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目的建立气相色谱-质谱法测定乳液类化妆品中氮芥的分析方法。方法样品用碳酸钠碱化,加无水硫酸钠吸水固化,然后用环己烷-乙酸乙酯(1∶1,V/V)溶液进行液固提取,提取液置于冰箱冷冻,高速离心后供气相色谱-质谱分析。结果氮芥在浓度为0.1μg/ml~5.0μg/ml时线性良好(r=0.999 95),在0.1μg/g~2.5μg/g添加水平回收率为89%~96%,相对标准偏差为4.2%~6.3%,检出限(LOD)为0.02μg/g,定量限(LOQ)为0.1μg/g。结论该方法能有效去除乳液类化妆品中复杂基质,方法灵敏度高,定性、定量准确,为测定乳液类化妆品中氮芥提供一种新的方法和思路。
Objective To establish a method for the determination of nitrogen mustards in latex cosmetics by gas chromatography-mass spectrometry. Methods The samples were alkalized with sodium carbonate and solidified by adding anhydrous sodium sulfate. The mixture was then liquid-solid extracted with cyclohexane-ethyl acetate (1: 1, V / V) solution. The extract was frozen in a freezer and centrifuged Gas chromatography - mass spectrometry. The results showed that the nitrogen mustard had a good linearity (r = 0.999 95) at the concentration of 0.1μg / ml ~ 5.0μg / ml and the recovery of 89% ~ 96% at the concentration of 0.1μg / g ~ 2.5μg / g with the relative standard deviation 4.2% ~ 6.3%, the limit of detection (LOD) was 0.02μg / g and the limit of quantification (LOQ) was 0.1μg / g. Conclusion The method can effectively remove complex matrix in emulsion cosmetics. The method is sensitive, qualitative and quantitative, and provides a new method and idea for the determination of nitrogen mustards in latex cosmetics.