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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。
Using ultra-high performance liquid chromatography (UPLC) technology, the rapid and simultaneous detection of limonin and numilin in kumquat was established. The sample was separated by sonication with dichloromethane and separated on an ACQUITY UPLC TMBEHC18 column (2.1 mm × 100 mm, 1.7 μm). The mobile phase consisted of acetonitrile-water (45:55) with gradient elution at a flow rate of 0.3 mL / Detection wavelength of 215nm. Limonin and nimolin can be achieved within 3min at the same time separation and determination. There was a good linear relationship between limonin and niminlin in the range of 1 ~ 1780μg / mL and 1 ~ 1720μg / mL (R2 = 0.9999). The detection limits were 1.65μg / g and 1.28μg / g, Rates were 97.19% ~ 100.06% and 95.35% ~ 99.83%, respectively. The relative standard deviations (RSDs) were less than 5%. This method has the advantages of short analysis time, high sensitivity, convenient operation and accurate results. It is suitable for the simultaneous determination of limonin and nimolimin in kumquat.