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25th September 2012 @ 04:31
Now that it looks like the formation of MNR46 is catalytic ([blog]6610[/blog]) it is worth while developing a reliable HPLC method to assay these experiments and calculate yields without the need of purification. Using HPLC1 early runs showed that there was a significant error in varying the injection volume therefore it was necessary to maintain a constant injection volume. It was also shown that, although the peaks did not "top out" on these runs, peak area at higher concentrations was inaccurate thus requiring us to keep the injection mass below 2 ug. [b]PZQ calibration[/b] Using the standard 0-100 over 30 mins method and 5 uL injections, PZQ solutions in MeCN showed a linear response with the R2 value of the calculated trend line being closer to one with data points below 2 ug of sample per injection. [b]MNR46 calibration[/b] Using the same method as above and 5 uL injections, MNR46 solutions in MeCN showed a linear response with the R2 value of the calculated trend line being closer to one with data points below 2 ug of sample per injection. It's unsure if the point at 14 ug is an error or due to the detector maxing out but it has not been followed up as it has been shown else where that the most accurate readings come with injections containing less than 2 ug of material. [b]Test samples of MNR46 and PZQ[/b] Using the above method samples or varrying concentrations of MNR46 were ran with a constant concentration of PZQ present in all the samples. The PZQ was expected to be horizontal but showed a linear response with increasing concentration of MNR46. The gradient of the trend line is also 2,000,000 units out. Due to limited data, it is unsure at this point if this is within reasonable error or if this is another problem with the product/PZQ mixture As this stands, this method has no value in following the formation of MNR46.
Attached Files
mnr46_with _PZQ_plot.PNG
mnr46_plot.PNG
pzq_plot.PNG