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PdX Palladium API Fluorescent Detection Kit

 

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New, Impoved PdXPalladium API Fluorescent Detection Kit


Catalog Number K007-F1

  • Determine Pd levels on 41 samples in 30 Minutes!
  • Suitable for APIs in HCl, NMP, Acetonitrile, DMF, EtOH or Toluene
  • Works on any fluorescent plate reader

 

 

In recent years, many new synthetic transformations have been developed that use palladium (Pd) compounds for the catalysis of carbon-carbon and carbon-heteroatom coupling reactions such as the Buchwald-Hartwig, Heck, Sonogashira, Suzuki-Miyaura, and Tsuji-Trost transformations. These reactions have found increased popularity for pharmaceutical processes as they utilize a wide-range of functional groups to build complicated molecules. However palladium-catalyzed reactions present a problem in that the palladium can often be retained in the isolated API product. Current FDA and EAEMP regulations limit all platinum group (Pt, Pd, Ir, Rh, Ru, Os) metal contamination (as a group) to less than 5-10 ppm. The standard methods of quantifying palladium in APIs are atomic absorption analysis, x-ray fluorescence, or inductively-coupled plasma mass spectroscopy (ICP-MS). These expensive instruments dictate a highly trained scientist to operate, suffer from cross-contamination of the probe and require scrupulous clean up methodology.

The PdX Palladium API Fluorescent Detection Kit is designed to allow rapid screening of methods for Pd removal from solutions of APIs in DMF, Acetonitrile, NMP, Ethanol, dilute HCl and Toluene. Standards or diluted samples are pipetted into a microtiter plate along with supplied Detection Reagent and Sodium Borohydride reducing agent. After 30 minutes the intensity of the generated fluorescence is read at 525 nm in a microtiter plate reader. Fluorescence is prooprtional to Pd level. No acid digestion required.

Reagents all stable at room temperature

Sensitivity
The sensitivity of the assay is 0.082 nM Equivalant to 0.1 ppm

Intra and Inter Assay Precision
Intra Assay precision between 4.1 and 5.5% for 3 catalysts run multiple times in the same assay.

Inter Assay precision between 9.9 and 14.9% for 3 catalysts run in multiple assays (n=20) by four people over two days.

Linearity
Linearity was determined by taking two palladium catalyst samples in toluene, diluted 1:20 in DMSO, and then diluted in Sample Diluent, one, Bis(dibenzylideneacetone) palladium(0), with a low diluted Pd level of 7.6 nM and one, 2-(2-Di-tert-butylphosphine)biphenylpalladium(II) acetate, with a higher diluted level of 59.5 nM were mixed at different ratios. Linearity averaged 92.6%

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Last modified: 05/29/09