Ac. Entwisle et al., AN INTERCOMPARISON OF METHODS FOR THE DETERMINATION OF OCHRATOXIN-A IN PIG-KIDNEY, Food additives and contaminants, 14(3), 1997, pp. 223-236
The preparation of two pig kidney materials is described, together wit
h a report on the results of an intercomparison study of methods to de
termine ochratoxin A levels in these materials. The materials were pre
pared, and the intercomparison study carried out within the European C
ommission, Measurements and Testing Programme, which is the successor
of the Community Bureau of Reference (BCR). The materials were prepare
d from blank and naturally-contaminated pig kidneys and were freeze-dr
ied. Details are given on the freeze-drying and packaging procedure, a
nd the checks to ensure homogeneity and stability of the freeze-dried
materials. The intercomparison study involved 20 European laboratories
, which analysed the naturally-contaminated (freeze-dried) sample (och
ratoxin A content approximately 10 mu g/kg based on fresh weight) and
the 'blank' sample (ochratoxin A content <0.6 mu g/kg based on fresh w
eight) using a variety of procedures for extraction and clean-up. All
laboratories used HPLC as the determinative step. Recoveries were foun
d to range from 43 to 128%. The study highlighted problems with recove
ry of spiked ochratoxin A from freeze-dried pig kidney material. There
is a clear need to improve analytical performance, particularly with
respect to the extraction efficiency from this type of matrix.