Chromatography Forum

I am a Ph.d Scholar working on sustained release prochlorperazine.I have schimadzu HPLC with uv and CHoulchem ECD DEtector.I have c18 column and my mob phase for uv analysis is is Nah2po4 30 mM Buffer :acetonitrile : methanol, 50:30:20, using flow rate 1 ml and wavelength 254, but getting no peaks.also tried ECD method having mob phase consisted of acetonitrile:ammonium phosphate
(100mM, pH6.5) (45:55, v/v) and EDTA50 g/l.Analytical cells
1 and 2 were respectively set at 400 and 550mV.gurd cell potential 750 bt again no peak. Please help me and guide.I cant get peak even with standard drug also.

With profound regards

Khalid Rauf.

In my whole 5 minutes of poking around the internet I found this nice review paper, you should read it:

Journal of Pharmaceutical and Biomedical Analysis
Volume 27, Issue 5, 1 February 2002, Pages 661-678

And another method that used 90% ACN to this and a related compound off of a cyano column.

And yet another ECD method that was using about 850mV.

Me, I would use a UV to detect while I worked on the seperation, then (and ony if I had to) throw on the ECD and sort out those conditions.

As well as looking at the review, I would look at the methods in the pharmacopoeia, eg the USP has an ion-pair UV assay method for the Oral Solution formula.

Bruce Hamilton