Validation for the determination of biuret in water-soluble, urea-based commercial inorganic fertilizer materials, urea solutions, and sulfur-coated urea products by reversed-phase liquid chromatography: single-laboratory validation of an extension of AOAC official methods 2003.14.

Abstract

A single-laboratory validation (SLV) study for the LC determination of biuret in dry and liquid urea-based commercial fertilizers was conducted. A total of 23 samples were used: 11 commercial dry urea products, two urea ammonium nitrate products, eight liquid urea-based commercial fertilizers, and four sulfur-coated urea samples from different sources. In addition, one biuret standard from Aldrich and one sample from the Magruder check sample program were used as validation samples. The proposed method is an extension of AOAC Official Method 2003.14 and is based on dissolution of the test portion in the LC mobile phase and determination by HPLC. The system is linear over a concentration range of 1.00-4.50 mg/L biuret, with a correlation coefficient > or = 0.9999. The biuret was well- separated from urea in the commercial urea samples, and from other constituents in the commercial liquid fertilizer with no observed interferences. Recoveries were determined by spiking four of the validation materials with a known amount of biuret standard and measuring the biuret level according to the method. The averaged recovery was 97%. Method precision was determined by quadruplicate analyses of four of the liquid and six of the commercially available dry urea validation materials using three and four replicate analyses. For the liquid fertilizer analyses, the RSD ranged from 7.04 to 13.31%. For the dry urea analyses, the RSDs ranged from 5.68 to 14.34%. Instrument precision was evaluated at the test initiation by using seven injections of five biuret standard solutions. SD varied from 0.27 to 1.02%, with RSDs averaging 1.14%. The LOD was determined to be 0.009% biuret in material, while the LOQ was determined to be 0.031% biuret in material. In addition to the intralaboratory study, interlaboratory studies were performed by two other outside laboratories using this method. Over a concentration range of 0.2 to 0.9% biuret, the average SD was 0.11%, the average RSD was 21.16%, and the average HorRat value was 4.73%. Furthermore, comparative studies for biuret using AOAC Official Methods 960.04 and 976.01 with the proposed LC method were performed. The three methods produced very close results; however, the two AOAC methods generate hazardous wastes and are more tedious. On the basis of accuracy and precision of the results for this SLV study, it is recommended that this method be collaboratively studied for the determination of biuret in dry and liquid urea-based commercial fertilizer materials.