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目的建立化妆品中抗生素快速筛查和确证的超高效液相色谱-线性离子阱/静电场轨道阱高分辨质谱法(ultra high performance liquid chromatography-linear ion trap/orbitrap high resolution mass spectrometry)。方法采用超声波辅助提取化妆品中的抗生素类化合物,提取液经ACQUITY BEH C18色谱柱分离,以水(含5 mmol/L乙酸铵和0.1%甲酸)-乙腈为流动相,梯度洗脱分离。静电场轨道阱一级全扫描得到的准分子离子的精确质量数用于快速筛选分析,保留时间和离子阱的二级质谱数据用于进一步定性确证。结果 36种抗生素的精确质量相对偏差小于5×10-6(5 ppm),线性相关系数r2大于0.994,方法检出限(limit of detection)均≤10μg/kg,方法的加标回收率为54.15%~117.55%,相对标准偏差(relative standard deviation)为1.19%~13.25%。结论应用该方法对不同剂型的50余种化妆品实际样品筛查的分析结果良好,说明该方法是化妆品中抗生素类成分快速筛选和确证的有效方法。
Objective To establish an ultra high performance liquid chromatography-linear ion trap / orbitrap high resolution mass spectrometry for the rapid screening and confirmation of antibiotics in cosmetics. Methods Ultrasound-assisted extraction of antibiotics in cosmetics was performed. The extract was separated on an ACQUITY BEH C18 column with gradient elution using water (containing 5 mmol / L ammonium acetate and 0.1% formic acid) -acetonitrile as mobile phase. The exact masses of quasi- ion ions obtained by full scan of the electrostatic field orbit well are used for rapid screening analysis, retention times, and ion trap secondary mass spectral data for further qualitative confirmation. Results The relative bias of 36 antibiotics was less than 5 × 10-6 (5 ppm) and the linear correlation coefficient (r2) was greater than 0.994. The limits of detection were all ≤ 10 μg / kg. The recoveries were 54.15 % ~ 117.55%, the relative standard deviation was 1.19% ~ 13.25%. Conclusion The method of this method is good for screening more than 50 kinds of cosmetic samples with different dosage forms, which shows that this method is an effective method for rapid screening and confirmation of antibiotic components in cosmetics.