摘要
目的建立化妆品中雄性激素睾丸酮、甲基睾丸酮的高效液相色谱鄄质谱(HPLC鄄MS)鉴定方法。方法样品用甲醇萃取后,用液相色谱鄄质谱分析鉴定,色谱柱为C18,流动相为甲醇∶水=80∶20(V/V);流速为0.98ml/min。质谱电离方式为ESI正模式,采用多级m/z303的特征碎片离子峰质谱功能。结果通过优化色谱和质谱仪器条件,选择二级质谱的特征碎片离子,睾丸酮离子峰m/z289的特征碎片离子峰m/z271,m/z253,甲基睾丸酮分子离子峰m/z303的特征碎片离子峰m/z285,m/z267,可以对样品进行准确的定性;采用柱后添加0.2%的甲酸,在相同浓度下,信号强度提高了近20倍。利用该方法对某雄激素疑似阳性的化妆品样品中的睾丸酮、甲基睾丸酮的进行鉴定,结果为阴性。结论该法特异性高,选择性强,灵敏度高,分析时间短,有较好的重现性,适合对化妆品中雄激素的定性。
Objective To establish an LC-M5 method for identification of testosterone and methyhestosterone in cosmetic. Methods Testosterone and methyltestosterone in cosmetic were determined by liquid chromatography mass spectrometry system which can incorporate electrospray ionization interface,post-column addition agent of formic acid. Results The condition of determination was investigated and optimized. The structure of testosterone and methyhestosterone were identified by direct comparison of the observed mass spectra or by the characteristic ions in the selected-ion monitoring as well as MS2 mode. A doubtful testosterone positive cosmetic was identified by this method, it was negative. Conclusion This method has a high sensitivity and a good reproducibility. It is proved that the method is especially suitable for detection of testosterone and methyltestosterone in cosmetics.
出处
《环境与健康杂志》
CAS
CSCD
北大核心
2005年第6期473-474,共2页
Journal of Environment and Health
关键词
化妆品
睾丸酮
甲基睾丸酮
液相色谱-质谱
Cosmetic
Testosterone
Methyltestosterone
Liquid chromatography mass spectrometry
作者简介
吴西梅（1971-）,女,主管技师,硕士,从事食品理化检验研究.
