Low-level (PPB) determination of cisplatin in cleaning validation (rinse water) samples. I. An atomic absorption...

Suitable analytical methods are required for quantitative determination of trace levels of ingredients in samples obtained for purposes of cleaning validation. We describe below an atomic absorption method for the quantitation of cisplatin, an antineoplastic agent, in aqueous samples. Cisplatin was reacted with diethyldithiocarbamic acid (DDTC), sodium salt, to yield a platinum-DDTC (Pt-DDTC) complex. The Pt-DDTC chelate was extracted into methylene chloride, the extract was mixed with acetonitrile, and the platinum content was then determined using a Zeeman atomic absorption (AA) spectrophotometer. The extraction conditions and AA experimental conditions were set up such that the detection level could be extended to 0.5 ng/ml. Reproducible results were obtained at a quantitative working standard concentration of 5 PPB. The absorbance response was found to be a linear function of cisplatin concentration in the region between 0.5 PPB and 20 PPB, which is about 10% to 400% of the target analyte concentration of 5 PPB. The target analyte concentration was set at 5 PPB such that it was at least 10 times the detection limit of about 0.5 PPB.