Is you analysis for a specific protocol (EPA, FDA, etc)?
The EPA recognizes two fundamentally different analytical techniques; those that have a "zero" signal level (typically spectroscopic techniques such as ICP) and those that do not (GC and GCMS).
For the former, you can measure background signal and use that to calculate a standard deviation which you can then relate to whatever signal to noise is appropriate (I've seen 3X and 10X used).
For the latter, what is done (for EPA work until they finish the re-work of their MDL protocol) is you run a minimum of 7 spiked samples (through whatever prep may be utilized) spiked at what near what you believe the lowest level you can detect. You quantitate these runs, and calculate the standard deviation for each analyte. You then multiply the standard deviation by the "Student-t" value of the analyses. The protocol can be found at:
http://ecfr.gpoaccess.gov/cgi/t/text/te ... .2&idno=40
Greg