摘要
建立了化妆品中苯海拉明的离子交换色谱-荧光检测方法及液相色谱-串联质谱确证方法。样品用含0.2%甲酸的乙腈提取,定量检测时以乙腈-0.05 mol/L KH2PO4溶液(7+3,V/V)为流动相,强阳离子交换色谱柱(250×4.6 mm,5μm)分离,荧光检测激发波长258 nm,发射波长288 nm,外标法定量,苯海拉明检出限为1.5 mg/kg,在0.2~20 mg/L范围内线性关系良好,相关系数为0.9999,方法的回收率在87.6%~106.3%范围内,相对标准偏差低于6.3%。质谱确证时用BEH C18色谱柱分离,乙腈-0.2%甲酸系统梯度洗脱,采用质谱碎片和相对离子丰度进行定性确认。
A quantitative method using ion exchange chromatography with fluorescence assay and a qualitative method using liquid chromatography-tandem mass spectrometry（LC-MS/MS） were developed for determination of diphenhydramine in cosmetics.Samples were extracted with acetonitrile containing 0.2% formic acid.Chromatographic analysis was performed on a strong cation exchange column using acetonitrile-0.05 mol/L potassium dihydrogen phosphate solution（7：3,V/V） as mobile phase.Quantitation analysis was carried out with the external standard method using fluorescence detector at excitation/emission wavelength 258/288 nm.The calibration curve was linear in the range of 0.2 - 20 mg/L（r = 0.9999） with detection limit of 1.5 mg/kg.The recoveries ranged from87.6 % to 106.3 % with relative standard deviations less than 6.3 %.Mass spectrometry method was performed on a BEH C18 column using a gradient acetonitrile-aqueous solution containing 0.1% formic acid system as mobile phase.Qualitative confirmation was depended on mass spectrometry fragments and the relative ion abundance.The method is accurate,fast,simple and practical,and has extensive application prospect.
出处
《分析试验室》
CAS
CSCD
北大核心
2017年第2期172-176,共5页
Chinese Journal of Analysis Laboratory
基金
国家质检总局科技计划项目(2015IK216)资助
关键词
化妆品
苯海拉明
离子交换色谱-荧光检测
液相色谱-串联质谱
Cosmetics
Diphenhydramine
Ion exchange chromatography with fluorescence assay
Liquid chromatography-tandem mass spectrometry
