摘要
采用超高效液相色谱结合荧光检测建立了美白化妆品中杜鹃醇的分析方法，并采用液相色谱-串联质谱法进行确证。化妆品试样以5％三氯乙酸-乙腈混合溶液（70：30）超声提取15min，离心过膜后，采用通用型的反相c。。色谱柱进行分离，以0．1％甲酸水-乙腈（75：25）为流动相，荧光检测器（λex／λem=280nm／315nm）检测，外标法定量；质谱确证采用水（含0．01％氨水）和乙腈作为流动相梯度洗脱，电喷雾负离子模式电离，多反应监测模式检测。结果显示，杜鹃醇在0．05-1．0mg／L范围内线性关系良好，相关系数为0．9996，方法的定量下限为2．5mg／kg。面膜、乳霜、乳液和爽肤水等样品在加标浓度为5．O，10，25mg／kg时的回收率为86．5％-103．4％，RSD（n=6）为1．1％～3．4％。该方法简便、灵敏，加标回收率和重现性良好，可用于化妆品中杜鹃醇的检测及其含量水平的普查。
A method was developed for the determination of rhododendrol（RD） in whitening cosmetics by ultra high performance liquid chromatography （UPLC） coupled with fluorescence detection, and the verification analysis was achieved by LC - MS/MS. The samples were extracted with 5% trichloroaeetie acid- acetonitrile mixed solution （70 ： 30）. After centrifugation and filtration, the a- nalysis of RD was performed by UPLC with a conventional C18 column, using 0. 1% formic acid - aeetonitrile （75 ： 25 ） as mobile phase. Fluorescence detection wavelengths were set at A ox/A om = 280 nm/315 nm. The verification analysis was performed by LC - MS/MS using water（ spiked 0.01% ammonia） -acetonitrile as mobile phase by gradient elution. The electrospray was operated in the negative mode（ ESI- ） under the multiple reaction monitoring（MRM） mode. A good linearity was ob- tained in the range of 0. 05 -1.0 mg/L, with a correlation coefficient（r） of 0. 999 6, and the limit of quantitation （ LOQ, SIN = 10） was 2. 5 mg/kg for whitening cosmetics. The recoveries of RD ranged from 86. 5% to 103.4% with relative standard deviations（ RSDs, n =6） of 1.1% - 3.4% at spiked levels of 5.0, 10, 25 mg/kg in facial mask, cream, lotion and skin water. This method.is simple, rapid and accurate, and is suitable for the detection of RD in whitening cosmetics.
出处
《分析测试学报》
CAS
CSCD
北大核心
2014年第7期792-797,共6页
Journal of Instrumental Analysis
基金
国家质检总局科技计划项目(2013IK165)
关键词
超高效液相色谱法
荧光检测
液相色谱-串联质谱
美白化妆品
杜鹃醇
ultra high performance liquid chromatography （UPLC）
fluorescence detection
liquid chromatography-tandem mass spectrometry（ LC -MS/MS）
whitening cosmetics
rhododendrol
