Determining PCMX concentraion method

[Krogan19]

I'm trying to determine PCMX concentrations in various solutions, but first need a set of standards that will give me a clear slope between 1.0mg/ml and 0.25mg/ml on an Elite 5 column. I've tried adding 0.1g PCMX to 100ml of acetonitrile with 2mg of BSTFA to derivatize. The solution was heated at 70degrees Celcius for an hour to facilitate the reaction, but I'm still not getting results. Any suggestions on a possible method of making standards and finding PCMX concentrations.
Thanks

[bunnahabhain]

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