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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。
The establishment of the cosmetics diphenhydramine ion exchange chromatography - fluorescence detection methods and liquid chromatography - tandem mass spectrometry method. The sample was extracted with acetonitrile containing 0.2% formic acid. The mobile phase consisted of acetonitrile-0.05 mol / L KH2PO4 solution (7 + 3, V / V) and strong cation exchange column (250 × 4.6 mm, 5 μm) Fluorescence detection excitation wavelength 258 nm, emission wavelength 288 nm, external standard quantitative, diphenhydramine detection limit of 1.5 mg / kg, 0.2 to 20 mg / L in the range of good linear relationship, the correlation coefficient of 0.9999, the method of The recoveries ranged from 87.6% to 106.3% with relative standard deviations below 6.3%. Confirmation of mass spectrometry with BEH C18 column, acetonitrile -0.2% formic acid gradient elution, the use of mass spectral fragments and relative abundance of ions for qualitative confirmation.