter-phenyl isomers Conventional C8 Column: Conventional C8 x. mm Sunrise C8, µm x. mm Methanol/water=9: Flow rate:. ml / min Temperature: oc Detection: UV@ nm Sample: = -Terphenyl, = m-terphenyl, = p- Terphenyl 7 Sunrise C

5 Sunrise C8-SAC lanol Activity Controlled C8 PLC Column New generation reversed-phase utilized silanol groups lanol group and peak tailing It is generally said that residual silanol groups on a stationary phase such as C8 (DS) causes absorption or peak tailing for a sample. Especially silanol groups near a hydrophobic site don t solvate with water completely, so that they show high absorption for basic compounds. Its peak shows terribly tailing. Several end-capping techniques have been developed to solve these problems for many years. st generation nd generation rd generation Bonded type th generation igh carbon and end-capped type th generation ighly endcapped type ybrid type lanol Activity Control Technology Sunniest C8 Sunrise C8 Sunrise C8-SAC Pellicular type lanol activity control technology ChromaNik developed the technique that decreased only silanol groups with high absorption activity to a basic compound and remained effective sailnol groups on the stationary phase. lanol activity control and no end-capping led the existence of silanol groups with high hydration which created a new and unique reversed-phase separation mode including hydrogen bond and ionexchange interaction. Furthermore, silanol activity controlling, then end-capping technique improved a peak shape of a basic compound exceedingly. C lanol groups with high absorption activity lanol Activity Control Technology C lanol activity control Changeover to siloxane bond Feature of Sunrise series Sunrise C8 The st Choice column as a fully end-capped C8 column Full end-capping after silanol activity control Reducing adsorption of a basic compound extremely A good peak shape for a metal cheleting compound Widely available for general reversed-phase separation Sunrise C8-SAC The "nd Choice" column which takes advantage of effective silanol groups interaction Reducing silanol groups with high adsorption activity The new separation mechanism including hydrogen bond and ion-exchange interaction Effective for separation of a basic compound and a polar compound Different selectivity and improvement of separation without changing a mobile phase The elution order of pyridine A) Sunrise C8 (end-capped) C) Sunrise C8-SAC (non end-capped) () B) Conventional no end-capped C8 () retention time / min Column size: x. mm C / =/7 Sample: = uracil () = pyridine = phenol ()

6 Sunrise C8-SAC lanol Activity Controlled C8 PLC Column Sunrise series create an unique separation Effectiveness of silanol activity control: Comparison between Sunrise C8 and C8-SAC Sunrise C8 is the so-called fully end-capped C8 column. It shows the same separation behavior as a conventional C8 column. n the other hand, Sunrise C8-SAC shows hydrogen bond and ion-exchange interactions based on a residual silanol on the silica support in addition to reversed-phase separation. For example Sunrise C8 column separates a basic compound similarly as a conventional C8, while Comparison of selectivity for basic compounds Sunrise C8-SAC makes retention of a basic compound be large because an ion-exchange interaction works although a non-ionic compound shows the almost same retention on both Sunrise C8 and C8-SAC. Furthermore, Sunrise C8-SAC shows large retention for a polar compound such as caffeine. Comparison of peak shape and retention A) Sunrise C8 p. A) Sunrise C8 Column size: x. mm C CN/mM P = :9 Flow rate:. ml/min Sample: = 8-Quinolinol (xine) = Caffeine B) Sunrise C8-SAC p. B) Sunrise C8-SAC A) Sunrise C8 B) Sunrise C8-SAC 8 Column size: x. mm C CN/mM Phosphate buffer p. or p. = : Flow rate:. ml/min Temperature: ºC N Sample: = Uracil = Propranolol N N C C p. p. 8 8 Comparison of caffeine A) Sunrise C8 B) Sunrise C8- SAC Column size: x. mm C /mm Phosphate buffer p. = :7 Flow rate:. ml/min Temperature: C Sample: = Theobromine = Theophylline = Caffeine = Phenol = Nortriptyline = Amitriptyline = Toluene C N C C N C 7 8 9

7 Sunrise C8-SAC lanol Activity Controlled C8 PLC Column Multiple mode separation is achieved on Sunrise series lanol groups controlled its activity functions as ion-exchange groups Sunrise C8-SAC is bonded with octadecylsilane on a pure silica gel and controlled its silanol activity without end-capping. Its carbon content is %. Separation of basic compounds with ammonium acetate: Effect of salt concentration(sunrise C8-SAC) mm mm mm mm mm Column size: x. mm C CN / acetate ammonium (p.) = 7: Flow rate:. ml/min Temperature: C Sample: = Uracil = Toluene = Propranolol = Nortriptyline = Amitriptyline 8 8 Separation on Sunrise C8-SAC is done including hydrogen bond and ion-exchange interaction based on silanol groups except for hydrophobic interaction. Control of p and salt concentration of a mobile phase can regulate retention. Relationship between buffer concentration and retention(sunrise C8-SAC) log k Toluene log [Buffer concentration] N (Amitriptyline) Amitriptyline Nortriptyline Propranolol,,, 8,,,, z B z B Vr log k = log[ A] + log[ A] + log + log K z z V z A A A:ion in eluent,b:ion of sample, k:retention of B,K:selection coefficient ZA, ZB:charge,Vr, Vm:resin volume and mobile phase volume in column m A N(Amitriptyline) N [Amitriptyline] B A Chromtograms under different p conditions (Sunrise C8-SAC) p.7 p. under acetic acid solution, p was.7 and there no ammonium ion. A basic compound shows tailing under p.7 (no ammonium ion). N=, Column size: x. mm C CN / mm acetate ammonium = 7: Flow rate:. ml/min Temperature: C Sample: N = Uracil N p. = Toluene C p. = Propranolol C N C p.9 = Nortriptyline = Amitriptyline N C p.8 N=, C N C

8 Sunrise C8, C8, C8-SAC Sunrise series Analytical and Preparative Columns Inner diameter length Sunrise C8, µm Sunrise C8, µm [mm] [mm] Cat. No. Cat. No.. ST ST 7 ST - ST ST ST7 ST7 ST8 ST8. ST ST ST ST 7 ST - ST ST ST7 ST7 - ST8. - ST78. - ST88 Inner diameter length Sunrise C8, µm Sunrise C8, µm Sunrise C8-SAC, µm Sunrise C8-SAC, µm [mm] [mm] Cat. No. Cat. No. Cat. No. Cat. No.. SB SB SA SA 7 SB - SA - SB SB SA SA SB7 SB7 SA7 SA7. SB SB SA SA SB SB SA SA 7 SB - SA - SB SB SA SA SB7 SB7 SA7 SA7 - SB8 - SA8. - SB78 - SA78. - SB88 - SA88 8