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作 者:黄键 张文国[1] 郭桂萍[1] 倪鹏[1] 施锦辉[1] 王金娟[1]
出 处:《理化检验(化学分册)》2017年第11期1318-1321,共4页Physical Testing and Chemical Analysis(Part B:Chemical Analysis)
摘 要:对膏状样品取1.0g,加入四氢呋喃4mL溶解后用甲醇定容至10mL;对乳状、水状及固体样品取1.0g,加入甲醇至近5mL,涡旋振荡1min,用甲醇定容至10mL。将上述试样溶液超声提取15min,离心分层,取上清液,用ZORBAX Eclipse Plus C_(18)色谱柱为分离柱,以甲醇与1.5%(体积分数)乙酸溶液按体积比35∶65组成的混合液为流动相,作色谱分离,在波长280nm处进行紫外检测。测得香兰素和乙基香兰素的质量浓度均在0.5~100mg·L^(-1)内与其对应的峰面积呈线性关系,其检出限(3S/N)均为0.2mg·kg^(-1)。以空白样品为基体,用标准加入法进行回收试验,测得回收率为91.3%~97.0%,测定值的相对标准偏差(n=6)为1.0%~1.7%。For creamy sample,1.0 g was taken and dissolved in 4 mL of tetrahydrofuran,and then its volume was made up to 10 mL with methanol.For emulsion,aqueous or solid sample,1.0 g was taken and methanol was added to make its total volume to near 5 mL,the mixture was shaked for 1 min by swirling.The total volume was then made up to 10 mL with methanol.For either case,the sample solution was extracted ultrasonically for 15 min,and centrifuged for phase separation.The supernatant was taken and chromatographic separation was made by using ZORBAX Eclipse Plus C_(18) column as the separation column and mixture composed of methanol and 1.5%(φ)acetic acid solution(mixed in the volumic ratio of 35 to 65)as the mobile phase.UV-detection at 280 nm was adopted.Linear relationships between values of peak area and mass concentration of vanillin and ethyl vanillin were found in the same range of 0.5-100 mg·L^(-1),with same detection limits(3 S/N)of 0.2 mg·kg^(-1).Test for recovery was made by standard addition method using a blank sample as matrix,values of recovery found were ranged from 91.3% to 97.0%.Values of RSD(n=6)found were in the range of 1.0%-1.7%.
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