Use of Design of Experiments to Optimize High-Throughput Semipreparative LC and LC/MS Methods

Journal of Combinatorial Chemistry

Volumn 6, Issue 1, 2004, Pages 78-82

  Cole, Derek C ^a   Pagano, Nicholas ^a   Kelly, Michael F ^a   Ellingboe, John ^a  

^a WYETH RESEARCH   (United States)

Author keywords

[No Author keywords available]

Indexed keywords

SOLVENT;

ARTICLE; DILUTION; EXPERIMENT; EXPERIMENTAL DESIGN; EXPERIMENTAL MODEL; FLOW RATE; HIGH PERFORMANCE LIQUID CHROMATOGRAPHY; LIQUID CHROMATOGRAPHY; MASS SPECTROMETRY; MULTIPLE REGRESSION; REGRESSION ANALYSIS; TEMPERATURE; TIME;

EID: 0942278904     PISSN: 15204766     EISSN: None     Source Type: Journal    
DOI: 10.1021/cc034013v     Document Type: Article

References (9)

1. www.umetrics.com.
2. Dolan, J. W. J. Chromatogr. A 2002, 965, 195-205. See also www.selerity.com.
3. Wheat, T. Abstracts of Papers, Pittsburgh Conference, New Orleans, LA, March 4-9, 2001; Pittsburgh Conference, Pittsburgh, PA, 2001; p 1948.
4. Blom, K. F. J. Comb. Chem. 2002, 4, 295-301.
5. Unoptimized HPLC conditions: solvent A, 0.02% TFA/ water; solvent B, 0.02% TFA/acetonitrile. Gradient: time 0 min, 95% A; 2 min, 95% A; 14 min, 10% A; 15 min, 10% A; 16 min, 95% A. Flow rate, 20 mL/min. Detection, 254-nm DAD. Sample size, 20-50 mg crude dissolved in 1-2 mL DMSO/MeOH/water. Column, Waters XTerra Prep MS C18 5 μM, 19 x 50 mm. Guard column, XTerra C18 5 μM, 10 x 10 mm.
6. www.gilson.com.
7. Lefebvre, P. M; West, W. R. Personal communications. See also Application Note LT40004, www.gilson.com.
8. www.j-kem.com.
9. Optimized HPLC conditions: Solvent A, 0.02% TFA/water; solvent B, 0.02% TFA/acetonitrile. Gradient: time 0 min, 95% A; 1 min, 95% A; 7 min, 10% A; 7.5 min, 10% A; 8 min, 95% A. Flow rate, 34 mL/min. ACD, 5% of solvent A (or MeOH) pumped through sample loop. (Note: the flow rate of pump A is decreased so the overall percent of A is unchanged.) Solvent temperature, 40°C. Detection, 254-nm DAD. Sample size, 20-50 mg crude dissolved in 1-2 mL DMSO/MeOH/water. Column, Waters XTerra Prep MS C18 5 μM, 19 x 50 mm. Guard column: XTerra C18 5 μM, 10 x 10 mm.