AOAC Official Method 977
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F7B0D547E9424098A6A9F3AB810DB424 |
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0.01 |
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1 |
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日期： |
2024-7-30 |
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28.3.01,AOAC Official Method 977.09,b-Asarone in Wines,Gas Chromatographic Method,First Action 1977,Final Action 1984,A. Apparatus and Reagents,(a) Gas chromatograph.—With flame ionization detector and,1.8 m ′2 (id) mm glass or stainless steel column packed with 10%,SP-1000 (No. 01-1872, Supelco, Inc.) on Chromosorb W HP,80/100. Typical operating conditions—temperatures (°C): column,180, detector and injection port 200; He carrier gas (with purifier,filter) flow rate 40 mL/min. Retention times of ethyl palmitate and,b-asarone are ca 5 min and 6 min, respectively.,(b) Ethyl palmitate internal standard solution.—Prepare,1 mg/mL solution in hexane.,(c) b-Asarone standard solution.—Prepare 1 mg/mL solution in,alcohol. (b-Asarone is available on special order as No. TT150 from,Fritzsche, Dodge, & Olcott, Inc., 76 Ninth Ave, New York, NY,10011, USA.),B. Preparation of Standard Curve,Prepare standard solutions containing 1, 2, 3, 4, and 5 mg,b-asarone/L by adding 100, 200, 300, 400, and 500 mL standard solution,to separate 100 mL volumetric flasks containing ca 90 mL,20% alcohol. Mix, dilute to volume with 20% alcohol, and remix.,Transfer entire solution, rinsing with 50mLH2O, to simple distilling,apparatus and distil ca 100 mL. Transfer distillate to 250mLseparator,add 100 mL saturated solution of NaCl, and mix. Add 10 mL,hexane, shake vigorously 2 min, and let separate. Drain and discard,aqueous solution. Dry inside of drain tube of separator with tissue or,pipe cleaner. Collect hexane in calibrated centrifuge tube,(10 ± 0.5 mL should be recovered). Add 200 mL ethyl palmitate internal,standard solution and mix well. Chromatograph 5 mL of each,extract and plot standard curve of original concentration of mg,b-asarone/L against peak height ratio of b-asarone:ethyl palmitate.,C. Determination,Distil 100 mL test portion and 50 mL H2O, collecting 100 mL distillate.,Transfer distillate, extract with 10mLhexane, and chromatograph,5 mL as in B. Check for presence of b-asarone and ethyl palmitate. If,there is no b-asarone peak, b-asarone is not present at 0.5 mg/L level. If,b-asarone is present in range of standard curve and no ethyl palmitate is,present, add 200mLethyl palmitate internal standard solution to hexane,extract, mix, and rechromatograph. Use ratio of peak heights to determine,b-asarone concentration from standard curve. If b-asarone peak is,off scale, dilute hexane extract with hexane to 1–5 mg b-asarone/L, add,internal standard solution, mix, and rechromatograph. If peak is present,in extract with same retention time as ethyl palmitate, use peak heights,directly to determine b-asarone concentration from standard curve prepared,from peak heights.,Reference: JAOAC 59, 675(1976).,CAS-5273-86-9 (b-asarone),. 2000 AOAC INTERNATIONAL……
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