method development from scracth

[pat_val]

what is the best way to start method development from scracth? Any articles or presentation? any suggestions? Thanks in advance for your help.

[Vlad Orlovsky]

Here are tools our company is offering for method development:

Interactive Step-by-Step Method Development Guide (based on the properies of your molecules):
http://www.sielc.com/MethodDevelopment_ ... dType.html

Method Development Guide (Buffer selection, pKa vs. pH values, detection techniques, etc.)
http://www.sielc.com/MethodDevelopment_Guide.html

[Uwe Neue]

We (Waters) are typically recommending a fixed set of screening runs, followed by the optimization of the best method.

We carry out screening gradients with methanol and acetonitrile, at low and high pH on three columns of known different selectivity. This is a total of 2x2x3 = 12 blind experiments. We use packings that are stable at high and low pH (pH 10 and 2), such as the XBridge family of packings. The packings are a C18 packing, a packing with an embedded polar groups, and a phenyl packing.

In the final method optimization, we finetune the gradient or the pH, and use temperature as additional variable.

These ideas have been published

U. D. Neue, E. S. Grumbach, J. R. Mazzeo, K. Tran, D. M. Wagrowski-Diehl, “Method development in reversed-phase chromatographyâ€

[pat_val]

Thanks for your prompt reply. The reason i am asking this, i have always work in generic industry. Where I rarely got chance to develop method form scratch. I always use to modify drug substance vendor method for drug product. But I have an interview next week and they are working on NCEs, so I would like to get some more idea for method development for scratch. Thanks in advance for your help.

[bisnettrj2]

Waters (Uwe's company) has software called the Fusion Method Development software that automates the process he described above. It's pretty fancy stuff, and good if you want a method that has to go through validation.

If you want generic method development ideas, you can see back copies of LC/GC for articles by John Dolan:

http://chromatographyonline.findanalyti ... 018?ref=25

http://chromatographyonline.findanalyti ... ail/439748

http://chromatographyonline.findanalyti ... ail/447624

http://chromatographyonline.findanalyti ... 547?ref=25

http://chromatographyonline.findanalyti ... 300?ref=25

http://chromatographyonline.findanalyti ... ail/477360

http://chromatographyonline.findanalyti ... ?id=480587

[Uwe Neue]

pat_val,

I need your email address if you want me to send some material. Contact me at neueud@yahoo.com or at Uwe_Neue@Waters.com.