二维高效液相色谱-质谱联用检测化妆品中乌洛托品等4种禁用物质的方法  

Determination of Four Prohibited Substances,Including Urotropine,in Cosmetics by Two-Dimensional High-Performance Liquid Chromatography-Mass Spectrometry

作　　者：刘益庆 陈洪岩 杨晖 左武剑 LIU Yiqing;CHEN Hongyan;YANG Hui;ZUO Wujian(Lianyungang Food and Drug Inspection and Testing Center,Lianyungang 222000,Jiangsu,China;Jiangsu Provincial Drug Administration,Nanjing 210019,Jiangsu,China)

机构地区：[1]连云港市食品药品检验检测中心,江苏连云港222000 [2]江苏省药品监督管理局,江苏南京210019

出　　处：《香料香精化妆品》2025年第2期106-110,共5页Flavour Fragrance Cosmetics

基　　金：江苏省药品监督管理局科研项目(编号202368)。

摘　　要：建立了化妆品中乌洛托品等4种禁用物质的二维高效液相色谱-三重四极杆质谱联用法。一维色谱以0.01 mol/L磷酸二氢钾溶液(用氢氧化钾调节pH值至6.5)-乙腈(体积比97∶3)为流动相,对待测组分进行分离及捕集;二维色谱以体积分数0.1%甲酸溶液-乙腈为流动相,进行梯度洗脱;采用电喷雾离子源,分别以正、负离子多反应监测模式(MRM)对目标化合物进行定性定量分析。乌洛托品、非那西丁、咪唑、磺胺酸钠分别在10.37~518.5、10.48~524.0、10.46~523.0、101.60~5078.0μg/L线性关系良好,相关系数(r)均大于0.9994,平均回收率在90.62%~103.60%。该方法无需前处理,可使用含盐流动相、专属性好、灵敏度高,适用于复杂化妆品体系中乌洛托品等4种禁用物质的检测。A two-dimensional high-performance liquid chromatography-triple quadrupole mass spectrometry method was established for the determination of 4 prohibited substances in cosmetics,including urotropine.One-dimensional chromatography used 0.01 mol/L potassium dihydrogen phosphate solution(pH adjusted to 6.5 with potassium hydroxide)-acetonitrile(volume ratio 97:3)as the mobile phase to separate and capture the components to be measured.Two⁃dimensional chromatography used 0.1%in volume fraction formic acid solution-acetonitrile as mobile phase for gradient elution.The target compounds were qualitatively and quantitatively analyzed by electrospray ion source with positive and negative ion multi reaction monitoring mode(MRM).The results showed that the linearities of urotropine,phenacetin,imidazole and sodium sulfamate were good in the range of 10.37-518.5,10.48-524.0,10.46-523.0,101.60-5078.0μg/L with the correlation coefficient(r)all greater than 0.9994.The average recoveries were in the range of 90.62%-103.60%.The method does not require pretreatment and can use salt-containing mobile phase.It has good specificity and high sensitivity,and is suitable for the detection of 4 prohibited substances such as urotropine in complex cosmetic systems.

关 键 词：二维高效液相-三重四极杆质谱联用 复杂化妆品体系 禁用物质 含盐流动相 

分 类 号：O657.7[理学—分析化学]