Can anyone suggest a detailed (best) analytical method of HPLC and LC-MS to determine concentrations of ANTIBIOTIC CIPROFLOXACIN from wastewater samples?
There are many Ciprofloxacin HPLC methods on the internet. Just syringe ultrafilter, dilute it in mobile phase, and shoot.
I am more interested in how i prepare the samples, I can't just directly use only wastewater, without properly preparing it?
As long as you filter it you can. Dilution in buffered mobile phase will also dilute out any harmful ions and pH extremes.
These samples are not sludges are they?
They are just wastewater coming from hospitals, in some researches the samples are adjusted to a pH of 3.
Good. Use a guard column (just in case). These samples seem quite compatible with pH 3 Phosphate buffer. Be sure to use a buffered mobile phase.
Can organic compounds such as humic acid play a role in the creation of errors in hospital wastewater?
Unknown, but unlikely. Cipro is typically tested in drug dosage forms. But, I would suspect humic acid to elute in the solvent front or be completely retained by a C18 column and thus not interfere with your quantitation of Cipro.
You will have to adapt (develop) a 'new' method and validate it per ICH Q2(r1) guidelines.
Why do you ask? What concentration are you expecting (your answer to this question will determine the detector you use and the mobile phase)?
It's already been done (see below)! Why are you reinventing the wheel?
Article Antibiotics in Wastewater of a Rural and an Urban Hospital b...
I'm currently in the middle of creating instructions for determination of ciprofloxacin in hospital waste waters.
You are correct, Luka. You have to worry about ciprofloxacin sorbed onto the wastewater solids. Filtration prior to extraction removes that fraction of the ciprofloxacin. I would recommend that you take a look at USEPA method 1694. It is a LC-MS/MS method specifically designed for the measurement of pharmaceuticals in water and wastewater.
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