高效液相色谱法同时测定化妆品中的17种过敏原.docVIP

高效液相色谱-串联质谱法测定化妆品中的壬基苯酚 席海为，马 强*，刘 茜，王 烨 （中国检验检疫科学研究院，北京 100123 摘 要：建立了测定化妆品中的液相色谱方法。不同类型的化妆品样品经甲醇超声提取，以8 000 r/min离心，取上清液。采用XBridge C18色谱柱（2.1 mm×150 mm, 3.5 μm）分离，以流动相梯度洗脱，流速 mL/min；电喷雾负离子模式电离，多反应监测模式检测，内标法定量。壬基苯酚监测离子对为m/z 219.1/132.9和219.1/147.0，选择4-n-壬基苯酚为内标，监测离子对为m/z 219.1/106.0和219.1/119.0。定量限为mg/kg，线性范围～0 μg/L。在、中、3个添加水平的平均回收率为%～%，相对标准偏差为～％。 关键词：液相色谱；；化妆品 Internal standard method determine Nonylphenol in Cosmetics by Liquid Chromatography Tandem Mass Spectrometry XI Hai-wei, MA Qiang*, LIU Xi, WANG Ye, DING Lan, SU Ning, BAI Hua,WANG Chao (Chinese Academy of Inspection and Quarantine, Beijing 100123, China) Abstract：A comprehensive analyticalliquid chromatography tandem mass spectrometry was developed for the determination of nonylphenol in cosmetics. Different cosmetic samples (cream, lotion, powder and lipstick) were extracted ultrasonically with methanol-methylene dichloride or ethanol-methylene dichloride mixture solutions for 30 min and then centrifuged at the speed of 8 000 r/min. The extract was cleaned up on an Oasis HLB solid phase extraction cartridge and separated on a Waters XBridge C18 column (2.1 mm × 150 mm, 3.5 μm) by gradient elution with methanol-ammonia (99.9+0.1) solution as the mobile phase at a flow rate of 0.25 mL/min. The analysis of nonylphenol was performed under ESI- multiple reaction monitoring (MRM) mode, and the quantification was conducted by internal calibration method. The monitoring ions for nonyphenol were m/z 219.1/132.9 and 219.1/147.0. 4-n-Nonylphenol was selected as internal standard with the monitoring ions of m/z 219.1/106.0 and 219.1/119.0. The limit of quantitation (LOQ) for nonylphenol was 0.2 mg/kg. The method showed a good linearity in the range of 10～0 μg/L. The mean recoveries at the low, middle and high spiked levels were in the range of 83.1%～% with the relative standard deviations (RSDs) of 2.75～. Key words: High performance liquid chromatography-tandem mass spectrometry; nonylphenol; cosmetics 壬基苯酚作为一种