AOAC Official Method 983
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B55D74525D784FCB00A2CBC47FF6651F |
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0.11 |
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4 |
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日期： |
2016-2-28 |
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47.2.02,AOAC Of fi cial Method 983.15,Phe no lic An ti ox i dants,in Oils, Fats, and But ter Oil,Liquid Chromatographic Method,First Ac tion 1983,Fi nal Ac tion,Re vised First Ac tion 1992,Fi nal Ac tion 1994,IUPAC–AOAC Method,(Ap pli ca ble to propyl gallate [PG], 2,4,5-trihydroxybutyrophenone,[THBP], tert-butylhydroquinone [TBHQ], nordihydroguaiaretic,acid [NDGA], 2- and 3-tert-butyl-4-hydroxyanisole [BHA],2,6-di-tert-butyl-4-hydroxymethylphenol [Ionox-100], and,3,5-di-tert-butyl-4-hydroxytoluene [BHT] at 20–200 mg/g in oils,and fats, 10–100 mg/g in but ter oil, and to octyl and dodecyl gallate,[OG and DG] at 10–100 mg/g in but ter oil.),See Ta bles 983.15A–C for the re sults of the interlaboratory study,sup port ing ac cep tance of the method.,A. Prin ci ple,Antioxidants are extracted into acetonitrile. Extract is concentrated,and di luted with 2-propanol. An ti ox i dants are sep a rated by liq uid,chromatography and mea sured by ul tra vi o let de tec tion at 280 nm.,B. Apparatus,(a) Gra di ent liq uid chromatograph.—With 10 mV re corder or,in te gra tor to elec tron i cally mea sure peak heights, 10 mL loop,in jec tion valve, and de tec tor to mea sure absorbance at 280 nm.,Typ i cal op er at ing con di tions: de tec tor sen si tiv ity, 0.05 AUFS;,tem per a ture, am bi ent; flow rate, 2.0 mL/min.,(b) LC col umn.—Packed with C18-bonded spher i cal (pre ferred),sil ica, or equiv a lent. Use guard col umn if de sired. Must be ca pa ble,of base line res o lu tion of all 9 an ti ox i dants as shown in,Fig ure 983.15. Ver ify peak iden ti ties, if nec es sary, by in jec tion of,in di vid ual standards.,(c) Glassware.—Rinse all glass ware with CHCl3, ac e tone, and,meth a nol, suc ces sively, and blow dry with N2.,C. Re agents,(a) Sol vents.—Acetonitrile, 2-propanol, and hex ane.,Dis tilled-in-glass grade.,(b) Mo bile phase.—(1) 5% Ace tic acid in H2O.—LC grade.,(2) Acetonitrile–meth a nol (1 + 1, v/v).—LC grade.,Ta ble 983.15A. Interlaboratory study results for phe no lic an ti ox i dants in oils, liq uid chro mato graphic method,An ti ox i danta Added, mg/gb Re cov ered, mg/g,Results,based on,mean,re cov ery, %,Re peat abil ity Reproducibility,sr RSDr, % sR RSDR, % HorRat,PG 193.7 184 95.2 16.0 8.66 16.0 8.66 1.20,PG 96.7 93.8 96.9 4.50 4.80 4.50 4.80 0.60,PG 19.4 17.6 90.9 2.01 11.5 2.52 14.3 0.25,THBPc 203.2 199 98.1 9.99 5.01 9.99 5.01 0.70,THBP 101.6 99.1 97.5 5.25 5.30 5.58 5.63 0.71,THBP 20.3 19.6 96.7 0.97 4.94 1.53 7.77 0.77,TBHQ 196.1 201 103 8.77 4.36 22.8 11.4 1.58,TBHQ 98.1 100 102 3.63 3.63 21.5 21.5 2.69,TBHQ 19.6 19.1 97.5 1.50 7.85 3.17 16.6 1.63,NDGA 93.8 91.7 97.8 5.06 5.51 6.39 6.97 0.87,NDGA 18.8 18.4 98.3 0.34 1.83 0.60 3.24 0.32,BHA 198.5 197 99.1 6.54 3.32 6.61 3.36 0.47,BHA 99.2 99.7 101 5.43 5.45 6.15 6.17 0.77,BHA 19.9 19.5 98.0 0.43 2.19 0.76 3.92 0.39,IONOX-100 208.2 198 95.3 17.7 8.92 19.4 9.76 1.37,IONOX-100 104.1 98.7 94.8 10.2 10.4 10.5 10.6 1.34,IONOX-100d 20.8 20.2 97.0 0.71 3.54 1.14 5.63 0.56,BHTd 202.9 170 83.8 3.50 2.06 4.54 2.67 0.37,BHTd 101.5 84.3 83.1 2.36 2.80 2.36 2.80 0.35,BHT 20.3 17.2 85.1 0.90 5.22 1.06 6.18 0.61,a PG = Propyl gallate, THBP = 2,4,5-trihydroxybutyrophenone, TBHQ = tert-butylhydroquinone, NDGA = nordihydroguaiaretic acid, BHA = 2- and,3-tert-butyl-4-hydroxyanisole, Ionox-100 = 2,6-di-tert-butyl-4-hydroxymethylphenol, BHT = 3,5-di-tert-butyl-4-hydroxytoluene.,b Antioxidant values measured to 4 significant figures, mg/g, but rounded to near est 0.1 mg/g.,c Two of 7 lab o ra to ries re jected as out li ers by the pair Grubbs test.,d One of 7 lab o ra to ries re jected as out lier by the sin gle Grubbs test.,2006 AOAC INTERNATIONAL,Ta ble 983.15B. Interlaboratory study results for phe no lic an ti ox i dants in lard, liq uid chro mato graphic method,An ti ox i danta Addedb, mg/g,Re cov ered,mg/g,Results,based on,mean,re cov ery, %,Re peat abil ity Reproducibility,sr RSDr, % sR RSDR, % HorRat,PG 96.9 90.1 93.0 3.18 3.53 3.18 3.53 0.44,PG 38.7 34.6 89.4 1.55 4.48 1.55 4.48 0.49,THBP 101.6 97.9 96.4 6.75 6.89 14.3 14.6 1.84,THBPc 40.7 36.4 89.5 1.35 3.71 1.47 4.06 0.45,TBHQ 98.1 95.6 97.5 7.71 8.07 22.1 23.2 2.91,TBHQ 39.3 35.0 89.0 6.04 17.3 11.6 33.2 3.62,NDGA 93.8 87.8 93.6 2.65 3.02 4.74 5.40 0.67,NDGA 37.5 35.3 94.2 1.06 3.01 1.79 5.06 0.55,BHA 99.2 97.4 98.2 2.49 2.56 3.72 3.82 0.48,BHA 39.7 38.3 96.6 1.90 4.97 1.90 4.97 0.54,IONOX-100 104.1 99.3 95.4 4.83 4.87 5.45 5.49 0.69,IONOX-100 41.7 40.7 97.7 3.49 8.56 4.90 12.0 1.32,BHT 101.5 87.9 86.6 4.63 5.27 4.90 5.58 0.70,BHT 40.6 34.6 85.2 1.11 3.22 1.17 3.39 0.37,a See Ta ble 983.15A for identification of antioxidants.,b Antioxidant values measured to 4 significa……
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