1. 广州市质量监督检测研究院
2. 国家化妆品质量监督检验中心,广州
3. 北京市海淀区产品质量监督检验所
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陈立伟, 冼燕萍, 穆同娜, 等. 超高效液相色谱法同时测定护肤品中的川芎嗪、甘草苷与荷叶碱[J]. 分析测试学报, 2013,32(12):1421-1426.
Determination of Tetramethylpyrazine,Liquiritin and Nuciferine in Skin Care Products by Ultra-high Performance Liquid Chromatography[J]. 2013,32(12):1421-1426.
建立了一种同时测定水剂、乳液、膏霜、啫喱类护肤品中川芎嗪、甘草苷和荷叶碱的超高效液相色谱(UPLC)分析方法。不同基质样品经甲醇超声提取后,采用Waters BEH C18色谱柱(2.1 mm×50 mm,1.7 μm),以0.05%磷酸水溶液-乙腈为流动相进行梯度洗脱分离,二极管阵列检测器检测,结合保留时间和光谱图定性,以标准曲线定量。实验结果表明,3种待测物在0.05~50.0 mg/L浓度范围内线性关系良好,相关系数为0.999 4 ~ 0.999 9;川芎嗪、甘草苷和荷叶碱的方法检出限(S/N=3)分别为0.6、0.6、0.3 mg/kg,方法定量下限(S/N=10)分别为2.0、2.0、1.0 mg/kg;加标水平为1~200 mg/kg时,3种待测物的平均回收率为85.6%~98.2%,相对标准偏差(RSD,n=6)为1.1%~6.1%。该法前处理简单、回收率高、精密度好,适用于不同护肤品中川芎嗪、甘草苷和荷叶碱的测定。
A method was established for the simultaneous determination of tetramethylpyrazine,liquiritin and nuciferine in toner,emulsion,cream and gel skin care products by ultra-high performance liquid chromatography with a diode array detector(UPLC-PDA).The different kinds of cosmetic samples were extracted with methanol by ultrasonic wave,then the extracts were centrifuged,filtrated,and analyzed by UPLC-PDA on a Waters BEH C18 column(2.1 mm×50 mm,1.7 μm),employing acetonitrile-0.05% phosphoric acid aqueous solution as mobile phase by gradient elution.The targets were qualitatively determined by retention time,and confirmed by ultraviolet spectra.The external standard method was applied for the quantification analysis.The results indicated that the linear correlation coefficients of three targets ranged from 0.999 4 to 0.999 9 within the linear range of 0.05-50.0 mg/L.The detection limits(S/N=3) of tetramethylpyrazine,liquiritin and nuciferine were 0.6,0.6,0.3 mg/kg,and the limits of quantitation(S/N=10) were 2.0,2.0,1.0 mg/kg,respectively.The spiked recoveres of three compounds at spiked levels of 1-200 mg/kg were between 85.6% and 98.2%,with RSDs(n=6) of 1.1%-6.1%.The results showed that this method was stable,accurate and precise,and could be used to assay the three mentioned compounds in different skin care products.
护肤品川芎嗪甘草苷荷叶碱超高效液相色谱法
skin care productstetramethylpyrazineliquiritinnuciferineultra high performance liquid chromatography(UPLC)
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