Meng Xian-Shuang, Bai Hua, Zhang Qing, Lv Qing, Chen Yun-Xia, Ma Hui-Juan, Li Jing-Rui, Ma Qiang
J AOAC Int. 2014 Nov-Dec;97(6):1538-45. doi: 10.5740/jaoacint.13-314.
A sensitive and reliable analytical method based on HPLC/MSIMS has been developed for the simultaneous determination of 15 nitroimidazoles in cosmetics. A diversity of cosmetic samples, including powder, lotion, shampoo, and cream were collected. The samples were ultrasonically extracted with aqueous methanol, and the extracts were then subjected to cleanup bySPE using an Oasis HLB cartridge followed by filtration with a 0.20 pm membrane filter. Afterwards, chromatographic separation was performed on an XSelect CSH C18 column (2.1 x 150 mm, 3.5 pm) maintained at 30°C within 15 min by a gradient of acetonitrile-0.1% aqueous formic acid solution at a flow rate of 0.25 mL/min. The mass spectrometric detection was carried, out using electrospray positive ionization under the multiple reaction monitoring mode. A good linearity was observed over the concentration range from 0.5 to 500 ng/mL. The intraday and interday precisions, which were investigated by determining all target compounds in cosmetics seven times/day and on 7 consecutive days, were below 5.00%. The mean recoveries at three spiked levels ranged from 80.42 to 100.83% with the RSDs from 0.45 to 9.02%. The LOQs were determined to be between 0.01 and 0.1 mg/kg. The method was sufficiently rapid, reliable, and sensitive for the determination of 15 nitroimidazoles in cosmetics.
已开发出一种基于高效液相色谱/质谱联用的灵敏可靠的分析方法,用于同时测定化妆品中的15种硝基咪唑。收集了多种化妆品样品,包括粉末、乳液、洗发水和面霜。样品用甲醇水溶液超声提取,提取物先用Oasis HLB柱进行固相萃取净化,然后用0.20μm的膜过滤器过滤。之后,在XSelect CSH C18柱(2.1×150mm,3.5μm)上进行色谱分离,柱温保持在30℃,在15分钟内用乙腈-0.1%甲酸水溶液梯度洗脱,流速为0.25mL/min。质谱检测采用电喷雾正离子模式下的多反应监测模式。在0.5至500ng/mL的浓度范围内观察到良好的线性关系。通过每天测定化妆品中的所有目标化合物7次并连续测定7天来研究日内和日间精密度,结果均低于5.00%。三个加标水平下的平均回收率在80.42%至100.83%之间,相对标准偏差在0.45%至9.02%之间。定量限测定为0.01至0.1mg/kg。该方法对于测定化妆品中的15种硝基咪唑足够快速、可靠且灵敏。