高效液相色谱-串联质谱法测定化妆品中壬基苯酚  

HPLC-MS/MS Determination of Nonylphenol in Cosmetics

作　　者：席海为[1] 马强[1] 刘茜[1] 王烨[1] 丁岚[1] 苏宁[1] 白桦[1] 王超[1] 

机构地区：[1]中国检验检疫科学研究院,北京100123

出　　处：《理化检验（化学分册）》2012年第8期970-973,共4页Physical Testing and Chemical Analysis(Part B:Chemical Analysis)

基　　金：国家标准化管理委员会计划资助项目(20090925-T-607);质检公益性行业科研专项计划资助项目(200910267;201010023)

摘　　要：提出了高效液相色谱-串联质谱法测定化妆品中壬基苯酚含量的方法。化妆品试液用甲醇-二氯甲烷(8+2)混合溶液超声提取30 min[唇膏类试样用无水乙醇-二氯甲烷(8+2)混合溶液],离心分离取上清液过Oasis HLB固相萃取柱净化。从SPE净化柱所得淋出液,以WatersXBridge C_(18)色谱柱(2.1 mm×150 mm,3.5μm)为固定相分离,以不同体积比的甲醇和氨水(0.1+99.9)溶液为流动相梯度洗脱,串联质谱进行测定。采用电喷雾负离子模式多反应监测,内标法定量。壬基苯酚的线性范围为10～500μg·L^(-1),测定下限(10S/N)为0.2 mg·kg。方法用于分析4种类型化妆品样品,回收率在83.1%～103.0%之间,相对标准偏差(n=6)在2.75%～9.24%之间。A method of HPLC-MS/MS for the determination of nonylphenol in cosmetics was proposed. The sample was extracted ultrasonically with mixture of CHa OH-CH2 Cl2 （8 ＋ 2） for 30 rain except using mixture of C2 H5 OH-CH2 Cl2 （8＋2） for lipstick. After centrifugation, the supernatant was taken for purification on Oasis H LB solid phase extraction column. The nonylphenol in the eluate from the SPE column was separated on Waters XBridge C18 column （2. 1 mm）〈 150 mm, 3. 5 /,m） by gradient elution with mixtures of CH3OH and ammonia （0. 1＋99.9） solution in different ratios, and determined by MS/MS. The negative electrospray ionization as well as multiple reactions monitoring mode was used in the detection. The internal standard method was used for quantification of nonylphenol. Linearity range of nonylphenol was kept from 10 to 500 μg · L-1, with lower limit of determination （10S/N） of 0. 2 mg · kg-1. The proposed method was applied to the analysis of 4 kinds of cosmetic samples, giving values of recovery in the range of 83. 1%-103. 0% and RSD＇s （n=6） in the range of 2. 75%-9. 24%.

关 键 词：高效液相色谱-串联质谱法 壬基苯酚 化妆品 

分 类 号：O657.62[理学—分析化学]