LC-Q-TOF和LC-MS/MS测定化妆品中地索奈德及甲基泼尼松龙醋酸酯同分异构体*
Rapid determination of desonide and methylprednisolone acetate in cosmetics by time of flight mass spectrometry and liquid chromatography-tandem mass spectrometry
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摘要: 运用LC-Q-TOF技术,研究了地索奈德和甲基泼尼松龙醋酸酯同分异构体的二级质谱特征信息;利用LC-MS/MS技术,优化了快速测定该组同分异构体的方法.样品经提取、净化后,使用C-18柱分离,以0.1%乙酸-水和0.1%乙酸-乙腈溶液为流动相进行梯度洗脱.6 min内实现了对该组同分异构体的快速测定.检出限为2μg /kg,定量限为6μg /kg;回收率为90.7%~101.1%,RSD为2.1 %~6.8%,方法对该组同分异构体的基质效应分别为0.95和1.07.Abstract: The LC-Q-TOF was used to study the secondary MS information of desonide and Methylprednisolone acetate isomers.A method was developed for determination of desonide and methylprednisolone acetate in cosmetics by LC-MS/MS.The samples were extracted and purified,separated with a C-18 column using a binary solvent system composed of 0.1% acetic acid water solution and 0.1% acetic acid acetonitrile solution by gradient elution in 6 minute.A rapid determination of the isomer of this group was achieved.The limits of detection(LODs) and quantitation( LOQs) were 2μg/kg and 6μg/kg,respectively.Satisfactory recoveries from 90.7% to 101.1%,and the relative standard deviations(RSDs) were in the range of 2.1%—6.8%.The matrix effects of this group isomers were 0.95 and 1.07,respectively.
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