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日用化学工业:2017,Vol.>>Issue(12):719-722
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高效液相色谱法同时测定化妆品中香豆素等15种化合物
高瑞芳,李祥胜
(安徽省食品药品检验研究院,安徽 合肥 230051)
Simultaneous determination of coumarin and other 14 compounds in cosmetics by high performance liquid chromatography
GAO RUI-fang,LI XIANG-sheng
(Anhui Institute for Food and Drug Control, Hefei, Anhui 230051, China)
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投稿时间:2017-09-01    
中文摘要: 建立了同时测定化妆品中香豆素等15种化合物(双香豆素、4-羟基香豆素、香豆素、7-甲氧基香豆素、6-甲基香豆素、8-羟基补骨脂素、补骨脂素、异补骨脂素、8-甲氧基补骨脂素、5-甲氧基补骨脂素、新补骨脂异黄酮、补骨脂二氢黄酮、三甲沙林、欧前胡内酯和异欧前胡内酯)的高效液相色谱分析方法。样品经甲醇超声提取,以10 000 r/min离心5 min,取上清液过滤后测定。采用Phenomenex Luna C18 (2) (250 mm×4.6 mm,5 μm)色谱柱分离,以乙腈-0.1%乙酸溶液为流动相梯度洗脱,流速1.0 mL/min,柱温30 ℃。采用二极管阵列检测器多波长检测(210,250和280 nm),标准曲线法定量。结果表明,香豆素等15种化合物的线性范围为0.1~10.0 mg/L,相关系数均大于0.999,检出限(LOD)为0.1~0.7 mg/kg。在3种加标水平下的平均加标回收率为90.5%~106.4%,相对标准偏差为0.7%~3.4% (n=6)。该方法准确、简便,适用于化妆品中香豆素等15种化合物的测定。
Abstract:A high performance liquid chromatographic (HPLC) method was developed for the simultaneous determination of coumarin and other 14 compounds, including dicoumarol, 4-hydroxycoumarin, 7-methoxycoumarin, 6-methylcoumarin, 8-hydroxypsoralene, psoralen, angelicin, 8-methoxypsoralen, 5-methoxypsoralen, neobavaisoflavone, bavachin, trioxsalen, imperatorin and isoimperatorin. The samples were extracted with methanol under the help of supersonic wave and centrifuged at 10 000 r/min for 5 min. The supernatant was separated on a Phenomenex Luna C18 (2) (250 mm×4.6 mm, 5 μm) column by gradient elution with acetonitrile-0.1% acetic acid solution as mobile phase at a flow rate of 1.0 mL/min and column temperature of 30 ℃. The analysis of 15 compounds was performed by HPLC with diode array detector at the wavelength of 210, 250, 280 nm, respectively. Identification of 15 compounds was achieved by retention time, and quantification analysis was performed by the calibration curve method. The method shows a good linearity in the range of 0.1~10.0 mg/L with correlation coefficients higher than 0.999. The limits of detection (LODs) for the 15 compounds were 0.1-0.7 mg/kg. The mean recoveries at three spiked levels were in the range of 90.5%-106.4% with RSDs of 0.7%-3.4%. The method is accurate and simple, and is suitable for the determination of 15 compounds.
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