固相萃取-液相色谱-串联质谱法测定祛痘化妆品中硝基咪唑类药物  

Determination of nitroimidazoles in acne dispelling cosmetics with solid phase extraction and high performance liquid chromatography-tandem mass spectrometry

作　　者：卢剑[1] 武中平[1] 车文军[1] 洪华[1] 杨洋[1] 

机构地区：[1]江苏省产品质量监督检验研究院国家化妆品质量监督检验中心,江苏南京210007

出　　处：《日用化学工业》2014年第11期652-655,660,共5页China Surfactant Detergent & Cosmetics

摘　　要：采用固相萃取（SPE）净化技术和高效液相色谱-串联质谱仪（HPLC-MS/MS）,研究并建立了同时测定祛痘化妆品中6种硝基咪唑类药物（甲硝唑、替硝唑、奥硝唑、地美硝唑、洛硝唑和塞克硝唑）的方法。样品用酸化乙腈溶液提取,阳离子固相萃取小柱净化,以体积分数为0.1%甲酸乙腈溶液-体积分数为0.1%甲酸水溶液为流动相,经C18色谱柱梯度洗脱分离,采用HPLC-MS/MS多反应监测模式（MRM）定量检测。结果表明,6种硝基咪唑类药物在质量浓度1.0~50.0μg·L-1内线性关系良好,相关系数均大于0.999;方法定量限均为0.5 mg·kg-1;在祛痘水和祛痘膏样品中进行3个水平的添加实验,平均回收率为89.7%~108.0%,相对标准偏差（n=6）为2.3%~6.5%。A method for simultaneous determination of six kinds of nitroimidazole drug （metronidazole （ MNZ）, tinidazole （ TNZ ）, ornidazole （ ONZ ）, dimetridazole （ DMZ ）, ronidazole （ RNZ ） and seenidazole （SCZ） ） in ache dispelling cosmetics adopting solid phase extraction （SPE） purification technology and high performance liquid chromatography - tandem mass spectrometry （HPLC - MS/MS ） was studied and established. Samples were extracted with acidified acetonitrile solution and the extract was purified with cation resin solid phase exchanging column. Then the purified extract was separated with a C18 column,by gradient elution with acetonitrile and water （containing 0. 1% formic acid, volume fraction ）, and detected by tandem mass spectrometry under multiple reaction monitoring （MRM） mode. The results indicated that good linearity displays when mass concentration of the six kinds of nitroimidazole is within 1.0 - 50. 0 μg .L- 1, and all the linear correlation coefficients are higher than 0. 999. All the limits of quantification （LOQ） are 0. 5 mg. kg-1. The recoveries of six kinds of nitroimidazole when three levels of standard were spiked into samples of ache dispelling cosmetics （both cream type and lotion type） range from 89.7% to 108.0% with RSD （n = 6） from 2.3% to 6.5%.

关 键 词：祛痘化妆品 硝基咪唑类药物 高效液相色谱-串联质谱法 固相萃取 

分 类 号：O657.63[理学—分析化学] TQ658[理学—化学]