AOAC OFFICIAL METHODS OF ANALYSIS (2016) (CEREAL FOODS Chapter 2, p. 67 32.2.04 AOAC Official Method 939.05 Fat Acidity—Grains Titrimetric Method First Action 1938 Final Aetion Codex-Adopted-AOAC Method” A. Reagents (2) Toluene-aleohol-phenolphthalein salution—0.02%. To 1 1. toluene add 1 | aleohol and 04 g phenolphthain, (b) Alcohol phenolphohalein solution —0.04%. To 1 I aleoho add 0.4 phenolphthalein (© Potassu Incraxide standard solution —0.0178 M, carbonate- fre, I ml.= I mg KOH, 2B. Apparatus (2) Grain mill Suitable for grinding small test samples. () Fat extraction device Soxhlet ot other suitable type (Durable paper thimbles or Alundutn RA-360 thimbles ae suitable for extraction.) ©. Method! Obiain representative test sample of ca 50g grain (com, 200 g) by hand quartering or by use of mechanical sampling device. Preferably grind test sample so that 90% will pass No, 40 sieve (somewhat coarser grind will not materially affect results). If test sample is too moist to grind readily, dry at temperature of ea 100°C just long enough to remove excess moisture, Extract 10 + 0.01 g test portion with petroleum ether ea 16 hy Jn extractor, Stan extraction as soon as possible after grinding and never let ground test sample remain overnight, Completely evaporate solvent ftom extract on stcam bath, Dissolve residue Jn extraction flask with $0 ml. toluenesslcohol-phenolphthalein solution and titrate with standard KOH solution to distinct pink, or incase of yellow solution to orange-pink, emulsion forms during titration, dispel hy adding second 50 mi portion of taluene-aleahol- phenolphtalein solution. End point should mateh eolor of solution made by adding 25 ml. 0.01% KMO, solution to $0 mL K,C1,0, solution of proper strength to match color of original solution being titrated, (Add 0.5% K,Cr,0, solution dropwise to 50 mL H,0 until color matches. Then add 2.5 mL 0.01% KMn0, solution ) “Make blank tiation on 50 ml. toluenesaleoholephenolphhalein solution and subteact this value feom itation value of est portion. If additional SO mL portion toluenesalcohol-phenolpbthalein solution was added, double blank tiation. Report Fat acidity as ‘mg KOH required to neutralize fice fatty aids from 100 g grain (ary basis. Fat acidity = 10» (titration blank) References: JAOAC 22, $26(1939); 23, 493(1940); 24, 587(1941) 50, 198(1967); TH, 84(1988) . Method I-Rapid Method for Corn (Result may be obtained in 3 min Carefully decant as much liquid as possible into 15 em folded paper inserted in 8 em glass funnel, and cover funnel with cover, lass to reduce evaporation, Collect exactly 25 ml. irate in 25m. volumetric flask, Transfer this filtrate 9 250 ml, Florence flask Refil volumetric ask to 25 ml. mark with aleohol-phenolphthalein solution and transfer to lask conning benzene extract. Using colorstandard preparedas nC, titrate extract with standard KOI solution to distinct pink in case of white cor, and to orangex pink for yellow corn IF emulsion forms during tration, dispel by adding 25 mL. each of benzene and of aleohol-phenolphthalein solution. Determine blank titration on mixture of 25 ml. benzene and 25 ml aleohol-phenolphthalein solution, If addtional benzene and elcohol were added, double blank titration, Report fat acidity as mg KOH required to neutralize free ftty acids from 100 g com (ary basis, Fat acidity = 10 (titration blank), calculated on dry basis References: JHOAC 23, 493(1940); 24, $87(1941) Adds Col Dna Meo i ee ay ai ea a Zearalenone in Corn ‘Thin-Layer Chromatographic Method First Action 1976 Final Action 1988 AACC-AOAC Method See 976.22 (see 49.8.0), Deoxynivalenol in Wheat Thin-Layer Chromatographic Method Fit Action 1986 AOAC-AACC Method ‘See 986.17 (ee 49.4.0), 32208 AOAC Official Method 979,10 ‘Starch in Cereals Glucoamylase Method First Action 1978 Final Action 1997 AACC-AOAC Method ‘A. Reagents (2) Glucoanylase solution—10 mg (30 IUyiml: H,0. Purity of enzyme is eitica; should be prepared from Rhizopus delemar Preparation Sumizyme 3000 from Shin Nihon Chemical Co. (Aichi, Japan) has been found satisfactory. (0) D.Glucose standard sofution—400 mg anhyérousL. Let stand 4h to complete mutarotation before use. (©) Acetate buffer—4 M, pll 48. Dilute 120 mL. glacial CH,COOL and 164 g anhydrous CLL,COONa to IL with 1,0. ‘©2016 AOAG INTERNATIONAL i i