摘要
建立了快速、准确测定网络销售婴幼儿湿疹类产品中43种糖皮质激素类药物的超高效液相色谱-串联三重四级杆质谱(UHPLC-MS/MS)检测方法。对样品前处理条件、色谱和质谱条件进行了优化,最终样品以乙腈超声提取,提取液稀释后直接进样,采用UHPLC-MS/MS在多重反应监测(MRM)模式下进行定性筛查。对筛查结果疑似阳性的样品,根据保留时间和特征离子对的相对丰度比定性,并采用定量离子对进行外标法定量。采用该方法对网络销售的41批湿疹相关“妆”字号产品和“消”字号产品进行检测,其中有6批产品中检出糖皮质激素,两类产品的检出率分别为5.9%和57.1%。该方法操作简便、准确可靠,可用于实际样品检测的需要,为化妆品安全监管提供技术支撑。
A fast and accurate method for the determination of 43 kinds of glucocorticoids in infant eczema products by UHPLC-MS/MS was established.The samples were extracted with acetonitrile ultrasonically.The supernatant was diluted and injected directly.After optimizing the sample pretreatment and chromatography conditions,as well as mass spectrometry parameters,UHPLC-MS/MS analysis method was performed for qualitative screening in MRM mode.The samples with suspected positive screening results were further confirmed.Qualitative analysis was conducted according to retention time and relative abundance ratio of characteristic ion pairs.Quantitative ion pairs were used for quantitative measurement by external standard method.This method was used for detecting 41 batches of eczema-related cosmetic products and disinfection products sold online.Glucocorticoids were detected in 6 batches of products,and the detection rates of the two types of products were 5.9% and 57.1%,respectively.The method is simple,accurate and reliable,which can be used for the actual sample detection and provide technical support for cosmetic safety supervision.
作者
董亚蕾
刘钊
王海燕
孙磊
DONG Ya-lei;LIU Zhao;WANG Hai-yan;SUN Lei(National Institutes for Food and Drug Control,Beijing 100050,China)
出处
《日用化学工业》
CAS
CSCD
北大核心
2020年第12期885-891,895,共8页
China Surfactant Detergent & Cosmetics