目的:建立了高效液相色谱同时测定山茶油中没食子酸、阿魏酸2种多酚类化合物的分析方法,并对不同产地样品中这两种多酚类成分进行测定,为评价其质量提供依据。方法:样品经过两次萃取后,合并上清液用甲醇定容;萃取液过滤膜后进行色谱分...目的:建立了高效液相色谱同时测定山茶油中没食子酸、阿魏酸2种多酚类化合物的分析方法,并对不同产地样品中这两种多酚类成分进行测定,为评价其质量提供依据。方法:样品经过两次萃取后,合并上清液用甲醇定容;萃取液过滤膜后进行色谱分析。色谱条件:ZORBAX SB-C18反相柱(4.6 mm × 150 mn,5.0 μm);DAD检测波长280 nm;柱温35℃;流量1.0 mL/min;进样量10 μL;流动相为0.5%乙酸(A) + 乙腈(B)。结果:没食子酸、阿魏酸在浓度范围为25~500 μg/mL都具有较好的线性关系,其方程为:没食子酸Y = 21.44X − 14.821 (R2 = 0.9993);阿魏酸Y = 23.091X − 65.104 (R2 = 0.9992),没食子酸、阿魏酸的检出限分别为0.2 μg/mL,0.6 μg/mL (S/N = 3),样品的加标回收率为96.94% (没食子酸)、92.56% (阿魏酸),且相对标准偏差(RSD)均小于3%。该方法具有准确快速、灵敏度高,满足山茶油中多酚类化合物的检测要求。Objective: To establish an analytical method using high-performance liquid chromatography (HPLC) for the simultaneous determination of gallic acid and ferulic acid, two phenolic compounds, in camellia oil from different geographical origins, and to measure the contents of these two phenolic components in samples from different regions as a basis for evaluating their quality. Methods: After two extractions, the supernatants were combined and diluted to volume with methanol;the extract was then filtered through a membrane before chromatographic analysis. Chromatographic conditions: ZORBAX SB-C18 reversed-phase column (4.6 mm × 150 mm, 5.0 μm);DAD detection wavelength at 280 nm;column temperature at 35˚C;flow rate of 1.0 mL/min;injection volume of 10 μL;mobile phase consisting of 0.5% acetic acid (A) and acetonitrile (B). Results: Gallic acid and ferulic acid showed good linearity in the concentration range from 25 to 500 μg/mL, with the equations: gallic acid Y = 21.44X − 14.821 (R² = 0.9993);ferulic acid Y = 23.091X − 65.104 (R² = 0.9992). The detection limits for gallic acid and ferulic acid were 0.2 μg/mL and 0.6 μg/mL, respectively (S/N = 3). Spike recoveries were 96.94% for gallic acid and 92.56% for ferulic acid, with relative standard variances (RSD) of less than 3% for both. This method meets the requirements for the detection of phenolic compounds in camellia oil by being accurate, rapid and highly sensitive.展开更多
文摘目的:建立了高效液相色谱同时测定山茶油中没食子酸、阿魏酸2种多酚类化合物的分析方法,并对不同产地样品中这两种多酚类成分进行测定,为评价其质量提供依据。方法:样品经过两次萃取后,合并上清液用甲醇定容;萃取液过滤膜后进行色谱分析。色谱条件:ZORBAX SB-C18反相柱(4.6 mm × 150 mn,5.0 μm);DAD检测波长280 nm;柱温35℃;流量1.0 mL/min;进样量10 μL;流动相为0.5%乙酸(A) + 乙腈(B)。结果:没食子酸、阿魏酸在浓度范围为25~500 μg/mL都具有较好的线性关系,其方程为:没食子酸Y = 21.44X − 14.821 (R2 = 0.9993);阿魏酸Y = 23.091X − 65.104 (R2 = 0.9992),没食子酸、阿魏酸的检出限分别为0.2 μg/mL,0.6 μg/mL (S/N = 3),样品的加标回收率为96.94% (没食子酸)、92.56% (阿魏酸),且相对标准偏差(RSD)均小于3%。该方法具有准确快速、灵敏度高,满足山茶油中多酚类化合物的检测要求。Objective: To establish an analytical method using high-performance liquid chromatography (HPLC) for the simultaneous determination of gallic acid and ferulic acid, two phenolic compounds, in camellia oil from different geographical origins, and to measure the contents of these two phenolic components in samples from different regions as a basis for evaluating their quality. Methods: After two extractions, the supernatants were combined and diluted to volume with methanol;the extract was then filtered through a membrane before chromatographic analysis. Chromatographic conditions: ZORBAX SB-C18 reversed-phase column (4.6 mm × 150 mm, 5.0 μm);DAD detection wavelength at 280 nm;column temperature at 35˚C;flow rate of 1.0 mL/min;injection volume of 10 μL;mobile phase consisting of 0.5% acetic acid (A) and acetonitrile (B). Results: Gallic acid and ferulic acid showed good linearity in the concentration range from 25 to 500 μg/mL, with the equations: gallic acid Y = 21.44X − 14.821 (R² = 0.9993);ferulic acid Y = 23.091X − 65.104 (R² = 0.9992). The detection limits for gallic acid and ferulic acid were 0.2 μg/mL and 0.6 μg/mL, respectively (S/N = 3). Spike recoveries were 96.94% for gallic acid and 92.56% for ferulic acid, with relative standard variances (RSD) of less than 3% for both. This method meets the requirements for the detection of phenolic compounds in camellia oil by being accurate, rapid and highly sensitive.
