CAJ | 학술논문

采用超高压液相方法检测鱼油中的二十碳五烯酸乙酯(EPA-EE)和二十二碳六烯酸乙酯(DHA-EE),采用UPLC BEH C18(2.1 mm×50 mm,1.7滋m)色谱柱,考察了流动相有机相比例、流速及柱温对鱼油中EPA-EE和DHA-EE分离的影响,确定了最佳色谱条件:等度洗脱,流动相为乙腈-水(80∶20,体积比),流速0.5 mL/min,柱温30℃,检测波长220 nm.该方法下,EPA-EE和DHA-EE分别在10.4滋g/mL~209滋g/mL、10.3滋g/mL~207滋g/mL范围内浓度和面积呈现良好的线性关系,相关系数r分别为0.9994和0.9997;EPA-EE和DHA-EE的方法的检测限为4 ng和6 ng,定量限分别为10 ng和15 ng,精密度试验RSD(n=6)分别为1.09%和0.34%,重复性试验RSD(n=6)分别为1.54%和1.25%,平均回收率分别为102.26%(RSD=1.33%)和96.64%(RSD=1.05%).本方法快速、简单、可靠、灵敏、重复性好,可用于鱼油中EPA-EE和DHA-EE的快速检测.
채용초고압액상방법검측어유중적이십탄오희산을지(EPA-EE)화이십이탄륙희산을지(DHA-EE),채용UPLC BEH C18(2.1 mm×50 mm,1.7자m)색보주,고찰료류동상유궤상비례、류속급주온대어유중EPA-EE화DHA-EE분리적영향,학정료최가색보조건:등도세탈,류동상위을정-수(80∶20,체적비),류속0.5 mL/min,주온30℃,검측파장220 nm.해방법하,EPA-EE화DHA-EE분별재10.4자g/mL~209자g/mL、10.3자g/mL~207자g/mL범위내농도화면적정현량호적선성관계,상관계수r분별위0.9994화0.9997;EPA-EE화DHA-EE적방법적검측한위4 ng화6 ng,정량한분별위10 ng화15 ng,정밀도시험RSD(n=6)분별위1.09%화0.34%,중복성시험RSD(n=6)분별위1.54%화1.25%,평균회수솔분별위102.26%(RSD=1.33%)화96.64%(RSD=1.05%).본방법쾌속、간단、가고、령민、중복성호,가용우어유중EPA-EE화DHA-EE적쾌속검측.
@@@@The article is researching determination of eicosapentaenoic acid ethyl ester (EPA -EE) and docosahexaenoic acid ethyl ester (DHA-EE) in Fish Oil by Ultra performance liquid chromatography(UPLC). The analysis was performed on an Acquity UPLC BEH C18 column (2.1 mm×50 mm, 1.7μm). The influence of flow rate, the proportion of organic phase in mobile phase, and column temperature on the separation of EPA-EE and DHA-EE in fish oil was comprehensively studied. The optimal separation condition was as follows:a mobile phase consisting ofacetonitrileandwater (80∶20,V/V)withaisocraticelutionprofile,UV detection wavelength at 220 nm, 0.5 mL/min of flow rate for mobile phase, 30℃of column temperature. On the above condition, good linearity between response (peak area) and concentration was found over a concentration range of 10.4μg/mL~209μg/mL for EPA-EE, and 10.3μg/mL~207μg/mL for DHA-EE respectively. And the correlation coefficient of the calibration curve was 0.999 4 for EPA-EE, and 0.999 7 for DHA-EE respectively. The limits of detection (S/N>3) were 4ng for EPA-EE and 6ng for DHA-EE respectively. The limits of quantification (S/N>10) were 10ng for EPA-EE and 15ng for DHA-EE respectively. The average recovery rates of EPA-EE and DHA-EE were 102.26% (RSD 1.33%) and 96.64% (RSD 1.05%) respectively. The RSD of repetition was 1.54%(n=6) for EPA-EE and 1.25%(n=6) for DHA-EE. This method was simple, accurate and sensitive with a good reproducibility. It is suitable for fast detection ofEPA-EEandDHA-EEinfishoil.