摘要
目的建立固相萃取-高效液相色谱法同时测定化妆品中香兰素和乙基香兰素的方法。方法样品经酸性乙腈提取后,采用固相萃取小柱HLB净化,洗脱液经氮气流吹干后用0.1%甲酸-乙腈(25∶75,V/V)溶液溶解,以0.1%甲酸-乙腈(25∶75,V/V)为流动相,经Shim-pack XR-ODSⅡ柱(75 mm×2.0 mm,2.2μm)分离后280 nm波长下检测,外标法定量。结果在0.02 mg/L^2.0 mg/L时线性相关系数>0.999 0,香兰素和乙基香兰素的检出限分别为0.02 mg/kg和0.03 mg/kg,最低定量限分别为0.07 mg/kg和0.10 mg/kg,3个加标浓度的回收率为87.0%~98.2%,相对标准偏差为1.9%~4.6%。结论本法具有简便、快速、准确、干扰少的优点,可用于化妆品中香兰素和乙基香兰素的同时测定。
Objective To develop a method for the simultaneous determination of vanillin and ethyl vanillin in cosmetics by high - performance liquid chromatography with solid - phase extraction. Methods Vanillin and ethyl vanillin in cosmetics sam- pies were extracted with acidified acetonitrile, cleaned up with HLB cartridges, then evaporated to nearly dryness under a nitro- gen stream, and finally dissolved in a mixed solution of 0.1% （V/V） formic acid - acetonitrile（25 ： 75, V/V）. Chromatograph- ic separation was carried out on a Shim - pack XR - ODS Ⅱ column （75 mm× 2.0 mm, 2.2 μm） by using a mixed solution of 0.1% （V/V） formic acid - acetonitrile（25 ： 75, V/V） as the mobile phase in isocratic elution. The detection was performed at 280 nm and quantification was based on the external standard curves. Results Linearity calibration curves were obtained, with correlation coefficients greater than 0.999 0, when the concentrations of vanillin and ethyl vanillin were within 0.02 mg/L - 2.0 mg/L. The lowest standard deviations were within 1.9% -4.6%. The limits of detection（LODs） in cosmetics samples were 0.02 mg/kg and 0.03 mg/kg, the method limits of quantification（LOQs） were 0.07 mg/kg and 0.10 mg/kg for vanillin and ethyl vanillin, respectively. The average recoveries at three spiked levels were in the range of 87.0% - 98.2% , with the relative standard deviation of 1.9% -4.6%. Conclusion The method is simple, rapid, accurate and with less interference, and it can be applied to the simultaneous determination of vanillin and ethyl vanillin in cosmeties samples.
作者
陈波
徐明敏
金米聪
CHEN Bo XU Ming- min JIN Mi -cong(Beilun District Center for Disease Control and Prevention, Ningbo, Zhefiang 315010, China)
出处
《中国卫生检验杂志》
CAS
2017年第10期1389-1392,1395,共5页
Chinese Journal of Health Laboratory Technology
基金
宁波市科技创新团队项目(2015C110019)
浙江省微量有毒化学物健康风险评估技术研究重点实验室开放基金(2014003)
关键词
高效液相色谱法
固相萃取
香兰素
乙基香兰素
化妆品
High - performance liquid chromatography
Solid - phase extraction
Vanillin
Ethyl vanillin
Cosmetics
