摘要
建立了高效液相色谱-二极管阵列检测器(HPLC-DAD)方法,用于测定化妆品中茶碱的含量。样品经甲醇超声提取后,高速离心处理,采用Ultimate-XB-C_(18)色谱柱(150 mm×4.6 mm×3μm)分离。以甲醇-0.1%(体积分数)磷酸水溶液为流动相,采用梯度洗脱。在272 nm波长下,8 min内完成定量分析。茶碱在0.5~20 mg/L内线性关系良好(r>0.999)。茶碱的检出限和定量限分别为10 mg/kg和25 mg/kg。在水基类、乳液类、膏霜类、粉类化妆品中,茶碱回收率为92.5%~111.0%,相对标准偏差(RSD,n=6)为0.4%~1.9%。对于高效液相色谱法检出或存在干扰的样品,进一步采用液相色谱-串联质谱法进行确证。方法具有简便、快捷、准确、灵敏等特点,可以满足进出口化妆品中茶碱含量准确定量的测定要求。
A method of high performance liquid chromatography-diode array detector(HPLC-DAD)was developed for the determination of theophylline in cosmetics.The sample was extracted with methanol in ultrasonic assisted extraction coupled with high speed centrifugation.The separation was performed on Ultimate-XB-C_(18) chromatographic column(150 mm×4.6 mm×3μm).Separation was carried out using methanol-0.1%(in volume fraction)phosphoric acid solution as the mobile phase for gradient elution.Quantitative analysis was completed within 8 min at a wavelength of 272 nm.The theophylline had a good linear relationship in the range of 0.5-20 mg/L(r>0.999).The detection limit of theophylline was 10 mg/kg,and the quantitative limit was 25 mg/kg.The recovery rates of theophylline were in the range of 92.5%-111.0%,with relative standard deviations(RSDs)of 0.4%-1.9%in water-based,emulsion,cream,and powder cosmetics.For samples that were detected or exhibiting interference in the liquid chromatography method,high-performance liquid chromatography tandem mass spectroscopy(HPLC-MS/MS)should be further employed for confirmation.The method with simple-pretreatment,high sensitivity is rapid,accurate,and suitable for the requirements of accurate quantitative determination of theophylline content in imported and exported cosmetics.
作者
洪灯
周江
严媛
尚凡贞
陈安
刘婷
王良莉
HONG Deng;ZHOU Jiang;YAN Yuan;SHANG Fanzhen;CHEN An;LIU Ting;WANG Liangli(Zhejiang Academy of Science and Technology for Inspection and Quarantine,Hangzhou 311215,Zhejiang,China;Technic Center of Hangzhou Customs,Hangzhou 311215,Zhejiang,China;Standardization Institute of Yiwu,Yiwu 322000,Zhejiang,China)
出处
《香料香精化妆品》
2025年第5期1-5,共5页
Flavour Fragrance Cosmetics
基金
杭州海关科研项目(编号2020HZ04)
海关总署科研项目(编号2024HK085)。
关键词
化妆品
高效液相色谱
茶碱
确证
cosmetics
high performance liquid chromatography(HPLC)
theophylline
confirmation
