摘要
取1.000 g化妆品置于10 mL具塞比色管中,用体积比4∶1的乙腈-四氢呋喃混合液定容,涡旋30 s,超声提取15 min,冷却,过0.45μm滤膜,采用高效液相色谱法测定滤液中视黄醇及其衍生物视黄酸、异视黄酸、视黄醛、视黄醇乙酸酯、羟基频哪酮视黄酸酯、视黄醇丙酸酯、视黄醇视黄酸酯、视黄醇棕榈酸酯的含量。以ZORBAX Eclispse Plus C18色谱柱为固定相,以不同体积比的乙腈-四氢呋喃-5 mmol·L^(−1)乙酸铵溶液的混合液为流动相进行梯度洗脱。结果表明,9种目标化合物的质量浓度在0.5~50 mg·L^(−1)内与对应的峰面积呈线性关系,检出限(3S/N)为0.5 mg·kg^(−1)。按照标准加入法进行回收试验,回收率为85.3%~116%,测定值的相对标准偏差(n=6)均小于10%。方法用于72批标识有视黄醇及其衍生物化妆品的分析,其中39批样品的检出结果与标识的不一致,6批样品中检出禁用的视黄酸、异视黄酸。
The cosmetic sample(1.000 g)was taken and placed in a 10 mL-stoppered colorimetric tube,and the mixture was made its volume up to 10 mL with the mixed solution of acetonitrile and tetrahydrofuran at a volume ratio of 4∶1.The mixture was vortexed for 30 s,extracted by ultrasound for 15 min and colded down.The mixed solution was passed through a 0.45μm filter membrane,and retinol and its derivatives,including retinoic acid,isoretinoic acid,retinal,retinol acetate,hydroxypinacolone retinoate,retinol propionate,retinol retinoate,and retinol palmitate in the filtrate were determined by high performance liquid chromatography.ZORBAX Eclispse Plus C18 chromatographic column was used as the stationary phase and the mixed solution composed of acetonitrile,tetrahydrofuran and 5 mmol·L^(−1) ammonium acetate solution at different volume ratios was used as the mobile phase for gradient elution.As shown by the results,linear relationships between the corresponding peak areas and mass concentrations of 9 target compounds were kept in the range of 0.5-50 mg·L^(−1),with detection limits(3S/N)of 0.5 mg·kg^(−1).Test for recovery was made by the standard addition method,giving results in the range of 85.3%-116%,with RSDs(n=6)of the determined values less than 10%.The method was applied to analysis of 72 batches of cosmetics labeled with retinol and its derivatives.The detection results of 39 batches of samples were inconsistent with the labels,and prohibited retinoic acid and isoretinoic acid were detected in 6 batches of samples.
作者
周智明
李静
陈张好
陆土柳
ZHOU Zhiming;LI Jing;CHEN Zhanghao;LU Tuliu(Guangdong Institute for Drug Control,National Medical Products Administration Key Laboratory for Safety Risk Assesment of Cosmetics,Guangzhou 510525,China)
出处
《理化检验(化学分册)》
北大核心
2025年第7期802-808,共7页
Physical Testing and Chemical Analysis(Part B:Chemical Analysis)
基金
广东省药品监督管理局化妆品风险评估重点实验室专项(2023ZDZ11)
广东省中医药局面上项目(20221053)
广东省药品监督管理局科技引导扶持专项(2022YDZ04)
广东省药品监督管理局科技创新团队项目(2022TDZ09)
广东省医学科学技术研究基金面上项目(B2021160)。
关键词
高效液相色谱法
化妆品
视黄醇及其衍生物
high performance liquid chromatography
cosmetic
retinol and its derivative
