HPLC外标法测定亚麻籽油中4种环肽含量的研究
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摘要
以环肽标准样品定性,采用外标法定量,建立了HPLC测定亚麻籽油中环肽A、环肽C、环肽D和环肽E的方法。采用固相萃取法提取亚麻籽油中的环肽,用Diamonsil C18色谱柱,以乙腈和水为流动相梯度洗脱,柱温35℃,二极管阵列检测器在波长214 nm处进行检测,30 min内完成对4种环肽的分离检测。结果表明:该方法的线性范围为10~160μg/m L,相关系数大于等于0.999 5;环肽A、环肽C、环肽D、环肽E的平均加标回收率分别为94.62%、92.25%、84.07%和100.14%。用该方法测定不同工艺制取的亚麻籽油中环肽的含量,发现未经过精炼的亚麻籽油中环肽含量高于市售亚麻籽油的,其中,冷榨工艺比热榨工艺更能保留亚麻籽油中的环肽。
The determination of contents of four cyclolinopeptides in flaxseed oil was studied by HPLC external standard method. Solid phase extraction( SPE) was used to extract cyclolinopeptides from flaxseed oil. The HPLC analysis conditions were obtained as follows: Diamonsil C18 chromatographic column,gradient elution using acetonitrile and water as the mobile phase,column temperature 35 ℃,photodiode array detector wavelength 214 nm. The contents of four cyclolinopeptides could be determined within 30 min under above conditions. The results showed that the linear range and correlation coefficient of the method were 10-160 μg / m L and higher than 0. 999 5 respectively. The average recoveries of standard addition of cyclolinopeptide A,cyclolinopeptide C,cyclolinopeptide D and cyclolinopeptide E were94. 62%,92. 25%,84. 07% and 100. 14%,separately. Using this method,it was discovered that the content of cyclolinopeptides in flaxseed oil without refining was higher than that in commerial flaxseed oil,and cold-pressing process could better preserve the cyclolinopeptides than hot-pressing process.
The determination of contents of four cyclolinopeptides in flaxseed oil was studied by HPLC external standard method. Solid phase extraction( SPE) was used to extract cyclolinopeptides from flaxseed oil. The HPLC analysis conditions were obtained as follows: Diamonsil C18 chromatographic column,gradient elution using acetonitrile and water as the mobile phase,column temperature 35 ℃,photodiode array detector wavelength 214 nm. The contents of four cyclolinopeptides could be determined within 30 min under above conditions. The results showed that the linear range and correlation coefficient of the method were 10-160 μg / m L and higher than 0. 999 5 respectively. The average recoveries of standard addition of cyclolinopeptide A,cyclolinopeptide C,cyclolinopeptide D and cyclolinopeptide E were94. 62%,92. 25%,84. 07% and 100. 14%,separately. Using this method,it was discovered that the content of cyclolinopeptides in flaxseed oil without refining was higher than that in commerial flaxseed oil,and cold-pressing process could better preserve the cyclolinopeptides than hot-pressing process.
引文
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[13]孙浩冉,姚虹,史高峰.脱脂亚麻籽中一种环肽类成分的研究[J].安徽农业科学,2010,38(4):1693-1694.
[14]GUI B,SHIM Y Y,DATLA R S S,et al.Identification and quantification of cyclolinopeptides in five flaxseed cultivars[J].J Agric Food Chem,2012,60(35):8571-8579.
[15]杨金娥,黄庆德,周琦,等.冷榨和热榨亚麻籽油挥发性成分比较[J].中国油料作物学报,2013,35(3):321-325.
[2]BRHL L,MATTHUS B,SCHEIPERS A,et al.Bitter off-taste in stored cold-pressed linseed oil obtained from different varieties[J].Eur J Lipid Sci Technol,2008,110:625-631.
[3]王荣栋,尹经章.作物栽培学[M].北京:高等教育出版社,2005.
[4]杨金娥,黄庆德,郑畅,等.烤籽温度对压榨亚麻籽油品质的影响[J].中国油脂,2011,36(6):28-31.
[5]GUI B,SHIM Y Y,REANEY M J T.Distribution of cyclolinopeptides in flaxseed fractions and products[J].J Agric Food Chem,2012,60(35):8580-8589.
[6]BENEDETTI E,PEDONE C.Cyclolinopeptide A:inhibitor,immunosuppressor or other?[J].J Peptide Sci,2005,11(5):268-272.
[7]MORITA H,SHISHIDO A,MATSUMOTO T,et al.Cyclolinopeptides B-E,new cyclic peptides from Linum usitatissimum[J].Tetrahedron,1999,55:967-976.
[8]MATSUMOTO T,SHISHIDO A,MORITA H,et al.Cyclolinopeptides F-I,cyclic peptides from linseed[J].Phytochemistry,2001,57(2):251-260.
[9]RUCHALA P,PICUR B,LISOWSKI M,et al.Synthesis,conformation,and immunosuppressive activity of CLX and its analogues[J].Biopolymers,2003,70:497-511.
[10]CHOO W S,BIRCH J,DUFOUR J P.Physicochemical and quality characteristics of cold-pressed flaxseed oils[J].J Food Compost Anal,2007,20(3):202-211.
[11]BRHL L,MATTHUS B,FEHLING E,et al.Identification of bitter off-taste compounds in the stored cold pressed linseed oil[J].J Agric Food Chem,2007,55(19):7864-7868.
[12]ALADEDUNYE F A,SOSINSKA E,PRZYBYLSKI R.Flaxseed cyclolinopeptides:analysis and storage stability[J].J Am Oil Chem Soc,2013,90:419-428.
[13]孙浩冉,姚虹,史高峰.脱脂亚麻籽中一种环肽类成分的研究[J].安徽农业科学,2010,38(4):1693-1694.
[14]GUI B,SHIM Y Y,DATLA R S S,et al.Identification and quantification of cyclolinopeptides in five flaxseed cultivars[J].J Agric Food Chem,2012,60(35):8571-8579.
[15]杨金娥,黄庆德,周琦,等.冷榨和热榨亚麻籽油挥发性成分比较[J].中国油料作物学报,2013,35(3):321-325.