一测多评法同时测定薏苡仁油中4种甘油三酯类抗肿瘤成分的含量
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篇名: 一测多评法同时测定薏苡仁油中4种甘油三酯类抗肿瘤成分的含量
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摘要: 目的:建立同时测定薏苡仁油中4种甘油三酯类抗肿瘤成分含量的方法。方法:采用高效液相色谱-蒸发光散射检测器法(HPLC-ELSD)。色谱柱为Inertsil ODS-3 C18,流动相为乙腈-异丙醇 (57 ∶ 43,V/V),流速为1.0 mL/min,柱温为30 ℃,进样量为10 μL;蒸发光散射检测器漂移管温度为70 ℃,气体流速为2 L/min。以甘油三油酸酯为内标,分别计算其与甘油三亚油酸酯、1,2-亚油酸-3-棕榈酸甘油酯、1-棕榈酸-2-油酸-3-亚油酸甘油酯的相对校正因子(RCF),通过RCF计算薏苡仁油中上述3种成分的含量,同时采用外标法测定薏苡仁油中这4种成分的含量,比较一测多评法和外标法的含量测定结果。结果:甘油三亚油酸酯、1,2-亚油酸-3-棕榈酸甘油酯、1-棕榈酸-2-油酸-3-亚油酸甘油酯、甘油三油酸酯进样量检测线性范围分别为0.15~4.50、0.15~4.50、0.35~10.50、0.35~10.50 μg(r≥0.999 5);定量限分别为0.13、0.06、0.07、0.12 μg,检测限分别为0.04、0.02、0.02、0.03 μg;精密度、稳定性、重复性试验的RSD<2.0%(n=6);加样回收率为95.43%~102.67%( RSD<2.0%,n=6)。甘油三亚油酸酯、1,2-亚油酸-3-棕榈酸甘油酯、1-棕榈酸-2-油酸-3-亚油酸甘油酯的平均RCF分别为0.31、0.88、1.21。在不同试验条件下,RCF重现性良好。一测多评法和外标法的含量测定结果比较,差异无统计学意义(P>0.05)。结论: 该方法操作简单快捷、结果准确可靠,可用于薏苡仁油中甘油三亚油酸酯、1,2-亚油酸-3-棕榈酸甘油酯、1-棕榈酸-2-油酸-3-亚油酸甘油酯、甘油三油酸酯4种抗肿瘤成分含量的同时测定。
ABSTRACT: OBJECTIVE: To establish a method for simultaneous determination of 4 triglyceride anti-tumor components in Coix lacryma seed oil. METHODS: HPLC-ELSD was adopted. The determination was performed on Inertsil ODS-3 C18 column with mobile phase consisted of acetonitrile-isopropanol (57 ∶ 43, V/V) at the flow rate of 1.0 mL/min. The column temperature was 30 ℃, and the sample size was 10 μL. Evaporative light scattering detector was used, the drift tube temperature was 70 ℃, and the gas flow rate was 2 L/min. Using glycerol trioleateas internal standard, relative correction factors (RCF) of linolein trilinolein, 1,2-linoleic acid-3-palmitic acid glyceride and 1-palmitic acid-2-oleic acid-3-linoleic acid glyceride were calculated respectively. The contents of above 3 components in C. lacryma seed oil were calculated by RCF. The contents of 4 components in C. lacryma seed oil were determined by external standard. The results of content determination by quatitative analysis of multi-components by single marker (QAMS) were compared with external standard method. RESULTS: The linear ranges were 0.15-4.50 μg for linolein trilinolein, 0.15-4.50 μg for 1,2-linoleic acid-3-palmitate, 0.35-10.50 μg for 1-palmitic acid-2-oleic acid-3-linoleic acid glyceride, 0.35-10.50 μg for glycerol trioleate (r≥0.999 5). The limits of quantification were 0.13, 0.06, 0.07, 0.12 μg. The limits of detection were 0.04, 0.02, 0.02, 0.03 μg, respectively. RSDs of precision, stability, and repeatability tests were less than 2.0%(n=6). The average recoveries were 95.43%-102.67%(RSD<2.0%, n=6). Average RCFs of linolein trilinolein, 1,2- linoleic acid-3-palmitic acid glyceride and 1-palmitic acid-2- oleic acid-3-linoleic acid glyceride were 0.31, 0.88, and 1.21, respectively. RCFs reproducibility was perfect under different experiment conditions. There was no significant difference in results of content determination between QAMS and external standard method (P>0.05). CONCLUSIONS: The method is simple, rapid, accurate and reliable. It is used for simultaneous determination of linolein trilinolein, 1, 2-linoleic acid-3-palmitate, 1-palmitic acid-2-oleic acid-3-linoleic acid glyceride and glycerol trioleateas in C. lacryma seed oil.
期刊: 2019年第30卷第10期
作者: 吴人杰,许平翠,寿旦,李功华,兰青山,王娜妮
AUTHORS: WU Renjie,XU Pingcui,SHOU Dan,LI Gonghua,LAN Qingshan,WANG Nani
关键字: 高效液相色谱法;一测多评法;薏苡仁油;甘油三酯类成分;相对校正因子
KEYWORDS: HPLC; Quatitative analysis of multi-components by single marker; Coix lacryma seed oil; Triglyceride; Relative correction factor
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