GAS-CHROMATOGRAPHIC METHOD FOR PUTRESCINE AND CADAVERINE IN CANNED TUNA AND MAHIMAHI AND FLUOROMETRIC METHOD FOR HISTAMINE (MINOR MODIFICATION OF AOAC-OFFICIAL-METHOD-977.13) - COLLABORATIVE STUDY

A collaborative study was conducted to test a modification to the AOAC fluorometric method for histamine (AOAC(R) Official Method 977.13) th at substitutes 75% methanol as the extracting solvent. AII other steps remain unchanged. The extracts prepared with 75% methanol were also u sed to collaboratively test a gas chromatographic (GC) method for dete rmination of putrescine and cadaverine in seafood. In the GC method, t he extracted diamines are converted to fluorinated derivatives, the re action mixtures are passed through solid-phase extraction columns, and the derivatives are quantitated by electron capture GC after separati on on an OV-225 column. Fourteen laboratories using the GC method for putrescine and cadaverine and 16 laboratories using the fluorometric m ethod for histamine analyzed 14 canned tuna and raw mahimahl (includin g blind duplicates and a spike) containing 0.2-2.6 ppm putrescine, 0.6 -9.1 ppm cadaverine, and 0.6-154 ppm histamine, At the 5 ppm level, re coveries ranged from 71 to 102% for putrescine and 77 to 112% for cada verine; the respective repeatability relative standard deviations (RSD r) were 5.2 and 15%, and the respective reproducibility relative stand ard deviations (RSDR) were 8.8 and 18%, At the 50 ppm level, histamine recoveries ranged from 84 to 125%, RSDr was 3.6%, and RSDR was 9.4%, The GC method for determination of putrescine in canned tuna and cadav erine in canned tuna and mahimahi has been adopted first action by AOA C INTERNATIONAL, and the AOAC Official Method 977.13, Histamine in Sea food, Fluorometric Method, has been modified.