New Developments in Hybrid Particle Technology: Stability, Selectivity Separation and SPEED

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Part Number:
Diane M. Wagrowski-Diehl, KimVan Tran, Eric Grumbach, Jon Belanger, Bob Brennick, Jeffrey R. Mazzeo, Uwe D. Neue[Waters]
AAPS 2002, Toronto
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Content Subtype:
Caffeine, Aniline, N-Methylaniline, 2-Ethylaniline, 4-Nitroanisole, N-N-Dimethylaniline, Acetanilide,Triamcinolone, Hydrocortisone, 2-Amino-7-chloro-5-oxo-5H-[1]benzopyrano[2,3-b]pyridine-3-carbonitrile, 6alpha-Methyl-17alpha-hydroxyprogesterone, 3-Aminofluoranthene, 2-Bromofluorene, Perylene, Naphtho(2,3-a)pyrene, Sulfadiazine, Sulfathiazole, Sulfamerazine, Sulfamethoxazole, Sulfisoxazole, Sulfadimethoxine, Atenolol, Metoprolol, Pindolol, Rat plasma, Lidocaine, Prednisolone, Naproxen, Amitriptyline, Ibuprofen
Spiked plasma samples, Protein precipitation,
XTerra MS C18 2.5 µm Steel 4.6 mm 20 mm XTerra MS C18 3.5 µm Steel 4.6 mm 20 mm XTerra MS C18 5 µm Steel 4.6 mm 150 mm
Pharmaceutical companies have been driven to bring products to market faster by sample throughput. To meet these goals, this has required new chromatographic approaches which expand the limits currently imposed by silica gel based reversed-phase separations. The development of hybrid particles for HPLC columns has set new limits for speed of analysis, operating temperatures and a wider useable pH range (1-12). Because of the mandate to run faster separations, researchers have tried to move away from hour-long separations on 15 or 25 cm columns. Many have turned to the monolith technology due to claims of reductions in separation time and increased sample throughput. However, running at such high flow rates (up to 10 mL/min) increases solvent consumption dramatically. Smaller i.d. monoliths have been promised, but are not yet available. Additionally, monolith technology is not yet available in preparative dimensions which creates a barrier to direct scale-up possibilities. New column hardware in 4.6 x 20 mm dimensions has been developed and packed with 2.5 µm and 3.5 µm XTerra® MS C18 particles. We have measured the peak capacities of these columns and found them to be comparable to results obtained with the monolith columns. We have developed several applications with total run times of 5 minutes or less, using reasonable flow rates. We will show how an application run on a long column can be transferred to these shorter columns resulting in optimum chromatographic performance in a much shorter run time. We also show 1000 injections of a protein precipitation sample on a 4.6 x 20 mm column packed with 2.5 µm particles.

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