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出 处:《中国卫生检验杂志》2017年第22期3221-3224,共4页Chinese Journal of Health Laboratory Technology
摘 要:目的建立化妆品中12种紫外吸收剂的高效液相色谱-四极杆飞行时间串联质谱(HPLC-Q-TOF-MS)检测方法。方法样品以甲醇-四氢呋喃-水-高氯酸(250∶450∶300∶0.2,V/V)的混合溶液溶解,经超声提取,0.22μm有机滤膜过滤,滤液以ZORBAX Eclipse XDB-C_(18)(3 mm×100 mm,1.8μm)为分离柱,5 mmol/L甲酸铵-0.1%甲酸水溶液-乙腈为流动相,梯度洗脱,用串联质谱电喷雾正离子模式(ESI+)进行测定,利用Targeted MS/MS模式,根据保留时间、一级质谱及二级质谱碎片信息进行定性、定量分析。结果 12种紫外吸收剂线性相关系数均>0.990,RSD均<5.7%,回收率为78.2%~119.7%。结论该方法简单、快速、灵敏,可用于化妆品中12种紫外吸收剂的检测。Objective To establish a high performance liquid chromatography quadrupole time of flight mass spectrometry( HPLC-Q-TOF-MS) method for the determination of twelve ultraviolet absorbents in cosmetics. Methods The samples were ultrasonically extracted with methanol-tetrahydrofuran-water-perchloric acid( 250 ∶ 450 ∶ 300 ∶ 0. 2,V/V) and filtrated with0. 22 μm organic filter membrane. The separation was performed on an ZORBAX Eclipse XDB-C18( 3 mm × 100 mm,1. 8 μm)column with 5 mmol/L ammonium formate( containing 0. 1% formic acid)-acetonitrile as mobile phase by gradient elution.Electrospay ionization( ESI) source was applied and operated in a positive ion mode. The qualitative and quantitative analysis were based on retention time,mass spectra and tandem mass spectra from the targeted MS/MS mode. Results The correlative coefficient of the twelve ultraviolet absorbents was above 0. 990,and the relative standard deviations( RSDs) were less than5. 7%. The average recoveries were within 78. 2%-119. 7%. Conclusion The method is simple,rapid and sensitive. It is suitable for the simultaneous determination of the twelve ultraviolet absorbents in cosmetics.
关 键 词:高效液相色谱-四极杆飞行时间串联质谱法 化妆品 紫外吸收剂
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