超高效液相色谱-三重四极杆质谱法测定化妆品中环吡酮胺含量  

Determination of Ciclopirox Olamine in Cosmetics by Ultra Performance Liquid Chromatography-triplequadrupole Mass Spectrometry

作　　者：李晓宇 曹海荣 王思怿 LI Xiao-yu;CAO Hai-rong;WANG Si-yi(Shanghai Research Institute of Chemical Industry Co.,Ltd.,Shanghai 200062,China;School of Chemical and Environmental Engineering,Shanghai Institute of Technology,Shanghai 201418,China)

机构地区：[1]上海化工研究院有限公司,上海200062 [2]上海应用技术大学化学与环境工程学院,上海201418

出　　处：《化学试剂》2021年第3期345-349,共5页Chemical Reagents

基　　金：上海市化学品公共安全工程技术研究中心项目(8DZ2280700)。

摘　　要：建立了一种超高效液相色谱-串联质谱(UPLC-MS/MS)的方法用来测定化妆品中环吡酮胺的含量。使用沃特世超高效液相色谱C18色谱柱(1.7μm×2.1 mm×50 mm),以甲醇/水(含0.1%甲酸)溶液为流动相进行梯度洗脱,流速设定为0.5 mL/min,进样量设置为2μL,在电喷雾正离子模式下(ESI^(+)),采用多反应监测(MRM)模式进行定性和定量测定。结果表明,建立的分析方法在所研究的范围内浓度和峰面积具有良好的线性关系,相关系数为0.999 6,平均加标回收率为107.9%(n=3),平均相对标准偏差(RSD)为4.80%(n=6),检出限浓度为0.066 8 mg/kg,定量限浓度为0.223 mg/kg,该方法方便、灵敏、准确,适用于化妆品中环吡酮胺的含量检测与质量监督。An UPLC-MS/MS method for the determination of ciclopirox olamine in cosmetic samples has been developed.The UPLC separation was carried out on a Waters Acquity UPLC^(®) BEH C_(18) column(1.7 μm×2.1 mm×50 mm) by gradient elution using methanol/water(containing 0.1% formic acid) system.The flow rate is 0.5 mL/min and sample injection amount is 2 μL.The electrospray ionization source in positive ion mode(ESI^(+)) was used for qualitative analyzing and quantitative analyzing of ciclopirox olamine in the multiple reaction monitoring(MRM) mode.The developed method has a good linear relationship between concentration and peak area in the corresponding concentration range.The linear correlation coefficient is 0.999 6,and the average recoveries of standard addition is 107.9%(n=3),and the average relative standard deviation is 4.80%(n=6),the limit of detection is 0.066 8 mg/kg,and the limit of quantification is 0.223 mg/kg.The method is convenient,sensitive and accurate,and the good analytical features of the proposed method make it useful to carry out the quality control of cosmetic products and raw materials to assure the safety of users.

关 键 词：环吡酮胺 化妆品 超高效液相色谱-串联质谱法 检出限 定量限 线性相关系数 

分 类 号：O657.63[理学—分析化学]