化妆品中致敏原香豆素及其衍生物的高效液相色谱法测定及质谱确证  

Determination of Coumarin Allergen and Its Derivatives in Cosmetics by HPLC and Their Verification by HPLC-MS/MS

作　　者：孟宪双[1] 马强[1] 袁汉成 白桦[1] 张庆[1] 郭项雨[1] 

机构地区：[1]中国检验检疫科学研究院,北京100176 [2]沃特世科技(上海)有限公司,上海201206

出　　处：《分析测试学报》2016年第7期799-804,共6页Journal of Instrumental Analysis

基　　金：国家科技支撑计划项目(2013BAK04B03);质检公益性行业科研专项项目(2012104013-4);国家标准化管理委员会计划项目(20130980-T-607)

摘　　要：建立了化妆品中致敏原香豆素及其7种衍生物（二氢香豆素、7-甲氧基香豆素、7-甲基香豆素、7-乙氧基-4-甲基香豆素、环香豆素、双香豆素和醋硝香豆素）的高效液相色谱测定方法。样品以0.1 mol/L氢氧化钠溶液-乙腈（1∶9,体积比）混合溶液进行超声提取,提取液经高速离心及微孔滤膜过滤后,ZORBAX SB-C18（250 mm×4.6 mm,5μm）色谱柱分离,0.05 mol/L乙酸铵溶液（含0.25%乙酸）和乙腈为流动相梯度洗脱,二极管阵列检测器检测,外标法定量。疑似阳性样品采用高效液相色谱-串联质谱法进行确证。结果表明,香豆素及其衍生物在一定浓度范围内线性良好（r2≥0.999 6）,定量下限为8～20 mg/kg。在低、中、高3个加标水平下,香豆素及其衍生物的平均回收率为84.6%～100.7%,相对标准偏差（n=6）为0.8%～9.7%。该方法准确、稳定性好、特异性强,能够为化妆品检验和日常生产质量控制提供科学依据及技术支持。A high performance liquid chromatographic （HPLC） method was developed for the deter- mination of coumarin allergen and its seven derivatives, including dihydrocoumarin, 7-methoxy- coumarin, 7-methylcoumarin, 7-ethoxy-4-methyleoumarin, cyclocoumarol, dicoumarol and aceno- coumarol in cosmetics. Cosmetic samples were ultrasonically extracted with 0. 1 mol/L aqueous sodi- um hydroxide -acetonitrile（ 1 ： 9）. The extract was centrifuged, and filtered by microporous mem- brane. The chromatographic separation for the analytes was achieved on a ZORBAX SB -C18 （250 mm ×4. 6 mm, 5 μm） column. Gradient elution was performed using 0. 05 mol/L aqueous ammoni- um acetate solution（containing 0. 25% acetic acid） and acetonitrile. The quantification was carried out by the external standard method, and the suspected samples were further verified by high perform- ance liquid chromatography -tandem mass spectrometry（ HPLC -MS/MS）. The experimental results indicated that good linearities were observed over a certain concentration range with correlation coeffi- cients better than 0. 999 6, and the limits of quantitation （LOQs） were between 8 and 20 mg/kg. The average recoveries for the analytes at three spiked levels ranged from 84.6% to 100.7% with rel- ative standard deviations （RSDs） of 0. 8% - 9.7% . The proposed method is accurate, robust and specific, and could provide scientific basis and a trol of cosmetics. technical support for the inspection and quality con-trol of cosmetics.

关 键 词：香豆素及其衍生物 致敏原 高效液相色谱 高效液相色谱-串联质谱 化妆品 

分 类 号：O657.63[理学—分析化学] TQ658[理学—化学]