高效液相色谱-串联质谱法测定化妆品中12种N-亚硝胺类物质

Determination of 12 N-nitrosamines in cosmetics by performance liquid chromatography-triple quadrupole mass spectrometry

建立了化妆品中12种N-亚硝胺类物质的高效液相色谱-串联三重四极杆质谱(HPLC-MS/MS)检测方法。0.5 g样品用25 mL 50%(V/V)甲醇水溶液溶解后,冰浴超声提取5 min, 10000 r/min离心5 min净化,以PFP色谱柱为分析柱,5 mmol/L甲酸胺(含0.1%甲酸)水溶液-甲醇为流动相梯度洗脱,大气压化学电离源电离后正离子、多反应监测模式测定,外标法定量。12种亚硝胺类物质在5~200μg/L范围内线性良好(r^(2)>0.99),检出限为5~50μg/kg。膏霜、乳液和水剂3种基质的平均回收率为78.9%~119.7%,相对标准偏差为0.71%~8.8%。本方法能够为化妆品中12种亚硝胺类物质的监测评估提供技术手段。

The method for the simultaneous determination of twelve N-nitrosamines from cosmetics by high performance liquid chromatography-triple quadrupole mass spectrometry (HPLC-MS/MS) was developed. 0.5 g of sample was dissolved in 25 mL of50%(V/V) methanol solution, then the twelve N-nitrosamines were extracted from cosmetics byice bath supersonic extraction for 5 min, and the extracts were purified by centrifugation with10000 r/min for 5 min. The chromatographic separation was performed on PFP column bygradient elution,with 5 mmol/L formic acid amine (containing 0.1% formic acid) aqueoussolution- methanol as mobile phase at a flow rate of 0.3 mL/min.The twelve N-nitrosamines wereanalyzed in positive ions mode under multiple reaction monitoring (MRM) mode, after ionizationby atmospheric pressure chemical ionization source, and quantified by external standard method.Results showed that there were good linear relationships for the twelve N-nitrosamines in therange of 5-200 µg/L, with their correlation coefficients (r^(2)) more than 0.99. The limits of detectionwere 5-50 µg/kg. The average recoveries of the twelve N-nitrosamines in cream, emulsion andwater ranged from 78.8% to 119.7%,with the relative standard deviations (RSDs) of 0.7%-8.8%.The method can be used for monitoring and evaluation of twelve N-nitrosamines in cosmetics.