酿酒科技
釀酒科技
양주과기
LIQUOR-MAKING SCIENCE & TECHNOLOGY
2012年
1期
112-115
,共4页
诸葛庆%李博斌%江涛%寿谦%葛乐勇%曾红艳
諸葛慶%李博斌%江濤%壽謙%葛樂勇%曾紅豔
제갈경%리박빈%강도%수겸%갈악용%증홍염
分析方法%高效液相色谱法%黄酒%氨基甲酸乙酯%固相萃取
分析方法%高效液相色譜法%黃酒%氨基甲痠乙酯%固相萃取
분석방법%고효액상색보법%황주%안기갑산을지%고상췌취
analytic methods%HPLC%yellow rice wine%ethyl carbamate%solid -phase extraction
建立一种反相高效液相色谱法测定黄酒中氨基甲酸乙酯的方法。样品经固相萃取柱净化后衍生,采用反相C18色谱柱XB—Cfsf4.6mm×250mm,5μm),以乙腈-0.02moL/L乙酸纳水溶液为流动相进行梯度洗脱,流速为lmL/min;设定荧光检测器中激发波长为233nm,发射波长为600nm,对黄酒中的氨基甲酸乙酯进行检测。结果表明,在50.0-250.0μg/L添加量范围内,平均回收率为92.9%,相对标准偏差为4.5%(n=6)。方法的检出限为10μg/L,线性范围为100~1500μg/L(R=0.9995),测定结果与标准气相色谱一质谱法基本相同。所建立的方法可以作为黄酒中氨基甲酸乙酯的检测方法。
建立一種反相高效液相色譜法測定黃酒中氨基甲痠乙酯的方法。樣品經固相萃取柱淨化後衍生,採用反相C18色譜柱XB—Cfsf4.6mm×250mm,5μm),以乙腈-0.02moL/L乙痠納水溶液為流動相進行梯度洗脫,流速為lmL/min;設定熒光檢測器中激髮波長為233nm,髮射波長為600nm,對黃酒中的氨基甲痠乙酯進行檢測。結果錶明,在50.0-250.0μg/L添加量範圍內,平均迴收率為92.9%,相對標準偏差為4.5%(n=6)。方法的檢齣限為10μg/L,線性範圍為100~1500μg/L(R=0.9995),測定結果與標準氣相色譜一質譜法基本相同。所建立的方法可以作為黃酒中氨基甲痠乙酯的檢測方法。
건립일충반상고효액상색보법측정황주중안기갑산을지적방법。양품경고상췌취주정화후연생,채용반상C18색보주XB—Cfsf4.6mm×250mm,5μm),이을정-0.02moL/L을산납수용액위류동상진행제도세탈,류속위lmL/min;설정형광검측기중격발파장위233nm,발사파장위600nm,대황주중적안기갑산을지진행검측。결과표명,재50.0-250.0μg/L첨가량범위내,평균회수솔위92.9%,상대표준편차위4.5%(n=6)。방법적검출한위10μg/L,선성범위위100~1500μg/L(R=0.9995),측정결과여표준기상색보일질보법기본상동。소건립적방법가이작위황주중안기갑산을지적검측방법。
A reverse phase HPLC method for the determination of ethyl carbamate in yellow rice wine had been developed. Wine samples were firstly pretreated by solid-phase extraction,ethyl carbamate was separated on a XB- CL8 (4.6mm×250 mm,5 μm) by using gradient elution (acetonitrile and 0.02 moL/L sodium acetate as the mobile phase) at a flow rate of lmL/min and detected by a fluorescence detector (kex=233 nm, hem=600 nm). At the spike levels of 50.0,100.0 and 250.0μg/L, the average recovery for ethyl carbamate was 92.9% with RSD as 4.5 % (n = 6), the detection limit was 10 μg/L, and the linear range was from 100-500μg/L(R=0.9995.The determination results by this method were almost the same as those by GCMS. Therefore, this method could be use to determine ethyl carbamate in yellow rice wine.