摘要
目的 建立同时检测化妆品中六氢化香豆素、7-甲基香豆素、7-甲氧基香豆素、4,6-二甲基-8-特丁基香豆素、7-羟基-6-甲氧基香豆素、7-乙氧基-4-甲基香豆素、5,7-二甲氧基香豆素、苯丙香豆素8种香豆素类化合物的气相色谱-质谱法。方法 采用二氯甲烷作为提取溶剂,超声处理;采用程序升温模式,经弱极性Thermo TG-5SILMS毛细管柱(30 m×0.25 mm,0.25μm)分离,经电子轰击(EI)离子源电离,采用选择离子监测(SIM)扫描测定;外标法定量。结果 上述8种香豆素类化合物的质量浓度分别在2.0~102.0 mg/L、1.0~51.7 mg/L、1.1~56.5 mg/L、1.1~54.4 mg/L、0.4~20.0 mg/L、1.1~55.6 mg/L、1.1~53.3 mg/L、1.0~51.3 mg/L范围内与峰面积线性关系良好,相关系数均大于0.997 0(n=6);7-羟基-6-甲氧基香豆素和苯丙香豆素的检测限分别为128 ng/g和177 ng/g,其余6种香豆素类化合物的检测限为6~41 ng/g。水剂类、乳液类和膏霜类3种基质的方法回收率为89.78%~116.64%(n=6);8种香豆素类化合物在3种不同基质中含量的RSD在0.91%~5.68%范围内,均小于6%。结论 该方法简便、可靠,能满足化妆品中8种香豆素类化合物的检测要求。
Objective To establish a gas chromatography-mass spectrometry (GC-MS) method for the simultaneous determination of eight coumarins including hexahydrocoumarin,7-methylcoumarin,7-methoxycoumarin,4,6-dimethyl-8-tert-butylcoumarin,scopoletin,7-ethoxy-4-methylcoumarin,5,7-dimethoxycoumarin and phenprocoumon in cosmetics.MethodsThe samples were dissolved in dichloromethane,and extracted by the ultrasound.The above eight coumarins were separated through a weak polar Thermo TG-5SILMS capillary column (30 m×0.25 mm,0.25μm) with the mode of programmed temperature.The ionization mode was adopted with the electron-impact (EI) ion source,the selected ion monitoring (SIM) mode was adopted to determine,and the external standard method was adopted for quantitative analysis.ResultsThe linear ranges of the above eight coumarins were 2.0-102.0 mg/L,1.0-51.7 mg/L,1.1-56.5 mg/L,1.1-54.4 mg/L,0.4-20.0 mg/L,1.1-55.6 mg/L,1.1-53.3 mg/L and 1.0-51.3 mg/L(r>0.997 0,n=6),respectively.The limit of detection (LOD) of scopoletin and phenprocoumon was 128 ng/g and 177 ng/g respectively,and that of the other six coumarins was in the range of 6-41 ng/g.The recovery rate of the three types of matrixes including liquid,emulsion and cream preparations was in the range of 89.78%-116.64%(n=6).The RSD of the content of eight coumarins in the above three different matrixes was in the range of 0.91%-5.68%,all lower than 6%.ConclusionThe method is simple and reliable,which can meet the requirements for the determination of eight coumarins in cosmetics.
作者
郑抒
谢静
秦剑
ZHENG Shu;XIE Jing;QIN Jian(Chongqing Institute for Food and Drug Control,Chongqing,China 401121)
出处
《中国药业》
CAS
2022年第17期77-80,共4页
China Pharmaceuticals
