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超高效液相色谱法快速并同时检测金柑中柠檬苦素和诺米林
Study on Rapid Simultaneous Determination of Limonin and Nomilin in Kumquat Using Ultra-Performance Liquid Chromatography
【摘要】 采用超高效液相色谱(UPLC)技术,建立金柑中柠檬苦素和诺米林的快速、同时检测技术。样品经二氯甲烷超声波提取,ACQUITYUPLCTMBEHC18色谱柱(2.1mm×100mm,1.7μm)分离,以乙腈-水(45∶55)为流动相,梯度洗脱,流速0.3mL/min,柱温35℃,检测波长215nm。柠檬苦素和诺米林可在3min内实现同时分离、测定。柠檬苦素和诺米林分别在1~1780μg/mL和1~1720μg/mL范围内线性关系良好(R2=0.9999),方法检出限分别为1.65μg/g和1.28μg/g,加标回收率分别为97.19%~100.06%和95.35%~99.83%,相对标准偏差(RSD)均小于5%。本法分析时间短,灵敏度高,操作方便,结果准确,适用于金柑中柠檬苦素和诺米林的同时测定。
【Abstract】 A method for the rapid simultaneous determination of limonin and nomilin in Kumquat by ultra performance liquid chromatography(UPLC) was developed. The limonin and nomilin in the samples were first extracted with methylene chloride by sonication. The analyses were performed on UPLC with an ACQUITY UPLCTM BEH C18 column(2.1 mm×100 mm,1.7 μm), using acetonitrile-water(45∶55, V/V) as the mobile phase at a flow rate of 0.3 mL/min. The column temperature is measured 35 ℃, with a detection wavelength of 215 nm. The two compounds were effectively separated by gadient elution and detected by PDA in 3 minutes. The Calibration curve were good linear in the range of 1~1 780 μg/mL for limonin and 1~1 720 μg/mL for nomilin, the correlation coefficient were both 0.9999. The limits of detection(LOD) were 1.65 μg/g and 1.28 μg/g. The additon recoveries were 97.19%~100.06% and 95.35%~99.83%, respectively. The relative standard deviations were less than 5%. The result indicated that the method is rapid, sensitive, convenient, accurate and may be used for determination of limonin and nomilin in kumquat.
【Key words】 ultra performance liquid chromatography(UPLC); limonin; nomilin; kumquat;
- 【文献出处】 中国食品学报 ,Journal of Chinese Institute of Food Science and Technology , 编辑部邮箱 ,2013年02期
- 【分类号】TS255.7;O657.72
- 【被引频次】25
- 【下载频次】416